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CN105255462A - Liquid silicon and preparation method thereof - Google Patents

Liquid silicon and preparation method thereof Download PDF

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Publication number
CN105255462A
CN105255462A CN201510557186.5A CN201510557186A CN105255462A CN 105255462 A CN105255462 A CN 105255462A CN 201510557186 A CN201510557186 A CN 201510557186A CN 105255462 A CN105255462 A CN 105255462A
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dispersion
liquid
liquid silicon
acid
tank
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CN105255462B (en
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李纪亮
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Nanjing Yunyue New Material Technology Co Ltd
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Nanjing Yunyue New Material Technology Co Ltd
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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
    • C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
    • C09K8/426—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells for plugging
    • 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
    • C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
    • C09K2208/32—Anticorrosion additives

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  • General Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

The invention discloses liquid silicon and a preparation method thereof. The liquid silicon comprises: by mass, micro silicon powder 15-50%, quartz sand 5-60%, deodorant 0.01-0.2%, pH modifier 0.01-0.65%, pH return modifier 0.01-0.65%, antiseptic 0.05-0.2% and the balance process water. The SiO2 content in the micro silicon powder is more than 85 wt%, and the micro silicon powder has the average particle diameter of 0.1-0.15 [mu]m. The SiO2 content in the quartz sand is more than 95 wt%. The deodorant is selected from peroxide, hypohalite, potassium ferrate and sodium nitrate. The pH modifier and pH return modifier are acid or alkali and match with each other. The liquid silicon is prepared by returning adjusting pH process under the conditions of high-speed distribution and external reflux, and the final pH value is 4.2-7.2. The salt prepared by in-situ reaction during returning adjusting pH process is absorbed on the surface of the dispersive SiO2 floccule, so that the tendencies of sedimentation and gelation of the silicon powder dispersion liquid are inhibited effectively. The liquid silicon can save for 5-6 months, is without obvious tendencies of sedimentation layering and gelation, and has uniform seriflux and good fluidity.

Description

A kind of liquid silicon and preparation method thereof
Technical field
The present invention relates to a kind of liquid silicon and preparation method thereof, more specifically to a kind of liquid silicon and preparation method thereof.
Background technology
API oil well cement is when temperature is lower than 110 DEG C, there is lower rate of permeation, and with the rising of temperature, ultimate compression strength improves, when temperature is more than 110 DEG C, especially when temperature is more than 125 DEG C, the rising ultimate compression strength with temperature significantly reduces, rate of permeation improves greatly, and this phenomenon is called cement strength degeneration at high temperature.Temperature is higher, and cement strength degradation phenomena is more serious, and cause and lose the protection borehole wall, supporting sleeve and packing effect, cause oil well to destroy.Can prevent Behavior of Hardened Cement Paste hot strength from degenerating, stabilizing cement stone intensity, reduce the admixture of Behavior of Hardened Cement Paste rate of permeation, be called the admixture preventing Behavior of Hardened Cement Paste hot strength from degenerating.
Silica flour, as the admixture preventing Behavior of Hardened Cement Paste hot strength from degenerating, is widely used in cement and concrete, especially heating exploitation viscous crude and deep-well cementing.
Silica flour main Types: ground silica (i.e. quartz sand) and SILICA FUME.
Silica flour, can the intergranular hole of filling concrete as a kind of high-temperature stabiliser, generates gelinite with hydrated product simultaneously.In cement, mix appropriate silica flour, can function as follows: the anti-permeability 1) significantly improving cement strength and grout.2) effect that there is water conservation, prevent segregation, reduce pumping resistance.3) work-ing life of significant prolongation oil well, particularly under the severe environment such as villiaumite system erosion, sulphate attack, high humidity.4) during high temperature and the Ca (OH) that releases of hydrated cementitious 2react, reduce the concentration of calcium ion in liquid phase, generate resistant to elevated temperatures C-S-H gel, improve its hot strength and thermostability.
Silica flour density is 2.1 ~ 3.1g/cm 3, generally at 2.3 ~ 2.6g/cm 3.Half security product tap density: 0.2 ~ 0.45g/cm 3.
Quartz sand by use purposes, can be divided into fine quartz powder and thick silica powder, wherein fine quartz powder is generally less than and equals 200 orders, domestic by different requirements, at high temperature widespread use ground silica as the anti-strength degradation agent of high temperature.
SILICA FUME is also silicon ash, be ferrosilicon and industrial silicon in the process of high melt, with the dust of waste gas effusion, SiO in flue gas 2content account for 85% of flue dust total amount, color is canescence, and granularity is very little, and median size is about 0.1 ~ 0.15 μm, in general, fineness be less than 1 μm account for more than 80%, minimum grain size about 0.01 μm.Its specific surface area can reach 20 ~ 28m 2/ g, larger than flyash about 50 times, about larger than cement 80 ~ 100 times.Condensation process when SILICA FUME is formed is very rapid, so SiO 2also do not form crystal, its mineral belong to unformed mineral, and it is the volcanic ash material that a kind of surfactivity is very high, are a kind of admixture for cement slurry of high-quality.
Directly use silica flour at well cementation scene, be dry mixed uneven, dust is large, and environmental pollution is large and high to labor protection requirement.If but silica flour original place is made into aqueous slurry in advance to be re-used, need the outer place of occupying volume.To Yu Haiyang well cementation and the limited place of Active workings, require to use and can keep stable silica flour aqueous slurry within a certain period of time, to add water the aqueous slurry that liquefaction processing becomes stable by silica flour, in industry, claim " liquid silicon ".Certain company external produces the SiO in liquid silicon 2grain diameter is 0.15 μm, and be more than one percent of cement median size, specific surface area is up to 21m 2/ g, has extremely strong surfactivity.
Liquid silicon is SiO 2, easily there is sedimentation layering and SiO in the dispersion liquid of solia particle in water 2gel tendency two large problems.The general storage 2-3 month, i.e. sedimentation layering, surperficial bleed, bottom deposit lumps, or gelation can not be flowed.U.S. US5176752 discloses the preparation method of hydramine as stablizer, EP1534646 discloses the method as stablizer such as xanthan gum, CMC, HEC and composition thereof, but dispersion agent disclosed in these patents and stablizer and method thereof, effect not obvious in actual use, and the organism introduced also add liquid silicon microbiological contamination probability, liquid silicon is deposited smelly summer, and sedimentation layering in winter and gel tendency seriously cannot recover mobility by stirring, and impact uses.
Summary of the invention
Easy rancid, liquid uneven first-class problem when storing for the silicon liquid that exists in prior art, the invention provides a kind of liquid silicon, this silicon liquid can suppress sedimentation and the gel tendency of silica flour dispersion liquid with imitating, and extends the shelf time.
Object of the present invention is achieved through the following technical solutions.
A kind of liquid silicon, comprise SILICA FUME, quartz sand, reodorant, pH adjusting agent, pH returns adjustment, sanitas, and each constituent mass per-cent is: SILICA FUME 15-50%; Quartz sand 5-60%; Reodorant 0.01-0.2%; PH adjusting agent 0.01-0.65%; PH returns adjustment 0.01-0.65%; Sanitas 0.05-0.2%; Add process water to 100%.
Preferably, described liquid silicon also comprises dispersion agent, deflocculant, antifreezing agent, and each constituent mass per-cent is: dispersion agent 0-0.50%; Deflocculant 0-0.50%; Antifreezing agent 0-25.0%.
Liquid silicon of the present invention adopts under high speed dispersion adds outer circulation condition, prepared by the method for the technique returning adjust pH.By selected SILICA FUME and/or quartz sand, under 1400-3000rpm high speed dispersion adds outer circulation condition, according to dispersion liquid initial acid, alkalescence, select alkali, silica flour dispersion liquid pH value is adjusted to 8.0-3.0 by acid, then with sour, alkali pH value returned and be adjusted to 4.2-7.2.Detailed process is: when SILICA FUME and quartz sand mixture dispersion liquid are initially neutrality or alkalescence, and select acid as pH adjusting agent, first adjusted to ph to 1.5-6.5, then returns adjustment with alkali as pH, returns and adjusts pH to 4.2-7.2; When SILICA FUME and quartz sand mixture dispersion liquid are initially acidity, select alkali as pH adjusting agent, first adjusted to ph to 7.0-8.5, then returns adjustment with acid as pH, returns and adjusts pH to 4.2-7.2.Control silica flour dispersion liquid final ph 4.2-7.2, viscosity is at 15-400mPa.s.Return in adjust pH process, generated in-situ salt, be adsorbed on the SiO of dispersion 2solidifying grain surface, increases the mutual expelling force between particulate, effectively suppresses sedimentation and the gel tendency of silica flour dispersion liquid.General storage can extend to the 4-6 month, and without obvious sedimentation layering and gelation tendency, slurries are comparatively even, and flowing keeps.
The SILICA FUME SiO that the present invention is selected 2content more than 85%, preferably more than 90%, most preferably more than 95%, color is canescence, and granularity is very little, and median size is about 0.1 ~ 0.15 μm, in general, fineness be less than 1 μm account for more than 80%, minimum grain size about 0.01 μm.The index request of the silica flour that this patent is selected and Typical Representative, in table 1.
The silica flour index request that table 1. this patent is selected and Typical Representative
Project Index B1 N A1 A2
SiO 2％，≥ 90.0 94.0 93.5 94.0 94.6
Moisture content and volatile matter % ,≤ 2.5 2.0 2.0 2.0 1.5
Igloss % ,≤ 3.0 1.6 2.0 1.6 1.2
PH value 2.0-8.5 7.2-8.5 6.8-7.2 5.5-6.8 2.5-5.5
Granularity (45 μm tail over) % ,≤ 5.0 2.5 3.0 2.5 2.1
Tap density g/cm 3 0.2～0.45 0.32～0.36 0.27～0.35 0.34～0.39 0.27～0.35
Selected silica powder SiO 2content more than 95%.SILICA FUME accounts for the 15-50% (wt%) of liquid silicon slurry, and silica powder accounts for the 5-60% (wt%) of liquid silicon slurry.In liquid silicon dispersion liquid, solid content is 40-80% (wt%), and general control is at about 50% (wt%).
The present invention looks the acid-basicity of selected silicon power raw material, selects neutralizing acid or alkali.If silica flour is neutral and alkalescence (5% pH value of water solution >=7.0), select acid neutralization and adjusted to ph to 1.5-6.5; If silica flour is acid (5% pH value of water solution < 7.0), select alkali to neutralize and adjusted to ph to 7.0-8.5; Available acid comprises: the mineral acids such as sulfuric acid, hydrochloric acid, phosphoric acid, nitric acid, and the organic acid such as formic acid, acetic acid, citric acid.Acid regulator consumption is generally at 0-0.65%; Available alkali comprises: alkali and alkaline earth metal ions oxyhydroxide, alkaline carbonate, and alkaline earth metal oxide, and alcamines organic bases etc., alkaline conditioner consumption is generally at 0-0.65%.Selected sour or alkali, can be pre-configured to the aqueous solution of 10-50%, in use to use and to control consumption.
The present invention returns alkali tune or acid regulator optional above-mentioned alkali or acid, i.e. previous alkali neutralization adjusted to ph is adjusted to 7.0-8.5, and this step acid is returned adjust ph and returned and be adjusted to 4.2-7.2; Previous acid neutralizes and adjusted to ph is adjusted to 1.5-6.5's, and this step alkali returns adjust ph to 4.2-7.2.Return alkali tune or acid regulator consumption generally at 0-0.65%.Control the whole pH value of silica flour dispersion liquid and adjust 4.2-7.2, viscosity is at 15-400mPa.s.Return in adjust pH process, generated in-situ salt, be adsorbed on the SiO of dispersion 2solidifying grain surface, suppresses sedimentation and the gel tendency of silica flour dispersion liquid effectively.General storage can extend to the 5-6 month, and without obvious sedimentation layering and gelation tendency, slurries are comparatively even, and flowing keeps.
Reodorant of the present invention for remove due to the micro-silicon ribbon of raw material enter containing S composition, in the smelly problem of chance water.Common superoxide, hypohalite, potassium ferrate, SODIUMNITRATE etc. all can be used as reodorant and use, the preferred SPC-D of this patent, chlorinated lime.Reodorant consumption is the 0.01-0.2% of slurry, preferred 0.02-0.1%.
Liquid silicon lay up period, in especially summer, there will be smelly phenomenon, selects the sanitas such as SODIUMNITRATE, Sodium Benzoate effectively can suppress to bite the generation of vitriol bacterium, avoids smelly phenomenon.General consumption accounts for the 0.01-0.02% of slurry.
This patent can select the phosphoric acid salt such as Sodium hexametaphosphate 99, sodium pyrosulfate, tripoly phosphate sodium STPP, and acrylate homopolymer and multipolymer etc. do dispersion agent, and the general consumption of dispersion agent accounts for the 0-0.5% of slurry, and preferred dispersants is the FS20 of BASF AG; This patent also can select the thickening material of xanthan gum, cellulose family, and the inorganic thickening agent such as wilkinite, attapulgite, sepiolite is as deflocculant, and general consumption accounts for the 0-0.5% of slurry.In order to can less than 0 DEG C use in the winter time, this patent formula is optional adds antifreezing agent, and antifreezing agent is generally polyalcohols, and antifreezing agent joins in advance to be made anti frozen liquid in the water of metering and re-use.Preferred antifreezing agent is ethylene glycol, and consumption accounts for the 0-25% of slurry, preferred 10-20.0%, can more than-20 DEG C easy to use.
This patent process water can be deionized water and tap water, and preferred deionized water, to 100%.
Another object of the present invention is to provide this liquid silicon preparation method.
Time in liquid silicon formula without antifreezing agent, dispersion agent, deflocculant, preparation method comprises the following steps:
1) be put into by the 60-70% process water of metering in stirring adjustment tank T-1, the process water of another part metering is put in high speed dispersion tank T-2, opens dispersion tank T-2 high speed disperser, under 1400-3000rpm, and room temperature dispersion 5-30min;
2) adjustment tank T-1 bottom discharge valve door is opened, open the submerged pump in dispersion tank T-2 simultaneously, material in dispersion tank T-2 is pumped in adjustment tank T-1 by 40 order strainers, by regulating unlatching or the closedown of the submerged pump in adjustment tank T-1 bottom discharge valve door aperture and dispersion tank T-2, control the material liquid level in dispersion tank T-2, set up Matter Transfer;
3) Matter Transfer is kept, add reodorant and sanitas in stirring adjustment tank T-1, after 10 ~ 20min, start to add SILICA FUME and quartz sand in dispersion tank T-2, detect material liquid pH value in dispersion tank T-2, add pH value regulator in adjustment tank T-1 by miniature volume pump;
4) keep Matter Transfer, 1-2h, adds silica flour,
5) detect material liquid pH value in dispersion tank T-2, add pH and return adjustment, return and adjust control ph to 4.2-7.2, control viscosity is at 15-400mPa.s;
6) 40 mesh sieves are crossed.
The preparation method of liquid silicon of the present invention, when having antifreezing agent, dispersion agent, deflocculant in described liquid silicon formula, comprises the following steps:
1) the 60-70% process water of metering and antifreezing agent are put in stirring adjustment tank T-1, the process water of another part metering is put in high speed dispersion tank T-2, opens dispersion tank T-2 high speed disperser, under 1400-3000rpm, add dispersion agent and deflocculant, room temperature dispersion 5-30min;
2) adjustment tank T-1 bottom discharge valve door is opened, open the submerged pump in dispersion tank T-2 simultaneously, material in dispersion tank T-2 is pumped in adjustment tank T-1 by 40 order strainers, by regulating unlatching or the closedown of the submerged pump in adjustment tank T-1 bottom discharge valve door aperture and dispersion tank T-2, control the material liquid level in dispersion tank T-2, set up Matter Transfer;
3) Matter Transfer is kept, add reodorant and sanitas in stirring adjustment tank T-1, after 10 ~ 20min, start to add SILICA FUME and quartz sand in dispersion tank T-2, detect material liquid pH value in dispersion tank T-2, add pH value regulator in adjustment tank T-1 by miniature volume pump;
4) keep Matter Transfer, 1-2h, adds silica flour,
5) detect material liquid pH value in dispersion tank T-2, add pH and return adjustment, return and adjust control ph to 4.2-7.2, control viscosity is at 15-400mPa.s;
6) cross 40 mesh sieves, obtain liquid silicon of the present invention after metering packing, pH value, viscosity and the settling property of sampling and measuring liquid silicon.
The preparation method of described liquid silicon, when SILICA FUME and quartz sand mixture dispersion liquid are initially neutrality or alkalescence, select acid as pH adjusting agent, first adjusted to ph, to 1.5-6.5, is returning adjustment with alkali as pH, returns and adjusts pH to 4.2-7.2; When SILICA FUME and quartz sand mixture dispersion liquid are initially acidity, select alkali as pH adjusting agent, first adjusted to ph to 7.0-8.5, then returns adjustment with acid as pH, returns and adjusts pH to 4.2-7.2.
The preparation method of described liquid silicon, selected pH adjusting agent or pH return the aqueous solution adjusted and be pre-configured to 10-50% when using.
Beneficial effect
Compared to prior art, the invention has the advantages that:
Return in adjust pH process, generated in-situ salt, be adsorbed on the SiO of dispersion 2solidifying grain surface, increases the mutual expelling force between particulate, effectively suppresses sedimentation and the gel tendency of silica flour dispersion liquid.General storage can extend to the 5-6 month, and without obvious sedimentation layering and gelation tendency, slurries are comparatively even, and flowing keeps.
And containing sanitas, reodorant in silicon liquid of the present invention, hot environment can be adapted to and store.
Each anti-gas channeling performance of silicon liquid of the present invention can meet service requirements.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1 (comparative example)
1) 560 grams of process waters are put in high speed dispersion tank.Open dispersion tank high speed disperser, under 2800-2900rpm, add FS20 dispersion agent 5.4 grams and xanthan gum deflocculant 5.4 grams, room temperature disperses about 5min.
2) again 1120 grams of process waters are put in high speed dispersion tank, add 1680 grams of silica flour B1, open dispersion tank high speed disperser, under 2800-2900rpm, room temperature disperses about 5min, detecting pH value is 7.8, is added dropwise to 1.2 grams of sulfuric acid (30%) control ph to 6.4.
3) adjustment tank is proceeded to, stir about 1hr under 40-100rpm.
4) sampling and measuring detects pH value 6.5, and control viscosity is at 40mPa.s.
Embodiment 2
1) be put into by 1120 parts of process waters in stirring adjustment tank T-1,560 parts of process waters are put in high speed dispersion tank T-2.Open dispersion tank T-2 high speed disperser, under 2900rpm.
2) open adjustment tank T-1 to stir, under 40-60rpm, and open bottom cycle baiting valve, open submerged pump bottom dispersion tank T-2 simultaneously, by strainer, Matter Transfer is got back in adjustment tank T-1.
3) 3.5kg reodorant SPC-D and 1.5kg preservative sodium benzoate is added in stirring adjustment tank T-1.Matter Transfer about 15min, starts to add in 1680kg silica flour B1 to dispersion tank T-2, on-line checkingi pH value 7.8, adds 3.0kg hydrochloric acid (10%) control ph to 3.6 by miniature volume pump.
4) keep circulation, about 1-2hrs, adds silica flour B1.
5) on-line checkingi pH value 3.4, viscosity is at 440mPa.s, and sampling is labeled as embodiment 2A.Add 3kg soda ash by miniature volume pump, return and adjust control ph to 5.4, control viscosity is at 64mPa.s.
6) cross 40 mesh sieves, after metering packing, obtain liquid silicon of the present invention.Sampling is labeled as embodiment 2B.
Embodiment 3
1) be put into by 1120 parts of process waters in stirring adjustment tank T-1,560 parts of process waters are put in high speed dispersion tank T-2.Open dispersion tank T-2 high speed disperser, under 1400rpm.
2) open adjustment tank T-1 to stir, under about 40rpm, and open bottom cycle baiting valve, open submerged pump bottom dispersion tank T-2 simultaneously, by strainer, Matter Transfer is got back in adjustment tank T-1.
Add 6.5kg reodorant SPC-D and 3.0kg preservative sodium benzoate in stirring adjustment tank T-1.Matter Transfer about 15min, starts to add in 1680kg silica flour A1 to dispersion tank T-2, on-line checkingi pH value 3.5.
3) 28.5.0kg sodium hydroxide (10%) control ph is added to 6.8 by miniature volume pump.
4) keep circulation, about 1-2hrs, adds silica flour A1.
5) on-line checkingi pH value 6.6, viscosity is at 260mPa.s, and sampling is labeled as embodiment 3A.Add 2kg acetic acid (50%) by miniature volume pump, return and adjust control ph to 5.8, control viscosity is at 45mPa.s.
6) cross 40 mesh sieves, after metering packing, obtain liquid silicon of the present invention.Sampling is labeled as embodiment 2B.
Embodiment 4
1) by 1120 parts by water: the anti frozen liquid that ethylene glycol weight ratio 4: 1 forms is put into and stirs in adjustment tank T-1, and 560 parts by water: the anti frozen liquid that ethylene glycol weight ratio 4: 1 forms is put in high speed dispersion tank T-2.Open dispersion tank T-2 high speed disperser, under 2890rpm.
2) open adjustment tank T-1 to stir, under about 40rpm, and open bottom cycle baiting valve, open submerged pump bottom dispersion tank T-2 simultaneously, by strainer, Matter Transfer is got back in adjustment tank T-1.
3) 4.5kg reodorant SPC-D and 2.0kg preservative sodium benzoate is added in stirring adjustment tank T-1.Matter Transfer about 15min, starts to add in 1680kg silica flour A2 to dispersion tank T-2, on-line checkingi pH value 3.1, adds 32.5.0kg sodium hydroxide (10%) control ph to 7.2 by miniature volume pump.
4) keep circulation, about 1-2hrs, adds silica flour A2.
5) on-line checkingi pH value 7.0, viscosity is at 820mPa.s, and sampling is labeled as embodiment 4A.Add 3kg acetic acid (50%) by miniature volume pump, return and adjust control ph to 5.5, control viscosity is at 55mPa.s.
6) cross 40 mesh sieves, after metering packing, obtain liquid silicon of the present invention.Sampling is labeled as embodiment 4B.
Embodiment 5
1) be put into by 1120 parts of process waters in stirring adjustment tank T-1,560 parts of process waters are put in high speed dispersion tank T-2.Open dispersion tank T-2 high speed disperser, under 1400rpm.
2) open adjustment tank T-1 to stir, under about 40rpm, and open bottom cycle baiting valve, open submerged pump bottom dispersion tank T-2 simultaneously, by strainer, Matter Transfer is got back in adjustment tank T-1.
3) 3.5kg reodorant chlorinated lime and 3.0kg sanitas SODIUMNITRATE is added in stirring adjustment tank T-1.Matter Transfer about 15min, starts to add in 1680kg silica flour N to dispersion tank T-2, on-line checkingi pH value 6.5, adds 1.5.0kg sodium hydroxide (10%) control ph to 7.2 by miniature volume pump.
4) keep circulation, about 1-2hrs, adds silica flour N.
5) on-line checkingi pH value 7.0, viscosity is at 560mPa.s, and sampling is labeled as embodiment 5A.Add 2kg acetic acid (50%) by miniature volume pump, return and adjust control ph to 5.8, control viscosity is at 25mPa.s.
6) cross 40 mesh sieves, after metering packing, obtain liquid silicon of the present invention.Sampling is labeled as embodiment 5B.
The present invention is further illustrated below by comparative example.
Experiment one: liquid silicon package stability test experience.Test result is in table 2.
Table 2. liquid silicon package stability contrasts
note * outward appearance: DL-grey uniform dispersion liquid; The slight chromatography dispersion liquid of CL-grey, swim in top layer, bottom deposit is few and loose; The obvious laminar dispersion liquid of EL-grey, top layer has swims in a large number, and bottom deposit is many and closely knit; GL-grey uniform gel, stirs gently, can recover uniform dispersion; GP-grey uniform gel, firmly stirs, can not recover uniform dispersion.
#pH value: 5% aqueous solution, room temperature measuring.
Viscosity, density: stir, room temperature measuring mpa.s.
Table 2. liquid silicon package stability comparing result shows, liquid silicon embodiment 2B of the present invention, 3B, 4B, 5B keep stream preferably to become and pH stability.Return in adjust pH process, generated in-situ salt, be adsorbed on the SiO of dispersion 2solidifying grain surface, suppresses sedimentation and the gel tendency of silica flour dispersion liquid effectively.Though the nano silica particle containing massfraction about 50%, can keep good rheological and stability.General storage can extend to the 4-6 month, and without obvious sedimentation layering and gelation tendency, slurries are comparatively even, the change of viscosity, pH value is little, and embodiment 2 stores 5-6 month, only occurs slight false set (GL), stir gently, can recover uniform dispersion, flowing keeps better.
Containing reodorant and sanitas in silicon liquid of the present invention, storage can extend to the 4-6 month, and free from extraneous odour, the storage of long period can be adapted to.
Experiment two: the comprehensive characteristic test mixing the cement slurry of liquid silicon of the present invention
By contrasting each embodiment, the quiet gelling transit time of grout and SPN value compare its anti-gas channeling performance
One, experiment condition:
1, multiviscosisty condition: 120 DEG C, 60MPa, 60min
2, supercharging maintenance: 150 DEG C, 21MPa;
3, High Temperature High Pressure dehydration: 93 DEG C, 6.9MPa, 30min
4, grout basic recipe.
Two, cement-slurry method: liquid silicon+polymer water mud system, 1.90g/cm 3
100%SD " G "+35%PC-P81+35.5%F/W+0.3%PC-X603L+0.7%PC-X66L+2.5%PC-J20L+ 10%PC-GR6+5%CG80L+1.7%PC-H40L+6% embodiment liquid silicon
Three, experimental principle
Evaluate grout anti-gas channeling performance, usually have following several method:
1, cement slurry thickening time: 30BC ~ 100BC < transit time 30min
2, static gel strength: 1001b/100ft 2~ 5001b/100ft 2transit time < 30min
3, SPN value: SPN value has reacted cement slurry water loss amount and cement slurry sets process change in resistance coefficient
SPN Anti-gas channeling performance
0＜SPN＜10 Very good
10＜SPN＜21 Medium
SPN＞21 Difference
4, anti-gas channeling instrument is evaluated: the method by 1 ~ 3 is evaluated.
Four, experimental data
Table 3, fundamental property:
Table 4, anti-gas channeling performance:
Five, experimental result:
1, cement slurry thickening time: the multiviscosisty of each embodiment grout is all less than 30 minutes transit time, and transit time is all very close, close to short transient time.
2, static gel strength: the 1001b/100ft of each embodiment grout 2~ 5001b/100ft 2transit time is all less than 30 minutes, and the transit time of the liquid silicon of embodiment 2,4 is shorter; The transit time of the liquid silicon of embodiment 1,3,5 is close.
3, SPN value is all significantly less than 10, but absolute value is all very close.
4, the grout slurry of each embodiment system is stablized, and free water is zero, without sedimentation.
Consider each factor, the anti-gas channeling performance of each embodiment system is all very close, can meet service requirements.
Liquid silicon of the present invention is suspension liquid active SiO2 and water are mixed to form by special treatment process.Experimental study shows, although the nano silica particle containing massfraction about 50% in liquid silicon, can keep good rheological and stability.SiO2 particle in liquid silicon is nano-level sphere particle.Therefore, on the one hand, liquid silicon can moisture in irreducible water mud, can control the free-water in grout preferably, prevent grout in flash generation water breakthrough groove problem when horizontal cementing; On the other hand, the solid phase particles in liquid silicon can be filled between cement granules, improves cement cementitious gain in strength speed, plays good anti-gas channeling effect.Rig-site utilization shows: liquid silicon can as the toughener of the density light-weight additive of low-density cement mortar and low-temperature low-density grout; The thixotropy of grout can be improved, contribute to controlled circulation leakage and anti-gas channeling; Can as the low temperature coagulant of brine cement slurry.The application of temperature 16-204 DEG C of liquid silicon, can stop Behavior of Hardened Cement Paste hot strength to fail.

Claims (10)

1. a liquid silicon, is characterized in that, comprises SILICA FUME, quartz sand, reodorant, pH adjusting agent, and pH returns adjustment, sanitas, and each constituent mass per-cent is:
SILICA FUME 15-50%
Quartz sand 5-60%;
Reodorant 0.01-0.2%;
PH adjusting agent 0.01-0.65%;
PH returns adjustment 0.01-0.65%;
Sanitas 0.05-0.2%;
Add process water to 100%;
Described SILICA FUME SiO 2more than content 85wt%, median size is 0.1 ~ 0.15 μm; Described silica powder SiO 2more than content 95wt%; Described reodorant is selected from superoxide, hypohalite, potassium ferrate, SODIUMNITRATE; Described pH adjusting agent and described pH return adjustment and match, and are acid or alkali; Described liquid silicon returns under adding outer circulation condition by high speed dispersion adjusts the processing method of pH to obtain, and final ph is 4.2-7.2.
2. liquid silicon according to claim 1, is characterized in that, described liquid silicon also comprises dispersion agent, deflocculant, antifreezing agent, and each constituent mass per-cent is:
Dispersion agent 0-0.50%;
Deflocculant 0-0.50%;
Antifreezing agent 0-25.0%;
Described dispersion agent is selected from the phosphoric acid salt such as Sodium hexametaphosphate 99, sodium pyrosulfate, tripoly phosphate sodium STPP, and acrylate homopolymer and multipolymer; Described stablizer is selected from xanthan gum, the thickening material of cellulose family, inorganic thickening agent; Described antifreezing agent is polyvalent alcohol.
3. liquid silicon according to claim 2, it is characterized in that, described acid is selected from sulfuric acid, hydrochloric acid, phosphoric acid, nitric acid, formic acid, acetic acid, citric acid, described alkali is selected from mineral alkali or organic bases, and described mineral alkali is alkali metal hydroxide, alkaline earth metal hydroxides, alkaline carbonate or alkaline earth metal oxide; Described sanitas is selected from SODIUMNITRATE or Sodium Benzoate; Described inorganic thickening agent is selected from wilkinite, attapulgite, sepiolite; Described antifreezing agent is ethylene glycol.
4. liquid silicon according to claim 1 and 2, it is characterized in that, described returning adjusts the processing method of pH to be specially: when SILICA FUME and quartz sand mixture dispersion liquid are initially neutrality or alkalescence, select acid as pH adjusting agent, first adjusted to ph is to 1.5-6.5, return adjustment with alkali as pH again, return and adjust pH to 4.2-7.2; When SILICA FUME and quartz sand mixture dispersion liquid are initially acidity, select alkali as pH adjusting agent, first adjusted to ph to 7.0-8.5, then returns adjustment with acid as pH, returns and adjusts pH to 4.2-7.2; Described silica flour dispersion liquid final ph is 4.2-7.2, and viscosity is 15-400mPa.s.
5. liquid silicon according to claim 1 and 2, is characterized in that, described liquid SILICA FUME and quartz sand total content 40-80wt%, and described reodorant is SPC-D or chlorinated lime, and described reodorant content is 0.02-0.1wt%.
6. liquid silicon according to claim 5, is characterized in that, SILICA FUME and quartz sand total content 48-55wt% in described liquid silicon.
7. the preparation method of liquid silicon according to claim 1, is characterized in that, comprise the following steps:
1) be put into by the 60-70% process water of metering in stirring adjustment tank, the process water of another part metering is put in high speed dispersion tank, opens dispersion tank high speed disperser, under 1400-3000rpm, and room temperature dispersion 5-30min;
2) adjustment pot bottom dispensing valve is opened, open the submerged pump in dispersion tank simultaneously, material in dispersion tank is pumped in adjustment tank by 40 order strainers, by regulating unlatching or the closedown of the submerged pump in adjustment pot bottom dispensing valve aperture and dispersion tank, control the material liquid level in dispersion tank, set up Matter Transfer;
3) keeping Matter Transfer, adding reodorant and sanitas to stirring in adjustment tank, after 10 ~ 20min, start to add SILICA FUME and quartz sand in dispersion tank, detecting material liquid pH value in dispersion tank, adding pH value regulator to adjusting in tank by miniature volume pump;
4) keep Matter Transfer, 1-2h, adds silica flour,
5) detect material liquid pH value in dispersion tank, add pH and return adjustment, return and adjust control ph to 4.2-7.2, control viscosity is at 15-400mPa.s:
6) 40 mesh sieves are crossed.
8. the preparation method of liquid silicon according to claim 7, is characterized in that, when having antifreezing agent, dispersion agent, deflocculant in described liquid silicon formula, antifreezing agent adds in stirring adjustment tank together with process water; After the high speed disperser unlatching of dispersion tank, under 1400-3000rpm, add dispersion agent and deflocculant.
9. the preparation method of liquid silicon according to claim 7, is characterized in that, when SILICA FUME and quartz sand mixture dispersion liquid are initially neutrality or alkalescence, select acid as pH adjusting agent, first adjusted to ph to 1.5-6.5, then returns adjustment with alkali as pH, returns and adjusts pH to 4.2-7.2; When SILICA FUME and quartz sand mixture dispersion liquid are initially acidity, select alkali as pH adjusting agent, first adjusted to ph to 7.0-8.5, then returns adjustment with acid as pH, returns and adjusts pH to 4.2-7.2.
10. the preparation method of liquid silicon according to claim 9, is characterized in that, selected pH adjusting agent or pH return the aqueous solution adjusted and be pre-configured to 10-50% when using.
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US4321243A (en) * 1980-08-05 1982-03-23 Cornwell Charles E Method of producing stabilized aqueous dispersions of silica fume
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Publication number Priority date Publication date Assignee Title
CN110157396A (en) * 2019-05-27 2019-08-23 四川华泽石油技术股份有限公司 One kind is from leak stopping anti-channeling cementing fluid
CN110157396B (en) * 2019-05-27 2021-12-14 四川华泽石油技术股份有限公司 Self-plugging anti-channeling well cementing fluid

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