CN106753319B - A kind of method of modifying of antisludging agent to ceramsite propping agent - Google Patents
A kind of method of modifying of antisludging agent to ceramsite propping agent Download PDFInfo
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- CN106753319B CN106753319B CN201611126143.2A CN201611126143A CN106753319B CN 106753319 B CN106753319 B CN 106753319B CN 201611126143 A CN201611126143 A CN 201611126143A CN 106753319 B CN106753319 B CN 106753319B
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- 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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/80—Compositions for reinforcing fractures, e.g. compositions of proppants used to keep the fractures open
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- C—CHEMISTRY; METALLURGY
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- 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
- C09K8/52—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning
- C09K8/528—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning inorganic depositions, e.g. sulfates or carbonates
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Abstract
The scale problems that present invention is generally directed to occur in oilfield exploitation procedure carry out scale inhibition to ceramsite propping agent and are modified, and provide a kind of more convenient, stable, sustainable mitigation and antiscaling technology in situ.The preparation method is that ceramsite propping agent is carried out adsorption of modification using HEDP, ATMP or HEDP/ATMP combinational antisludging agent as primary raw material.Each material concentration are as follows: HEDP3.0-30.0mg/mL, ATMP3.0-40.0mg/mL, HEDP/ATMP3.0-30.0mg/mL.The modified ceramsite propping agent of scale inhibition prepared by the present invention combines fracturing propping agents and antisludging agent together, traditional oil-gas field development scale inhibition technique is innovated, the application field of ceramsite propping agent is expanded, have the characteristics that scale inhibition is high-efficient, the duration is long and scale inhibition performance is stablized, a large amount of antisludging agent injection environment are avoided, environmental risk is reduced.
Description
Technical field
The present invention relates to a kind of preparation methods with scale-inhibiting properties ceramsite propping agent, belong to petroleum propping agent modification technology
Field
Background technique
In recent years, the successful exploitation of U.S.'s shale oil gas has caused the exploitation upsurge of global shale petroleum resources, waterpower pressure
Technology is split also to reach its maturity therewith.Petroleum fracturing propping agent is the important filled media in hydraulic fracturing, it is therefore an objective in high pressure water
After stream presses off oil-gas Layer, supports the crack pressed off and it is made to remain open configuration, improve the permeability of oil reservoir, increase simultaneously
Oil gas well yield improves oil/gas well development benefit.Current proppant mainly has ceramsite propping agent, quartz sand and overlay film support
Agent three categories, wherein overlay film proppant is divided into precoated sand and two kinds of film-coated ceramisite again.Quartz sand proppant have density it is smaller, at
The advantages that this is lower, but its there are intensity the disadvantages of lower, easily broken, finish and sphericity are low, flow conductivity is poor, are only fitted
For burying shallower, clossing pressure and in the lower hydraulic fracturing of oil-gas Layer.And ceramsite propping agent is with of uniform size, chemical
Property is stable and quartz sand compatibility is good, the row of returning is easy, high temperature high voltage resistant, can extend the advantages that oil/gas well service life, suitable for burying
Hiding compared with deep, permeability is lower, in clossing pressure and the higher hydraulic fracturing of temperature.Therefore, both at home and abroad to the need of ceramsite propping agent
The amount of asking is continuously increased.
Country's ceramsite propping agent is mainly using bauxite as raw material at present, and using sintering process technology of preparing, but prepared by this method
Ceramsite propping agent density it is all higher, limit the formation of long slit band and the promotion of flow conductivity.And with hydraulic fracturing skill
The development of art, it is higher and higher to the performance requirement of ceramsite propping agent therefore domestic mainly to high-strength low-density proppant at present
Research and development and application carried out extensive research.
In addition to this, scale problems are also to influence a major issue of oil-gas field development economic benefit.In oil field development
In the process, fluid can flow out inside oil-gas reservoir by oil-gas Layer, and the defeated system of collection on ground is successively finally reached by pit shaft, well head
System, and variation and pressure of the incrustation ion in water flooding by oil gas water equilibrated state, temperature change etc. are influenced, and are caused
Inorganic salts dirt deposition and generate dirt.Particularly to the oil-gas field development middle and later periods, scale problems can be protruded more, development cost also phase
It should be significantly increased.It is reported that the U.S. every year because caused by ground installation and oil/gas well fouling economic loss be up to 1,000,000,000 dollars.Knot
Dirt can cause pipeline blockage, increase energy consumption, reduce oilfield yield, can lure that well pipeline locally corrodes into, cause to infuse
The leakage of water pipeline is more frequently even perforated, and pit shaft fouling can also cause the blockings such as screen casing, pump card and down-hole string, makes to monitor
Instrument and power tool are unable to operate normally.The more and more oil fields in China enter mid-later development phase, fouling bring economy
Efficiency problem also becomes increasingly conspicuous.
Currently, the processing technique for oilfield scales includes physical method, chemical method and Process etc..Wherein physical scale inhibition skill
Art investment is smaller, but technology is immature, and carry out antiscale cannot still be used alone；Technique antiscaling effect is undesirable, chemical scale-inhibitor
Invest less, effect is preferable, is the main means of oil field antiscale.But in practical applications, interval dosing method scale inhibition performance is with adding
The medicine period is fluctuated up and down, and equipment investment need to be increased by continuously pumping note dosing technique, and stratum squeezing technique needs special medical fluid, and dosage
Greatly, costly.It is therefore desirable to seek a kind of convenience, economy, efficient oil field mitigation and antiscaling technology.
Most popular in oil field at present is organic phosphine acids antisludging agent, mainly (referred to as with aminotrimethylenephosphonic acid
ATMP) and based on 1-hydroxy ethylidene-1,1-diphosphonic acid (abbreviation HEDP), both antisludging agents are still widely used so far.Therefore, for current
Scale problems in oilfield development process, it is modified that the present invention carries out scale inhibition to ceramsite propping agent for the first time, and to antisludging agent type and
Its scale inhibition performance etc. is studied, which can realize the scale inhibition in situ of oil field development, improves its economic benefit.
Summary of the invention
The scale problems that present invention is generally directed to occur in oilfield exploitation procedure carry out scale inhibition to ceramsite propping agent and change
Property, a kind of more convenient, stable, sustainable mitigation and antiscaling technology in situ is provided.
The present invention is with antisludging agent 1-hydroxy ethylidene-1,1-diphosphonic acid (abbreviation HEDP) common in current oil field and amino trimethylene methene
Phosphonic acids (abbreviation ATMP) is modified ceramsite propping agent, method particularly includes:
With scale-inhibiting properties ceramsite propping agent preparation process, characterized in that
1. preparation method described in is using HEDP, ATMP or HEDP/ATMP combinational antisludging agent as primary raw material, by haydite branch
It supports agent and carries out adsorption of modification.Each material concentration are as follows: HEDP 3.0-30.0mg/mL, ATMP 3.0-40.0mg/mL, HEDP/
ATMP 3.0-30.0mg/mL.10.0-50.0g ceramsite propping agent is placed in conical flask, it is molten that certain density antisludging agent is added
Liquid is allowed to flood proppant, after 40~80 DEG C of water-baths preheat 10~30min, oscillating reactions 1.0 under the conditions of 50~300r/min
~6.0h, then takes out haydite, with deionized water flushing 3~4 times, is after 80~110 DEG C of 0.5~4.0h of electric heating forced air drying
Obtain the modified ceramsite propping agent of scale inhibition.
Each material concentration is preferred in above-mentioned reaction: HEDP 10.0-25.0mg/mL, ATMP 15.0-30.0mg/mL,
HEDP/ATMP 10.0-20.0mg/mL；
Ceramsite propping agent dosage is preferred in above-mentioned reaction: 10.0-20.0g；
HEDP is compounded with ATMP than preferred in above-mentioned reaction: 3: 2
Preferred 50-60 DEG C of temperature in above-mentioned reaction；
The preferred 100-200r/min of oscillating reactions speed in above-mentioned reaction, oscillating reactions time preferred 3-5h；
Preferred 90-110 DEG C of drying temperature in above-mentioned reaction, drying time preferred 2-3h；
The modification ceramsite propping agent scale inhibition efficiency of above-mentioned reaction preparation is up to 30%~90%；
Beneficial effect
Compared with prior art, the invention has the following beneficial effects:
1. the modified ceramsite propping agent of scale inhibition prepared by the present invention combines fracturing propping agents and antisludging agent together, biography has been innovated
The oil-gas field development scale inhibition technique of system, has expanded the application field of ceramsite propping agent；
2. the modified ceramsite propping agent of scale inhibition prepared by the present invention can realize scale inhibition in situ, reduce in oilfield exploitation procedure because
The expenses such as medicament, the equipment for preventing fouling from generating, can reduce capital investment, and can realize industrialized production, have warp well
Benefit of helping and social benefit；
3. antisludging agent original position slow release can be had scale inhibition efficiency by the modified ceramsite propping agent of scale inhibition prepared by the present invention
The features such as height, duration length and scale inhibition performance are stablized avoids a large amount of antisludging agents injection environment, reduces environmental risk.
The feature of ceramsite propping agent
The basic parameter of 3.1 ceramsite propping agent of table
Material phase analysis is carried out to haydite using German Brooker company D8 ADVANCE type x-ray diffractometer (XRD)；
Fig. 1 is ceramsite propping agent XRD material phase analysis figure, and as seen from the figure, most of crystal phase of ceramsite propping agent is corundum, together
Shi Hanyou a small amount of mullite and few quartz belong to high density proppants, and clossing pressure is higher, it is suitable for 3600~
The hydraulic fracturing of 5000m.
The influence of antisludging agent type and concentration to scale inhibition efficiency
Calcium ion concentration in solution is measured according to GB 7476-87 " water quality calcium catalyst EDTA titration "；
Antisludging agent is measured according to GBT16632-2008 " measurement of water treatment agent scale-inhibiting properties --- tosca method "
Scale inhibition efficiency；
Water treatment agent scale inhibition performance (static scale inhibition method) is calculated as follows:
In formula
ρ 4 --- the concentration of Ca2+ after water treatment agent ATMP solution, unit mg/mL is added；
ρ 3 --- the concentration of Ca2+ in water treatment agent blank solution, unit mg/mL are not added；
0.240 --- test the concentration of Ca2+ in preceding configured test solution, unit mg/mL；
Fig. 2 is influence of antisludging agent ATMP, HEDP concentration to scale inhibition efficiency.ATMP can form stabilization with calcium ion in water
Soluble chelating object, make salt solubility increase, inhibit the precipitating and growth of scale, particularly with calcium carbonate scale influence pole
Greatly, and ATMP will not react generation novel substance under the action of water, be not easy to chemically react with other materials.It can by figure
Know, with the increase of ATMP concentration, scale inhibition efficiency is gradually risen, and after concentration reaches 15mg/L, scale inhibition performance increase rate becomes
Slow, when the concentration of ATMP is 40mg/L, scale inhibition performance can reach 83.6%.
The hydroxyl that HEDP contains easily forms hydrogen bond between calcium carbonate, to strengthen the inhibitory effect to dirt growth, especially
It has good inhibiting effect to the calcite in calcium carbonate crystal.Resistance still can be played under stable and high temperature with property under high ph-values
The characteristics of dirt effect.As shown in Figure 2, similar to ATMP, with the increase of concentration, scale inhibition efficiency is gradually risen.When HEDP's
When concentration is 15mg/L, scale inhibition performance increase rate starts to slow down, and when HEDP concentration is 40mg/L, scale inhibition performance can reach 87.2%,
Scale inhibition efficiency is better than ATMP.
Fig. 3 is HEDP and influence of the ATMP compound proportion to scale inhibition efficiency.As seen from the figure, under the conditions of same compound proportion,
Scale inhibition performance gradually rises with the increase of combinational antisludging agent concentration.Change mixing antisludging agent composition, comparison HDEP/ATMP is 2/
3,1/1,3/2 when scale inhibition efficiency can obtain, when inhibitor concentration be 30mg/L, HEDP/ATMP concentration proportioning be 3/2 when scale inhibition
For rate up to 87.7%, scale inhibition efficiency is higher than 2/3 and 1/1, and is better than the single antisludging agent scale inhibition effect of same concentrations.
Influence of the preparation condition to modified ceramsite propping agent scale-inhibiting properties
Fig. 4 is influence of the inhibitor concentration to modified ceramsite propping agent scale inhibition efficiency.As seen from the figure, with single antisludging agent phase
Than the modified ceramsite propping agent of combinational antisludging agent scale inhibition efficiency with higher is real when inhibitor concentration is 6mg/mL
Scale inhibition performance is up to 62.2% under the conditions of testing.
Detailed description of the invention
Attached drawing 1 is ceramsite propping agent XRD material phase analysis figure.
Attached drawing 2 is influence of antisludging agent ATMP, HEDP concentration to scale inhibition efficiency.
Attached drawing 3 is HEDP and influence of the ATMP compound proportion to scale inhibition efficiency.
Influence of 4 inhibitor concentration of attached drawing to modified haydite scale inhibition efficiency.
Specific embodiment
Embodiment 1:
10.0g ceramsite propping agent is taken to be placed in 100mL conical flask, the HEDP solution that 30mL concentration is 6.0mg/mL, which is added, to be made
Flood proppant, 50 DEG C of water-baths preheat 15min, adjust hunting speed 100r/min, oscillating reactions 4.0h.Haydite is taken out, with
Deionized water is rinsed 3~4 times, and filter paper blots surface moisture, and dry 2.0h, is cooled to room temperature in 105 DEG C of electric drying oven with forced convections
Afterwards up to the modified ceramsite propping agent of scale inhibition.
Embodiment 2:
10.0g ceramsite propping agent is taken to be placed in 100mL conical flask, the ATMP solution that 30mL concentration is 6.0mg/mL, which is added, to be made
Flood proppant, 50 DEG C of water-baths preheat 15min, adjust hunting speed 100r/min, oscillating reactions 4.0h.Haydite is taken out, with
Deionized water is rinsed 3~4 times, and filter paper blots surface moisture, and dry 2.0h, is cooled to room temperature in 105 DEG C of electric drying oven with forced convections
Afterwards up to the modified ceramsite propping agent of scale inhibition.
Embodiment 3:
10.0g ceramsite propping agent is taken to be placed in 100mL conical flask, it is 6.0mg/mL, HEDP/ that 30mL total concentration, which is added,
The solution that ATMP concentration ratio is 2: 3 is allowed to flood proppant, and 50 DEG C of water-baths preheat 15min, adjusts hunting speed 100r/min, vibration
Swing reaction 4.0h.Haydite is taken out, with deionized water flushing 3~4 times, filter paper blots surface moisture, in 105 DEG C of electric heating forced air dryings
Dry 2.0h in case is cooled to after room temperature up to the modified ceramsite propping agent of scale inhibition.
Embodiment 4:
10.0g ceramsite propping agent is taken to be placed in 100mL conical flask, it is 6.0mg/mL, HEDP/ that 30mL total concentration, which is added,
The solution that ATMP concentration ratio is 1: 1 is allowed to flood proppant, and 50 DEG C of water-baths preheat 15min, adjusts hunting speed 100r/min, vibration
Swing reaction 4.0h.Haydite is taken out, with deionized water flushing 3~4 times, filter paper blots surface moisture, in 105 DEG C of electric heating forced air dryings
Dry 2.0h in case is cooled to after room temperature up to the modified ceramsite propping agent of scale inhibition.
Embodiment 5:
10.0g ceramsite propping agent is taken to be placed in 100mL conical flask, it is 6.0mg/mL, HEDP/ that 30mL total concentration, which is added,
The solution that ATMP concentration ratio is 3: 2 is allowed to flood proppant, and 50 DEG C of water-baths preheat 15min, adjusts hunting speed 100r/min, vibration
Swing reaction 4.0h.Haydite is taken out, with deionized water flushing 3~4 times, filter paper blots surface moisture, in 105 DEG C of electric heating forced air dryings
Dry 2.0h in case is cooled to after room temperature up to the modified ceramsite propping agent of scale inhibition.
Embodiment 6:
Take 10.0g ceramsite propping agent, with 50% sulfuric acid solution impregnate 17h, to surface carry out acidification, then with go from
Sub- water rinses, until flushing water switchs to neutrality, the acidified modified ceramsite propping agent in surface is dried to obtain in air blast under the conditions of 110 DEG C.
The modified proppant of acid is placed in 100mL conical flask, addition 30mL total concentration is 6.0mg/mL, and HEDP/ATMP concentration ratio is
3: 2 solution is allowed to flood proppant, and 50 DEG C of water-baths preheat 15min, adjust hunting speed 100r/min, oscillating reactions 4.0h.
Haydite is taken out, with deionized water flushing 3~4 times, filter paper blots surface moisture, dry in 105 DEG C of electric drying oven with forced convections
2.0h is cooled to after room temperature up to the modified ceramsite propping agent of scale inhibition.Scale inhibition is modified again after the acidification of surface, ceramsite propping agent resistance
Dirty efficiency reduces by 60%, therefore is not suitable for such ceramsite propping agent.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (9)
1. a kind of antisludging agent method modified to ceramsite propping agent, characterized in that the method for modifying be with HEDP, ATMP or
HEDP/ATMP combinational antisludging agent is primary raw material, and ceramsite propping agent is carried out adsorption of modification；Each material concentration are as follows: HEDP3.0-
30.0mg/mL or ATMP3.0-40.0mg/mL or HEDP/ATMP3.0-30.0mg/mL；
Specific preparation method is: 10.0-50.0g ceramsite propping agent being placed in conical flask, it is molten that certain density antisludging agent is added
Liquid is allowed to flood proppant, after 40~80 DEG C of water-baths preheat 10~30min, oscillating reactions 1.0 under the conditions of 50~300r/min
~6.0h, then takes out haydite, with deionized water flushing 3~4 times, is after 80~110 DEG C of 0.5~4.0h of electric heating forced air drying
Obtain the modified ceramsite propping agent of scale inhibition.
2. according to the method described in claim 1, it is characterized in that reaction in each material concentration are as follows: HEDP10.0-25.0mg/mL
Or ATMP15.0-30.0mg/mL or HEDP/ATMP10.0-20.0mg/mL.
3. according to the method described in claim 1, it is characterized in that ceramsite propping agent dosage is 10.0-20.0g in reaction.
4. according to the method described in claim 1, it is characterized in that HEDP is compounded with ATMP than being 3: 2 in reaction.
5. according to the method described in claim 1, it is characterized in that temperature is 50-60 DEG C in reaction.
6. according to the method described in claim 1, it is characterized in that oscillating reactions speed is 100-200r/min, oscillation in reaction
Reaction time is 3-5h.
7. according to the method described in claim 1, it is characterized in that reaction in drying temperature be 90-110 DEG C, drying time 2-
3h。
8. a kind of antisludging agent method modified to ceramsite propping agent, characterized in that 10.0g ceramsite propping agent is taken to be placed in 100mL cone
In shape bottle, the HEDP solution that 30mL concentration is 6.0mg/mL is added and is allowed to flood proppant, 50 DEG C of water-baths preheat 15min, adjust
Hunting speed 100r/min, oscillating reactions 4.0h take out haydite, and with deionized water flushing 3~4 times, filter paper blots surface moisture,
The dry 2.0h in 105 DEG C of electric drying oven with forced convections is cooled to after room temperature up to the modified ceramsite propping agent of scale inhibition.
9. a kind of antisludging agent method modified to ceramsite propping agent, characterized in that 10.0g ceramsite propping agent is taken to be placed in 100mL cone
In shape bottle, the ATMP solution that 30mL concentration is 6.0mg/mL is added and is allowed to flood proppant, 50 DEG C of water-baths preheat 15min, adjust
Hunting speed 100r/min, oscillating reactions 4.0h take out haydite, and with deionized water flushing 3~4 times, filter paper blots surface moisture,
The dry 2.0h in 105 DEG C of electric drying oven with forced convections is cooled to after room temperature up to the modified ceramsite propping agent of scale inhibition.
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| CN109943315B (en) * | 2019-03-21 | 2021-09-28 | 中国石油天然气股份有限公司 | Scale inhibition proppant and preparation method thereof |
| CN111621284A (en) * | 2020-06-05 | 2020-09-04 | 西南石油大学 | Water-control scale-inhibition coated proppant and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102250604A (en) * | 2011-05-27 | 2011-11-23 | 门正国 | Controlled releasing microcapsule for scale prevention, wax prevention or viscosity reduction of oil well |
| CN105038758A (en) * | 2015-07-13 | 2015-11-11 | 洛阳赛罗帕陶瓷科技有限公司 | Porous petroleum fracturing propping agent and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102250604A (en) * | 2011-05-27 | 2011-11-23 | 门正国 | Controlled releasing microcapsule for scale prevention, wax prevention or viscosity reduction of oil well |
| CN105038758A (en) * | 2015-07-13 | 2015-11-11 | 洛阳赛罗帕陶瓷科技有限公司 | Porous petroleum fracturing propping agent and preparation method thereof |
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