CN105017478B - A kind of high temperature resistance, anti-high salt concentration flow pattern regulator and preparation method thereof - Google Patents
A kind of high temperature resistance, anti-high salt concentration flow pattern regulator and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses a kind of high temperature resistance being used in oil and gas drilling fluid, anti-high salt concentration flow pattern regulator, and the flow pattern regulator is by four kinds of monomers:N, N DMAAs, the methyl propane sulfonic acid of 2 acrylamido 2, acrylamide and acrylic acid are under a kind of effect of crosslinking agent, a kind of crosslinking copolymerization thing blob of viscose of space net structure molecule is cross-linked to form in copolymerization, blob of viscose sodium hydroxide solution neutralizing hydrolysis, obtain the sulfonate sodium and carboxylic acid sodium salt of crosslinking copolymerization thing micelle, by 120 DEG C of dryings, crush, that is, prepare crosslinking copolymerization into flow pattern regulator spatial networks macromolecular.Contain organic sulfonic group CH in its structure of the flow pattern regulator of the present invention2SO3 ‑With branched alkyl CH3, both high temperature resistances, and anti-high salt concentration, in high temperature(120℃)And high salt(Saturated brine)The solution of lower configuration has higher viscosity, good with other inorganic agent compatibilities, and preparation method is simple, and raw material is easy to get, moderate cost.
Description
Technical field
The present invention relates to a kind of drilling fluid flow pattern regulator, specifically a kind of high temperature resistance, anti-high salt concentration flow pattern regulator,
Belong to petroleum drilling technology field.
Background technology
High density drilling fluid can push down stratum, safeguard that wellbore stability prevents the generation of the accidents such as overflow, blowout, therefore,
High density drilling fluid has particularly significant meaning for the exploration and development of deep formation oil-gas reservoir.
But in hp-ht well drilling process, the flow pattern regulation of high density drilling fluid is a problem.On the one hand, due to
Solid concentration in high density drilling fluid is high, under the high temperature conditions the rheological characteristic of drilling fluid not easy-regulating, it is difficult to which satisfaction takes sand will
Ask, on the other hand, the contamination resistance of high density drilling fluid is poor, and when running into saline bed, its rheological characteristic easily deteriorates.It is high to improve
Rheological characteristic of the density drilling fluid under the conditions of high temperature and high salt, often adds high temperature resistance, the regulation of anti-high salt concentration flow pattern in drilling fluid
Agent.
Conventional flow pattern regulator includes polysaccharide, and such as biopolymer XC is in single yellow born of the same parents by polysaccharide natural goods
Produced under bacillus enzyme effect, ehter bond-C-O-C- keys are contained on its main chain, at high temperature easy fracture, its high-temperature resistance is poor;Separately
One class is alkenyl monomer copolymer analog, and its main chain is-C-C- chains, and high-temperature resistance is strong, but its hydrophilic radical is carboxyl, nitrile
Base-CN and amide groups, these group saline-alkaline tolerances are poor.
Therefore, offer one kind is provided badly and is provided simultaneously with high temperature resistance, anti-high salt concentration performance, can be improved under the conditions of high temperature and high salt
The flow pattern regulator of rheological performance of high-density drilling fluid.
The content of the invention
It is an object of the invention to provide one kind with 2- acrylamide-2-methylpro panesulfonic acids, N, N- DMAAs,
Acrylamide, four kinds of monomers of acrylic acid and a kind of high temperature resistance of crosslinking agent crosslinking copolymerization, anti-high salt concentration flow pattern regulator,
The flow pattern regulator can improve the rheological property of high density drilling fluid under the conditions of high temperature and high salt, improve conventional high-density drilling fluid
High temperature resistance, saline-alkaline tolerance, and compatibility is good.
The present invention also aims to provide a kind of preparation method of above-mentioned flow pattern regulator.
Technical scheme is as follows:A kind of high temperature resistance, anti-high salt concentration flow pattern regulator, are by 2- acrylamides
Base -2- methyl propane sulfonic acids, N, N- DMAAs, acrylamide, acrylic acid and crosslinking agent are by weight 2 ~ 3:1~2:1:
0.8~1.6:0.02 ~ 0.06 crosslinking copolymerization is formed;During preparation, using following steps:
(1)The sodium hydroxide solution of mass concentration 40% is configured to sodium hydroxide and distilled water, it is standby;
(2)Take the distilled water of 8 ~ 12 times of acrylamide quality to be placed in reaction vessel, sequentially add 2- acrylamidos -2-
Methyl propane sulfonic acid, N,N-DMAA, acrylamide, acrylic acid, crosslinking agent, are sufficiently stirred for 1 ~ 2 hour, make its abundant
Dissolving, adds redox initiator, reacts 25 ~ 35 minutes, and temperature rises to 90 DEG C, is kept for 1 ~ 2 hour, natural cooling makes temperature
50 DEG C are down to, crosslinking copolymerization thing blob of viscose is obtained, blob of viscose is granulated with comminutor, obtain copolymer micelle;
(3)Copolymer micelle is mixed with the sodium hydroxide solution of mass concentration 40%, is stirred continuously at 80 DEG C, is neutralized
Hydrolysis 2 ~ 3 hours, be then made the conditioning agent with spatial networks macromolecular structure by product in 120 DEG C of dryings, crushing;
Wherein, the crosslinking agent is methene base bisacrylamide;The redox initiator is ferrous sulfate or tertiary fourth
Base hydrogen peroxide.
It is preferred that, the 2- acrylamide-2-methylpro panesulfonic acids, N,N-DMAA, acrylamide, propylene
Acid, the weight ratio of crosslinking agent are 2.93:1.40:1:1.01:0.04.
It is preferred that, the 2- acrylamide-2-methylpro panesulfonic acids, N,N-DMAA, acrylamide, propylene
Acid, the molecular proportion of crosslinking agent are 1:1:1:1:0.011.
The optimal technical scheme of the present invention is as follows:The conditioning agent is the raw material preparation by following quality proportioning:2- propylene
Amide groups -2- methyl propane sulfonic acid 73.8g, N,N-DMAA 35.3g, acrylamide 25.2g, acrylic acid
25.2g, crosslinking agent 1.0g, redox initiator 0.4g, distilled water 322.7ml, sodium hydroxide 55.1g;Its preparation side
Method uses following steps:
(1)Sodium hydroxide is taken to be made into the sodium hydroxide solution of mass concentration 40% with distilled water 82.7ml;
(2)Distilled water 240mL is taken, in the reactor for the liner temperature resistance plastics polytetrafluoroethylene (PTFE) for adding 1 liter of volume, 2- is added
Acrylamide-2-methylpro panesulfonic acid, N,N-DMAA, acrylamide, acrylic acid, crosslinking agent, with rotating speed 100 ~
600r/min is sufficiently stirred for 1 hour, makes after raw material fully dissolves, to add redox initiator, react 30 minutes, temperature rises to
90 DEG C, in the temperature 1 hour, 50 DEG C are naturally cooled to, crosslinking copolymerization thing blob of viscose is obtained, whole blob of viscoses is granulated with blob of viscose
Machine is granulated, and obtains copolymer micelle;
(3)By copolymer micelle and step(1)The sodium hydroxide solution of configuration, is stirred continuously at 80 DEG C, neutralizes, hydrolyzes
2 hours, then product is made in 120 DEG C of dryings, crushing.
Having the beneficial effect that relative to prior art of the invention:The flow pattern regulator of the present invention is employed to be handed in copolymerization
The thinking of connection is synthesized, and is synthesized with four kinds of monomers and a kind of crosslinking agent, and under crosslinking agent effect, four kinds of monomers are handed in copolymerization
Connection forms a kind of crosslinking copolymerization thing blob of viscose of space net structure molecule, and blob of viscose sodium hydroxide solution neutralizing hydrolysis is total to
The sulfonate sodium and carboxylic acid sodium salt of poly- cross-linking agent micelle, by 120 DEG C of dryings, crush, that is, prepare crosslinking copolymerization into flow pattern
Conditioning agent spatial networks macromolecular;Its formula of the flow pattern regulator and preparation method are simple, and raw material is easy to get, moderate cost, due to
Contain organic sulfonic group-CH in its structure2SO3 -With branched alkyl-CH3, therefore ensure its both high temperature resistance, and anti-high salt concentration,
High temperature(120℃)And high salt(Saturated brine)The solution of lower configuration has higher viscosity, in drillng operation, with other places
Manage agent compatibility good.
Embodiment
The present invention is described in further details below by embodiment, these embodiments are only used for illustrating the present invention, and
Do not limit the scope of the invention.
Embodiment 1 prepares a kind of high temperature resistance, anti-high salt concentration flow pattern regulator as follows:
1st, by weight 2.93:1.40:1:1.01:0.04 prepares four kinds of monomers and crosslinking agent raw material:2- acrylamidos-
2- methyl propane sulfonic acid 73.8g, N,N-DMAA 35.3g, acrylamide 25.2g, acrylic acid 25.2g, methene base
Bisacrylamide 1.0g, ferrous sulfate 0.4g, distilled water 322.7ml, sodium hydroxide 55.1g;
2nd, preparation process:
(1)Sodium hydroxide is taken to be made into the sodium hydroxide solution of mass concentration 40% with distilled water 82.7ml;
(2)Distilled water 240mL is taken, in the reactor for the liner temperature resistance plastics polytetrafluoroethylene (PTFE) for adding 1 liter of volume, 2- is added
Acrylamide-2-methylpro panesulfonic acid, N,N-DMAA, acrylamide, acrylic acid, methene base bisacrylamide,
It is sufficiently stirred for 1 hour with rotating speed 100r/min, makes after raw material fully dissolves, to add TBHP, after 5 minutes, copolymerization
Cross-linking reaction starts, and reaction is exothermic reaction, and temperature gradually rises, and after reacting 30 minutes, temperature rises to 90 DEG C, is protected in the temperature
Temperature 1 hour, natural cooling after one hour temperature be reduced to 50 DEG C, obtain crosslinking copolymerization thing blob of viscose, whole blob of viscoses made with blob of viscose
Grain machine granulation, obtains copolymer micelle;
(3)By copolymer micelle and step(1)The sodium hydroxide solution of configuration, is stirred continuously at 80 DEG C, neutralizes, hydrolyzes
2 hours, crosslinking copolymerization thing sulfonate sodium, carboxylic acid sodium salt micelle are obtained, product is then made sky in 120 DEG C of dryings, crushing
Between net macromolecular structure flow pattern regulator.
The viscosity of the flow pattern regulator for preparing in different systems is measured with shear force:
(1)Determine its viscosity and shear force in distilled water:Determination step is:350ml distilled water is taken, in 500-
Stirring adds 1.75g flow pattern regulators under 1000rpm, is then stirred 20 minutes under 11000rpm rotating speeds, viscous in six speed rotations
The viscosity and shear force of this solution are determined on degree meter;
(2)Survey its viscosity and shear force in 4% salt solution:Determination step is:350ml distilled water is taken, 14.0g is added
NaCl, is stirred 20 minutes under 11000rpm rotating speeds, and this solution is 4% salt solution;It is accurate to measure the salt solution of 350ml 4%, add 3.5 g
Flow pattern regulator, is stirred 20 minutes under 11000rpm rotating speeds, and the viscosity of this solution is determined with cutting on six fast rotation viscometers
Power;
(3)Determine its viscosity and shear force in saturated brine:Determination step is as follows:350ml distilled water is taken, is added
122.5 g NaCl, are stirred 20 minutes under 11000rpm rotating speeds, and this solution is saturated brine;Accurately measure 350ml saturated salts
Water, adds 3.5 g flow pattern regulators, is stirred 20 minutes under 11000rpm rotating speeds, and it is molten to determine this on six fast rotation viscometers
The viscosity and shear force of liquid;
(4)Determine its viscosity and shear force in 100%Weigh3 solution:Determination step is as follows:350ml distilled water is taken, plus
Enter 350 g Weigh3, high-speed stirred 20 minutes, this solution is 100%Weigh3 solution;Accurately measure 350ml100%Weigh3
Solution, adds 3.5 g flow pattern regulators, and high-speed stirred 20 minutes determines the viscosity of this solution on the fast viscosimeters of FANNShi six
With shear force.
After being determined through above-mentioned steps, the flow pattern regulator is in distilled water, 4% salt solution, saturated brine, 100%Weigh3 solution
In viscosity and shear force it is as shown in the table:
。
Embodiment 2 prepares a kind of high temperature resistance, anti-high salt concentration flow pattern regulator as follows:
(1)By weight 3:1.6:1:1.05:0.05 prepares four kinds of monomers:2- acrylamide-2-methylpro panesulfonic acids, N,
N- DMAAs, acrylamide, acrylic acid and methene base bisacrylamide;
(2)Sodium hydroxide is taken, it is standby with the sodium hydroxide solution of distilled water configuration quality concentration 40%;
(3)Take the distilled water of 10 times of acrylamide quality to be placed in reaction vessel, sequentially add 2- acrylamido -2- first
Base propane sulfonic acid, N,N-DMAA, acrylamide, acrylic acid, methene base bisacrylamide, rotating speed 400r/min are abundant
Stirring 1 hour, makes it fully dissolve, and adds ferrous sulfate, reacts 35 minutes, and temperature rises to 90 DEG C, is kept for 1 hour, naturally cold
But temperature is down to 50 DEG C, obtain crosslinking copolymerization thing blob of viscose, blob of viscose is granulated with comminutor, obtain copolymer micelle;
(3)Copolymer micelle is mixed with the sodium hydroxide solution of mass concentration 40%, is stirred continuously at 80 DEG C, is neutralized
Hydrolysis 2.2 hours, be then made the conditioning agent with spatial networks macromolecular structure by product in 120 DEG C of dryings, crushing.
Embodiment 3 prepares a kind of high temperature resistance, anti-high salt concentration flow pattern regulator as follows:
(1)By weight 2:1:1:0.8:0.02 prepares four kinds of monomers:2- acrylamide-2-methylpro panesulfonic acids, N, N-
DMAA, acrylamide, acrylic acid and methene base bisacrylamide;
(2)Sodium hydroxide is taken, it is standby with the sodium hydroxide solution of distilled water configuration quality concentration 40%;
(3)Take the distilled water of acrylamide quality 8 to be placed in reaction vessel, sequentially add 2- acrylamido -2- methyl
Propane sulfonic acid, N,N-DMAA, acrylamide, acrylic acid, methene base bisacrylamide, rotating speed 600r/min are fully stirred
Mix 1.5 hours, it is fully dissolved, add TBHP, react 25 minutes, temperature rises to 90 DEG C, and holding 1.2 is small
When, natural cooling makes temperature be down to 50 DEG C, obtains crosslinking copolymerization thing blob of viscose, blob of viscose is granulated with comminutor, obtain copolymer micelle;
(3)Copolymer micelle is mixed with the sodium hydroxide solution of mass concentration 40%, is stirred continuously at 80 DEG C, is neutralized
Hydrolysis 2.5 hours, be then made the conditioning agent with spatial networks macromolecular structure by product in 120 DEG C of dryings, crushing.
Embodiment 4 prepares a kind of high temperature resistance, anti-high salt concentration flow pattern regulator as follows:
(1)By weight 2.5:1.5:1:1.0:0.04 prepares four kinds of monomers:2- acrylamide-2-methylpro panesulfonic acids,
N, N- DMAA, acrylamide, acrylic acid and methene base bisacrylamide;
(2)Sodium hydroxide is taken, it is standby with the sodium hydroxide solution of distilled water configuration quality concentration 40%;
(3)Take the distilled water of 9 times of acrylamide quality to be placed in reaction vessel, sequentially add 2- acrylamido -2- first
Base propane sulfonic acid, N,N-DMAA, acrylamide, acrylic acid, methene base bisacrylamide, rotating speed 200r/min are abundant
Stirring 2 hours, makes it fully dissolve, and adds ferrous sulfate, reacts 30 minutes, and temperature rises to 90 DEG C, is kept for 1.5 hours, natural
Cooling makes temperature be down to 50 DEG C, obtains crosslinking copolymerization thing blob of viscose, blob of viscose is granulated with comminutor, obtain copolymer micelle;
(3)Copolymer micelle is mixed with the sodium hydroxide solution of mass concentration 40%, is stirred continuously at 80 DEG C, is neutralized
Hydrolysis 2.5 hours, be then made the conditioning agent with spatial networks macromolecular structure by product in 120 DEG C of dryings, crushing.
Embodiment 5 prepares a kind of high temperature resistance, anti-high salt concentration flow pattern regulator as follows:
(1)By weight 3: 2:1:0.8:0.06 prepares four kinds of monomers:2- acrylamide-2-methylpro panesulfonic acids, N, N-
DMAA, acrylamide, acrylic acid and methene base bisacrylamide;
(2)Sodium hydroxide is taken, it is standby with the sodium hydroxide solution of distilled water configuration quality concentration 40%;
(3)Take the distilled water of 12 times of acrylamide quality to be placed in reaction vessel, sequentially add 2- acrylamido -2- first
Base propane sulfonic acid, N,N-DMAA, acrylamide, acrylic acid, methene base bisacrylamide, rotating speed 500r/min are abundant
Stirring 2 hours, makes it fully dissolve, and adds TBHP, reacts 30 minutes, and temperature rises to 90 DEG C, is kept for 2 hours,
Natural cooling makes temperature be down to 50 DEG C, obtains crosslinking copolymerization thing blob of viscose, blob of viscose is granulated with comminutor, obtain copolymer micelle;
(3)Copolymer micelle is mixed with the sodium hydroxide solution of mass concentration 40%, is stirred continuously at 80 DEG C, is neutralized
Hydrolysis 3 hours, be then made the conditioning agent with spatial networks macromolecular structure by product in 120 DEG C of dryings, crushing.
Claims (5)
1. a kind of high temperature resistance, anti-high salt concentration flow pattern regulator, it is characterised in that:Prepared by the raw material of following quality proportioning:2-
Acrylamide-2-methylpro panesulfonic acid 73.8g, N,N-DMAA 35.3g, acrylamide 25.2g, acrylic acid
25.2g, crosslinking agent 1.0g, redox initiator 0.4g, distilled water 322.7ml, sodium hydroxide 55.1g;Its preparation side
Method uses following steps:
(1)Sodium hydroxide is taken to be made into the sodium hydroxide solution of mass concentration 40% with distilled water 82.7ml;
(2)Distilled water 240mL is taken, in the reactor for the liner temperature resistance plastics polytetrafluoroethylene (PTFE) for adding 1 liter of volume, 2- propylene is added
Amide groups -2- methyl propane sulfonic acids, N,N-DMAA, acrylamide, acrylic acid, crosslinking agent, with 100 ~ 600r/ of rotating speed
Min is sufficiently stirred for 1 hour, makes after raw material fully dissolves, to add redox initiator, react 30 minutes, temperature rises to 90 DEG C,
In the temperature 1 hour, 50 DEG C are naturally cooled to, crosslinking copolymerization thing blob of viscose is obtained, whole blob of viscoses is made with blob of viscose comminutor
Grain, obtains copolymer micelle;
(3)By copolymer micelle and step(1)The sodium hydroxide solution of configuration, is stirred continuously at 80 DEG C, neutralizes, to hydrolyze 2 small
When, then product is made in 120 DEG C of dryings, crushing.
2. a kind of high temperature resistance, anti-high salt concentration flow pattern regulator, it is characterised in that:Prepared using following steps:
(1)By weight 3:1.6:1:1.05:0.05 prepares four kinds of monomers and crosslinking agent:2- acrylamido -2- methyl-prop sulphurs
Acid, N, N- DMAAs, acrylamide, acrylic acid and methene base bisacrylamide;
(2)Sodium hydroxide is taken, it is standby with the sodium hydroxide solution of distilled water configuration quality concentration 40%;
(3)Take the distilled water of 10 times of acrylamide quality to be placed in reaction vessel, sequentially add 2- acrylamido -2- methyl-props
Sulfonic acid, N,N-DMAA, acrylamide, acrylic acid, methene base bisacrylamide, rotating speed 400r/min are sufficiently stirred for
1 hour, it is fully dissolved, add ferrous sulfate, react 35 minutes, temperature rises to 90 DEG C, kept for 1 hour, natural cooling makes
Temperature is down to 50 DEG C, obtains crosslinking copolymerization thing blob of viscose, blob of viscose is granulated with comminutor, obtain copolymer micelle;
(4)Copolymer micelle is mixed with the sodium hydroxide solution of mass concentration 40%, is stirred continuously at 80 DEG C, neutralizing hydrolysis
2.2 hours, product is then made the conditioning agent with spatial networks macromolecular structure in 120 DEG C of dryings, crushing.
3. a kind of high temperature resistance, anti-high salt concentration flow pattern regulator, it is characterised in that:Prepared using following steps:
(1)By weight 2:1:1:0.8:0.02 prepares four kinds of monomers and crosslinking agent:2- acrylamide-2-methylpro panesulfonic acids,
N, N- DMAA, acrylamide, acrylic acid and methene base bisacrylamide;
(2)Sodium hydroxide is taken, it is standby with the sodium hydroxide solution of distilled water configuration quality concentration 40%;
(3)Take the distilled water of 8 times of acrylamide quality to be placed in reaction vessel, sequentially add 2- acrylamido -2- methyl-props
Sulfonic acid, N,N-DMAA, acrylamide, acrylic acid, methene base bisacrylamide, rotating speed 600r/min are sufficiently stirred for
1.5 hours, it is fully dissolved, add TBHP, react 25 minutes, temperature rises to 90 DEG C, kept for 1.2 hours,
Natural cooling makes temperature be down to 50 DEG C, obtains crosslinking copolymerization thing blob of viscose, blob of viscose is granulated with comminutor, obtain copolymer micelle;
(4)Copolymer micelle is mixed with the sodium hydroxide solution of mass concentration 40%, is stirred continuously at 80 DEG C, neutralizing hydrolysis
2.5 hours, product is then made the conditioning agent with spatial networks macromolecular structure in 120 DEG C of dryings, crushing.
4. a kind of high temperature resistance, anti-high salt concentration flow pattern regulator, it is characterised in that:Prepared using following steps:
(1)By weight 2.5:1.5:1:1.0:0.04 prepares four kinds of monomers and crosslinking agent:2- acrylamido -2- methyl-prop sulphurs
Acid, N, N- DMAAs, acrylamide, acrylic acid and methene base bisacrylamide;
(2)Sodium hydroxide is taken, it is standby with the sodium hydroxide solution of distilled water configuration quality concentration 40%;
(3)Take the distilled water of 9 times of acrylamide quality to be placed in reaction vessel, sequentially add 2- acrylamido -2- methyl-props
Sulfonic acid, N,N-DMAA, acrylamide, acrylic acid, methene base bisacrylamide, rotating speed 200r/min are sufficiently stirred for
2 hours, it is fully dissolved, add ferrous sulfate, react 30 minutes, temperature rises to 90 DEG C, kept for 1.5 hours, natural cooling
Temperature is down to 50 DEG C, obtain crosslinking copolymerization thing blob of viscose, blob of viscose is granulated with comminutor, obtain copolymer micelle;
(4)Copolymer micelle is mixed with the sodium hydroxide solution of mass concentration 40%, is stirred continuously at 80 DEG C, neutralizing hydrolysis
2.5 hours, product is then made the conditioning agent with spatial networks macromolecular structure in 120 DEG C of dryings, crushing.
5. a kind of high temperature resistance, anti-high salt concentration flow pattern regulator, it is characterised in that:Prepared using following steps:
(1)By weight 3: 2:1:0.8:0.06 prepares four kinds of monomers and crosslinking agent:2- acrylamide-2-methylpro panesulfonic acids,
N, N- DMAA, acrylamide, acrylic acid and methene base bisacrylamide;
(2)Sodium hydroxide is taken, it is standby with the sodium hydroxide solution of distilled water configuration quality concentration 40%;
(3)Take the distilled water of 12 times of acrylamide quality to be placed in reaction vessel, sequentially add 2- acrylamido -2- methyl-props
Sulfonic acid, N,N-DMAA, acrylamide, acrylic acid, methene base bisacrylamide, rotating speed 500r/min are sufficiently stirred for
2 hours, it is fully dissolved, add TBHP, react 30 minutes, temperature rises to 90 DEG C, kept for 2 hours, it is natural
Cooling makes temperature be down to 50 DEG C, obtains crosslinking copolymerization thing blob of viscose, blob of viscose is granulated with comminutor, obtain copolymer micelle;
(4)Copolymer micelle is mixed with the sodium hydroxide solution of mass concentration 40%, is stirred continuously at 80 DEG C, neutralizing hydrolysis 3
Hour, product is then made the conditioning agent with spatial networks macromolecular structure in 120 DEG C of dryings, crushing.
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