CN105237679B - A kind of preparation method of oil-well cement emulsion polymer fluid loss agent - Google Patents
A kind of preparation method of oil-well cement emulsion polymer fluid loss agent Download PDFInfo
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Abstract
The present invention discloses a kind of preparation method of oil-well cement emulsion polymer fluid loss agent, comprises the following steps：(1) by water, the methyl propane sulfonic acid of 2 acrylamido 2, acrylamide, α methacrylic acids, N, N methylene-bisacrylamides, maleic anhydride and pH value regulator are configured to solution A；Surfactant, emulsifying agent and 25# transformer oil are configured to solution B；(2) solution A made from step (1) and solution B are put into together in emulsification container and emulsified, question response emulsion is obtained after emulsification uniformly；(3) question response emulsion made from step (2) is transferred in reaction vessel, stirred, heat temperature raising, then add initiator solution initiation reaction, reaction can obtain oil-well cement emulsion polymer fluid loss agent after terminating.Polymer fluid loss agent produced by the present invention not only has the advantages of liquid-phase product effective content is high, product viscosity is small, and reaction solution is stable in preparation process, side reaction is few, course of reaction is easy to control.
Description
Technical field
The present invention relates to oil field chemical new technical field.Dropped more particularly, to a kind of oil-well cement emulsion polymer
The preparation method of dehydration agent.
Background technology
At present, oil-well cement filtrate reducer is more using 2- acrylamide-2-methylpro panesulfonic acids as principal monomer synthesized polymer
Objects system.Such fluid loss agent generally polymerize to obtain with aqueous process, and due to the limitation of polymerization, liquid-phase product effectively contains
Amount is generally 10%-25%, and effective content is low, and dosage is big, improves use and cost of transportation.In addition, oil phase during emulsion polymerization
Frequently with white oil, kerosene, solvent naphtha, and emulsion is unstable during these three oil phase sinteticses, and product viscosity is big, and side reaction is more,
Process is difficult to control.
The content of the invention
It is an object of the present invention to provide a kind of high oil-well cement emulsion polymer drop of liquid-phase product effective content
The preparation method of dehydration agent, not only obtained product viscosity is small, and reaction solution stabilization, side reaction are few, anti-in preparation process
Answer process easy to control.
To reach above-mentioned purpose, the present invention uses following technical proposals：
A kind of preparation method of oil-well cement emulsion polymer fluid loss agent, comprises the following steps：
(1) by water, 2- acrylamide-2-methylpro panesulfonic acids, acrylamide, α-methacrylic acid, N, N- di-2-ethylhexylphosphine oxides
Acrylamide, maleic anhydride and pH value regulator are configured to solution A；By surfactant, emulsifying agent and 25# transformer oil
It is configured to solution B；
(2) solution A made from step (1) and solution B are put into together in emulsification container and emulsified, treated after emulsification uniformly
React emulsion；
(3) question response emulsion made from step (2) is transferred in reaction vessel, stirred, heat temperature raising, then added and draw
Agent solution initiation reaction is sent out, reaction can obtain oil-well cement emulsion polymer fluid loss agent after terminating.
The preparation method of above-mentioned oil-well cement emulsion polymer fluid loss agent, the compound method of solution A is in step (1)：
Water is put into reaction vessel, opens stirring, then put into successively 2- acrylamide-2-methylpro panesulfonic acids, acrylamide, α-
Methacrylic acid, N, N- methylene-bisacrylamides and maleic anhydride, then it will be mixed with pH value regulator in reaction vessel
The pH value of compound is adjusted to 4~5.
The preparation method of above-mentioned oil-well cement emulsion polymer fluid loss agent, the water for preparing solution A are distilled water or gone
Ionized water；PH value regulator is potassium hydroxide solution or sodium hydroxide solution or potassium hydroxide solution and sodium hydroxide solution
Mixture.
The preparation method of above-mentioned oil-well cement emulsion polymer fluid loss agent, the compound method of solution A are：By 34~88 matter
Measure in part distilled water input reaction vessel, open stirring, then put into 29~36 mass parts 2- acrylamido -2- methyl successively
Propane sulfonic acid, 3.8~4.6 mass parts acrylamides, 0.4~0.5 mass parts α-methacrylic acid, 0.03~0.04 mass parts N, N-
Methylene-bisacrylamide, 1.2~1.4 mass parts maleic anhydrides, optimal monomer is preferably gone out by the experiment of orthogonal cement mortar
Ratio is 2- acrylamide-2-methylpro panesulfonic acids：Acrylamide：α-methacrylic acid：N, N- methylene-bisacrylamide：It is suitable
Anhydride maleique=84.5：10.9：1.2：0.08：3.4, then with the sodium hydroxide solutions of 17~20 mass parts by reaction vessel
The pH value of interior mixture is adjusted to 4~5, during the pH value of mixture in reaction vessel is adjusted, is mixed in reaction vessel
The temperature of compound material is less than or equal to 40 DEG C.
The preparation method of above-mentioned oil-well cement emulsion polymer fluid loss agent, concentration of sodium hydroxide solution 40wt%.
The preparation method of above-mentioned oil-well cement emulsion polymer fluid loss agent, in step (1), the surfactant is tells
One or both of temperature 20, polysorbate40, polysorbate60 and Tween 80 and two or more mixtures, the emulsifying agent are span 20
Or sorbester p17 or the mixture of span 20 and sorbester p17.
The preparation method of above-mentioned oil-well cement emulsion polymer fluid loss agent, the compound method of solution B is in step (1)：
1~2 mass parts sorbester p17,0.2~0.4 mass parts polysorbate60 and 7.5~11 mass parts 25# are put into successively into reaction vessel to become
Depressor oil, then mixes the mixture rising temperature for dissolving in reaction vessel, you can obtains solution B.
The preparation method of above-mentioned oil-well cement emulsion polymer fluid loss agent, the initiator solution is by 0.04~0.05 matter
Measure part ammonium persulfate and 2 mass parts distilled water form.
The preparation method of above-mentioned oil-well cement emulsion polymer fluid loss agent, step (3) are：It will be treated made from step (2)
Reaction emulsion is transferred in reaction vessel, is stirred, and is heated to 60~65 DEG C, adds initiator solution, and stirring motor is turned
Velocity modulation stirs to 300r/min to be triggered, and question response solution temperature rises to 70 DEG C, stirring motor rotating speed is adjusted into 1200r/min, opened
Cooling device is opened by the temperature control of reaction solution below 100 DEG C, when temperature is down to 70 DEG C, stirring motor rotating speed is adjusted to
600r/min, reaction solution constant temperature is set to produce oil-well cement emulsion polymer fluid loss agent after 80 DEG C are continued to react 1h.
The preparation method of above-mentioned oil-well cement emulsion polymer fluid loss agent, comprises the following steps：
(1) solution A is prepared：34~88 mass parts distilled water are put into reaction vessel, stirring is opened, then puts into successively
29~36 mass parts 2- acrylamide-2-methylpro panesulfonic acids, 3.8~4.6 mass parts acrylamides, 0.4~0.5 mass parts α-
Methacrylic acid, 0.03~0.04 mass parts N, N- methylene-bisacrylamide, 1.2~1.4 mass parts maleic anhydrides, so
The pH value of mixture in reaction vessel is adjusted to 4~5 with the sodium hydroxide solution of 17~20 mass parts afterwards, to being mixed in reaction vessel
During the pH value of compound is adjusted, the temperature of mixed material is less than or equal to 40 DEG C in reaction vessel；Prepare solution B：
1~2 mass parts sorbester p17,0.2~0.4 mass parts polysorbate60 and 7.5~11 mass parts 25# are put into successively into reaction vessel to become
Depressor oil, then mixes the mixture rising temperature for dissolving in reaction vessel, you can obtains solution B；
(2) obtained solution B and (1) the step of 85.43~104.54 mass parts in the step of taking 5~10 mass parts (1)
In obtained solution A be put into together emulsification container in emulsified, emulsification uniformly after produce question response emulsion；
(3) the obtained band reaction emulsion of step (2) is transferred in reaction vessel, stirs, be heated to 60~65 DEG C,
Initiator solution is added, the initiator solution is made up of 0.04~0.05 mass parts ammonium persulfate and 2 mass parts distilled water, will
Stirring motor rotating speed, which is adjusted to 300r/min stirrings, to be triggered, and question response solution temperature rises to 70 DEG C, stirring motor rotating speed is adjusted to
1200r/min, unlatching cooling device below 100 DEG C, when temperature is down to 70 DEG C, will stir the temperature control of reaction solution
Motor speed is adjusted to 600r/min, reaction solution constant temperature is produced oil-well cement emulsion polymer after 80 DEG C are continued to react 1h
Fluid loss agent.
Beneficial effects of the present invention are as follows：
1. by fluid loss agent produced by the present invention, not only liquid-phase product effective content is high, and product viscosity is small.
2. present invention reaction solution during fluid loss agent is prepared is stable, side reaction is few, and course of reaction is easy to control.
3. this patent is added using the larger oil-well cement emulsion polymer fluid loss agent of the method synthesis concentration of emulsion polymerization
Amount control that (dosage is the percentage relative to cement quality, i.e. this hair of 1-1.5 grams of every 100 grams of cement addition in 1%-1.5%
Bright oil-well cement emulsion polymer fluid loss agent), it is only necessary to 1/5th of aqueous solution polymerization product dosage, greatly reduce use
And cost of transportation.
4. this patent selects oil phase of the 25# transformer oil as emulsion polymerization, sintetics viscosity is low, emulsion-stabilizing, energy
Enough preserve 3 years and performance is not any change, course of reaction is easy to control.
5. comparing solid aqueous solution polymer fluid loss agent, oil-well cement emulsion polymer fluid loss agent of the present invention is liquid
State, the operation such as oil phase, purification and drying need not be removed in preparation process, and technique is relatively simple；And the holding time is very long.
Embodiment
In order to illustrate more clearly of the present invention, with reference to preferred embodiment, the present invention is described further.Ability
Field technique personnel should be appreciated that following specifically described content is illustrative and be not restrictive, and this should not be limited with this
The protection domain of invention.
Embodiment 1：
(1) preparation of solution A：190kg distilled water is put into reactor, opens stirring, then put into 165kg2- third successively
Acrylamide base -2- methyl propane sulfonic acids, 21kg acrylamides, 2.2kg α-methacrylic acids, 0.2kgN, N- methylene bisacrylamide acyls
Amine, 6.25kg maleic anhydrides, then adjusted with the sodium hydroxide solution that 91.5kg sodium hydroxide mass fraction is 40wt%
Section material pH value is 4-5, and temperature is controlled during pH value regulation no more than 40 DEG C, standby as aqueous phase solution.
(2) preparation of solution B：Put into 10kg sorbester p17s, 1.3kg polysorbate60s, 49.3kg25# transformations successively into reactor
Device oil is warming up to 60 ± 2 DEG C of dissolving mixing.
(3) emulsion polymerization process：Shifted after 49.3kg solution Bs and 486.15kg solution As are emulsified uniformly in emulsifying kettle
Into reactor, reactor stirring is opened, material is warming up to 60-65 DEG C, added by 0.2kg ammonium persulfates and 10kg distilled water
The initiator solution being configured to, regulation stirring motor rotating speed stirs in 300r/min to be triggered, and is treated that temperature of charge rises to 70 DEG C, is improved
Stirring motor speed treats that temperature is down to 70 DEG C, adjusts stirring motor to 1200 ± 2r/min, control material temperature below 100 DEG C
Rotating speed 600r/min, make material constant temperature continue to react 1h at 80 DEG C, be down to less than 50 DEG C and produce oil-well cement emulsion polymer drop
Dehydration agent product, preserving 3 years can still use, and performance does not have any change.The embodiment is most preferred embodiment, product
Viscosity is low, emulsion-stabilizing, and liquid phase fluid loss agent dosage can be reduced to 1.5%, and (dosage is the percentage relative to cement quality, i.e.,
Every 100 grams of cement adds 1.5 grams of oil-well cement emulsion polymer fluid loss agent), you can reach solid aqueous solution polymer drop
The level of dehydration agent dosage (liquids in general aqueous polymer fluid loss agent dosage is 5%)；Gained liquid product viscosities are
80MPa·s。
Embodiment 2：
(1) preparation of solution A：190kg distilled water is put into reactor, opens stirring, then put into 165kg2- third successively
Acrylamide base -2- methyl propane sulfonic acids, 21kg acrylamides, 2.2kg α-methacrylic acids, 0.2kgN, N- methylene bisacrylamide acyls
Amine, 6.25kg maleic anhydrides, then adjusted with the sodium hydroxide solution that 91.5kg sodium hydroxide mass fraction is 40wt%
Section material pH value is 4-5, and temperature is controlled during pH regulations no more than 40 DEG C, standby as aqueous phase solution.
(2) preparation of solution B：Put into 5kg sorbester p17s, 0.65kg polysorbate60s, 19kg25# transformers successively into reactor
Oil vapour is warming up to 60 ± 2 DEG C of dissolving mixing.
(3) emulsion polymerization process：Shifted after 24.65kg solution Bs and 486.15kg solution As are emulsified uniformly in emulsifying kettle
Into reactor, reactor stirring is opened, material is warming up to 60-65 DEG C, added by 0.2kg ammonium persulfates and 10kg distilled water
The initiator solution being configured to, regulation stirring motor rotating speed stirs in 300r/min to be triggered, and is treated that temperature of charge rises to 70 DEG C, is improved
Stirring motor speed treats that temperature is down to 70 DEG C, adjusts stirring motor to 1200 ± 2r/min, control material temperature below 100 DEG C
Rotating speed 600r/min, make material constant temperature continue to react 1h at 80 DEG C, produce oil-well cement emulsion polymer fluid loss agent product, protect
Depositing 3 years can still use, and performance does not have any change.The embodiment obtains product dosage, and (dosage is relative for 2.0%
In the percentage of cement quality, i.e., every 100 grams of cement adds 2 grams of oil-well cement emulsion polymer fluid loss agent), you can reach
The level of solid aqueous solution polymer fluid loss agent dosage (liquids in general aqueous polymer fluid loss agent dosage is 5%)；Breast
Liquid is stable, viscosity 123Pas.
Embodiment 3：
(1) preparation of solution A：By in 240kg distilled water input reactor, stirring is opened, then put into 165kg2- successively
Acrylamide-2-methylpro panesulfonic acid, 21kg acrylamides, 2.2kg α-methacrylic acids, 0.2kgN, N- methylene bisacrylamides
Acid amides, 6.25kg maleic anhydrides, the sodium hydroxide solution for being then 40wt% with 91.5kg sodium hydroxide mass fraction
Regulation material pH value is 4-5, and temperature is controlled during pH value regulation no more than 40 DEG C, standby as aqueous phase solution.
(2) preparation of solution A：Put into 10kg sorbester p17s, 1.3kg polysorbate60s, 49.3kg25# transformations successively into reactor
Device oil is warming up to 60 ± 2 DEG C of dissolving mixing.
(3) emulsion polymerization process：Shifted after 49.3kg solution Bs and 526.15kg solution As are emulsified uniformly in emulsifying kettle
Into reactor, reactor stirring is opened, material is warming up to 60-65 DEG C, added by 0.2kg ammonium persulfates and 10kg distilled water
The initiator solution being configured to, regulation stirring motor rotating speed stirs in 300r/min to be triggered, and is treated that temperature of charge rises to 70 DEG C, is improved
Stirring motor speed treats that temperature is down to 70 DEG C, adjusts stirring motor to 1200 ± 2r/min, control material temperature below 100 DEG C
Rotating speed 600r/min, make material constant temperature continue to react 1h at 80 DEG C, produce oil-well cement emulsion polymer fluid loss agent product, protect
Depositing 3 years can still use, and performance does not have any change.It is 74mPas that the embodiment, which obtains product viscosity, and dosage is
2.0% (dosage is the percentage relative to cement quality, i.e., every 100 grams of cement adds 2 grams of oil-well cement emulsion polymer drop
Dehydration agent), you can reach level (the liquids in general aqueous polymer drop dehydration of solid aqueous solution polymer fluid loss agent dosage
5%) agent dosage is；Emulsion-stabilizing, course of reaction are more easy to control.
Embodiment 4
(1) preparation of solution A：By in 200kg distilled water input reactor, stirring is opened, then put into 165kg2- successively
Acrylamide-2-methylpro panesulfonic acid, 21.3kg acrylamides, 2.3kg α-methacrylic acids, 0.15kgN, N- di-2-ethylhexylphosphine oxides third
Acrylamide, 6.6kg maleic anhydrides, then adjusted with the sodium hydroxide solution that 94kg sodium hydroxide mass fraction is 40wt%
Section material pH value is 4-5, and temperature is controlled during pH value regulation no more than 40 DEG C, standby as aqueous phase solution.
(2) preparation of solution A：7.5kg sorbester p17s, 1.5kg polysorbate60s, 47.5kg25# is put into successively into reactor to become
Depressor oil is warming up to 60 ± 2 DEG C of dissolving mixing.
(3) emulsion polymerization process：Shifted after 56.5kg solution Bs and 489.35kg solution As are emulsified uniformly in emulsifying kettle
Into reactor, reactor stirring is opened, material is warming up to 60-65 DEG C, added by 0.2kg ammonium persulfates and 10kg distilled water
The initiator solution being configured to, regulation stirring motor rotating speed stirs in 300r/min to be triggered, and is treated that temperature of charge rises to 70 DEG C, is improved
Stirring motor speed treats that temperature is down to 70 DEG C, adjusts stirring motor to 1200 ± 2r/min, control material temperature below 100 DEG C
Rotating speed 600r/min, make material constant temperature continue to react 1h at 80 DEG C, produce oil-well cement emulsion polymer fluid loss agent product, protect
Depositing 3 years can still use, and performance does not have any change.It is 74mPas that the embodiment, which obtains product viscosity, and dosage is
1.5% (dosage is the percentage relative to cement quality, i.e. every 100 grams of cement adds 1.5 grams of oil-well cement emulsion polymer
Fluid loss agent), you can reach level (the liquids in general aqueous polymer drop mistake of solid aqueous solution polymer fluid loss agent dosage
5%) aqua dosage is.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention, for those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms, all embodiments can not be exhaustive here, it is every to belong to this hair
Row of the obvious changes or variations that bright technical scheme is extended out still in protection scope of the present invention.
Claims (5)
1. a kind of preparation method of oil-well cement emulsion polymer fluid loss agent, it is characterised in that comprise the following steps：
(1) compound method of solution A is：34~88 mass parts distilled water are put into reaction vessel, open stirring, then successively
Put into 29~36 mass parts 2- acrylamide-2-methylpro panesulfonic acids, 3.8~4.6 mass parts acrylamides, 0.4~0.5 mass
Part α-methacrylic acid, 0.03~0.04 mass parts N,N methylene bis acrylamide, 1.2~1.4 mass parts maleic acids
Acid anhydride, the pH value of mixture in reaction vessel is then adjusted to 4~5 with the sodium hydroxide solution of 17~20 mass parts, reaction is held
During the pH value of mixture is adjusted in device, the temperature of mixed material is less than or equal to 40 DEG C in reaction vessel；
The compound method of solution B is：Put into 1~2 mass parts sorbester p17,0.2~0.4 mass parts tween successively into reaction vessel
60 and 7.5~11 mass parts 25# transformer oil, then the mixture rising temperature for dissolving in reaction vessel is mixed, you can obtain solution
B；
(2) solution A made from step (1) and solution B are put into together in emulsification container and emulsified, question response is obtained after emulsification uniformly
Emulsion；
(3) question response emulsion made from step (2) is transferred in reaction vessel, stirs, heat temperature raising, then add initiator
Solution initiation reaction, reaction can obtain oil-well cement emulsion polymer fluid loss agent after terminating.
2. the preparation method of oil-well cement emulsion polymer fluid loss agent according to claim 1, it is characterised in that hydrogen-oxygen
It is 40wt% to change sodium solution concentration.
3. the preparation method of oil-well cement emulsion polymer fluid loss agent according to claim 1, it is characterised in that described
Initiator solution is made up of 0.04~0.05 mass parts ammonium persulfate and 2 mass parts distilled water.
4. the preparation method of oil-well cement emulsion polymer fluid loss agent according to claim 3, it is characterised in that step
(3) it is：Question response emulsion made from step (2) is transferred in reaction vessel, stirred, is heated to 60~65 DEG C, is added
Initiator solution, stirring motor rotating speed is adjusted to 300r/min stirrings and triggered, question response solution temperature rises to 70 DEG C, by stirring electricity
Machine rotating speed is adjusted to 1200r/min, and the temperature control of reaction solution below 100 DEG C, is treated that temperature is down to 70 by unlatching cooling device
DEG C when, stirring motor rotating speed is adjusted to 600r/min, make reaction solution constant temperature 80 DEG C continue react 1h after, produce oil-well cement
Emulsion polymer fluid loss agent.
5. according to the preparation method of any described oil-well cement emulsion polymer fluid loss agents of claim 1-4, its feature exists
In comprising the following steps：
(1) solution A is prepared：By 34~88 mass parts distilled water put into reaction vessel in, open stirring, then successively input 29~
36 mass parts 2- acrylamide-2-methylpro panesulfonic acids, 3.8~4.6 mass parts acrylamides, 0.4~0.5 mass parts Alpha-Methyl
Acrylic acid, 0.03~0.04 mass parts N, N- methylene-bisacrylamide, 1.2~1.4 mass parts maleic anhydrides, Ran Houyong
The pH value of mixture in reaction vessel is adjusted to 4~5 by the sodium hydroxide solution of 17~20 mass parts, to mixture in reaction vessel
PH value be adjusted during, in reaction vessel the temperature of mixed material be less than or equal to 40 DEG C；Prepare solution B：To anti-
Answer and put into 1~2 mass parts sorbester p17,0.2~0.4 mass parts polysorbate60 and 7.5~11 mass parts 25# transformers in container successively
Oil, then the mixture rising temperature for dissolving in reaction vessel is mixed, you can obtain solution B；
(2) obtained solution B in (1) the step of 85.43~104.54 mass parts with making in the step of taking 5~10 mass parts (1)
The solution A obtained is put into emulsification container and emulsified together, and question response emulsion is produced after emulsification uniformly；
(3) the obtained band reaction emulsion of step (2) is transferred in reaction vessel, stirs, be heated to 60~65 DEG C, add
Initiator solution, the initiator solution are made up of 0.04~0.05 mass parts ammonium persulfate and 2 mass parts distilled water, will stirred
Motor speed, which is adjusted to 300r/min stirrings, to be triggered, and question response solution temperature rises to 70 DEG C, stirring motor rotating speed is adjusted into 1200r/
Min, cooling device is opened by the temperature control of reaction solution below 100 DEG C, when temperature is down to 70 DEG C, stirring motor is turned
Velocity modulation makes reaction solution constant temperature after 80 DEG C are continued to react 1h, produces the drop dehydration of oil-well cement emulsion polymer to 600r/min
Agent.
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