CN105237679A - Preparation method of oil well cement emulsion polymer fluid loss agent - Google Patents
Preparation method of oil well cement emulsion polymer fluid loss agent Download PDFInfo
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Abstract
The invention discloses a preparation method of an oil well cement emulsion polymer fluid loss agent. The method comprises the following steps: (1) water, 2-acrylamido-2-methylpropanesulfonic acid, acrylamide, alpha-methacrylic acid, N, N-methylene bis-acrylamide, maleic anhydride and a pH value adjusting agent are prepared into a solution A; a surfactant, an emulsifier and 25# transformer oil are prepared into a solution B; (2) the solution A and the solution B obtained in the step (1) are emulsified together in an emulsifying container; and when the mixture is uniformly emulsified, an emulsion for reaction is obtained; (3) the emulsion for reaction obtained in the step (2) is transferred into a reaction container, and is stirred; heating is carried out, and an initiator solution is added for initiating a reaction; and after the reaction, the oil well cement emulsion polymer fluid loss agent can be obtained. The polymer fluid loss agent provided by the invention has the advantages of high liquid-phase product effective content and low product viscosity. During the preparation process, a reaction solution is stable, side reaction amount is low, and the reaction process is easy to control.
Description
Technical field
The present invention relates to oil field chemical new technical field.More specifically, a kind of preparation method of oil well cement emulsion polymer water retaining is related to.
Background technology
At present, oil-well cement filtrate reducer is principal monomer synthesized polymer objects system mainly with 2-acrylamide-2-methylpro panesulfonic acid.Such water retaining obtains with aqueous process polymerization usually, and due to the restriction of polymerization process, liquid-phase product effective content is generally 10%-25%, and effective content is low, and dosage is large, improves use and transportation cost.In addition, during letex polymerization, oil phase often adopts white oil, kerosene, solvent oil, and during this three kinds of oil phase sinteticses, emulsion is unstable, and product viscosity is large, and side reaction is many, and process is difficult to control.
Summary of the invention
One object of the present invention is the preparation method of the oil well cement emulsion polymer water retaining providing a kind of liquid-phase product effective content high, not only obtained product viscosity is little, and in preparation process, reaction soln is stable, side reaction is few, reaction process is easy to control.
For achieving the above object, the present invention adopts following technical proposals:
A preparation method for oil well cement emulsion polymer water retaining, comprises the steps:
(1) water, 2-acrylamide-2-methylpro panesulfonic acid, acrylamide, α-methacrylic acid, N,N methylene bis acrylamide, MALEIC ANHYDRIDE and pH value regulator are mixed with solution A; Tensio-active agent, emulsifying agent and 25# transformer oil are mixed with solution B;
(2) solution A that step (1) is obtained is put into the emulsification of emulsification container together with solution B, after emulsification evenly, obtain question response emulsion;
(3) transfer in reaction vessel by the question response emulsion that step (2) is obtained, stir, heat temperature raising, then adds initiator solution initiation reaction, can obtain oil well cement emulsion polymer water retaining after reaction terminates.
The preparation method of above-mentioned oil well cement emulsion polymer water retaining, in step (1), the compound method of solution A is: dropped into by water in reaction vessel, open and stir, then 2-acrylamide-2-methylpro panesulfonic acid, acrylamide, α-methacrylic acid, N is dropped into successively, N-methylene-bisacrylamide and MALEIC ANHYDRIDE, be then adjusted to 4 ~ 5 by pH value regulator by the pH value of mixture in reaction vessel.
The preparation method of above-mentioned oil well cement emulsion polymer water retaining, the water of obtain solution A is distilled water or deionized water; PH value regulator is the mixture of potassium hydroxide solution or sodium hydroxide solution or potassium hydroxide solution and sodium hydroxide solution.
The preparation method of above-mentioned oil well cement emulsion polymer water retaining, the compound method of solution A is: dropped into by 34 ~ 88 mass parts distilled water in reaction vessel, open and stir, then 29 ~ 36 mass parts 2-acrylamide-2-methylpro panesulfonic acids are dropped into successively, 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 ANHYDRIDE, optimizing best monomer ratio by orthogonal grout experiment is 2-acrylamide-2-methylpro panesulfonic acid: acrylamide: α-methacrylic acid: N, N-methylene-bisacrylamide: MALEIC ANHYDRIDE=84.5:10.9:1.2:0.08:3.4, then with the sodium hydroxide solution of 17 ~ 20 mass parts, the pH value of mixture in reaction vessel is adjusted to 4 ~ 5, in the process that the pH value of mixture in reaction vessel is regulated, in reaction vessel, the temperature of mixture is less than or equal to 40 DEG C.
The preparation method of above-mentioned oil well cement emulsion polymer water retaining, concentration of sodium hydroxide solution is 40wt%.
The preparation method of above-mentioned oil well cement emulsion polymer water retaining, in step (1), described tensio-active agent is one or both and two or more mixtures in polysorbas20, polysorbate40, polysorbate60 and tween 80, and described emulsifying agent is the mixture of span 20 or sorbester p17 or span 20 and sorbester p17.
The preparation method of above-mentioned oil well cement emulsion polymer water retaining, in step (1), the compound method of solution B is: in reaction vessel, drop into 1 ~ 2 mass parts sorbester p17,0.2 ~ 0.4 mass parts polysorbate60 and 7.5 ~ 11 mass parts 25# transformer oil successively, then by reaction vessel mixture rising temperature for dissolving mixing, solution B.
The preparation method of above-mentioned oil well cement emulsion polymer water retaining, described initiator solution is made up of 0.04 ~ 0.05 mass parts ammonium persulphate and 2 mass parts distilled water.
The preparation method of above-mentioned oil well cement emulsion polymer water retaining, step (3) is: the question response emulsion that step (2) is obtained is transferred in reaction vessel, stir, be heated to 60 ~ 65 DEG C, add initiator solution, agitator motor rotating speed is adjusted to 300r/min and stirs initiation, question response solution temperature rises to 70 DEG C, agitator motor rotating speed is adjusted to 1200r/min, the temperature of reaction soln controls below 100 DEG C by open cold radiator cooler, when temperature is down to 70 DEG C, agitator motor rotating speed is adjusted to 600r/min, after making reaction soln constant temperature continue reaction 1h at 80 DEG C, obtain oil well cement emulsion polymer water retaining.
The preparation method of above-mentioned oil well cement emulsion polymer water retaining, comprises the steps:
(1) obtain solution A: 34 ~ 88 mass parts distilled water are dropped in reaction vessel, open and stir, then 29 ~ 36 mass parts 2-acrylamide-2-methylpro panesulfonic acids are dropped into successively, 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 ANHYDRIDE, then with the sodium hydroxide solution of 17 ~ 20 mass parts, the pH value of mixture in reaction vessel is adjusted to 4 ~ 5, in the process that the pH value of mixture in reaction vessel is regulated, in reaction vessel, the temperature of mixture is less than or equal to 40 DEG C, obtain solution B: drop into 1 ~ 2 mass parts sorbester p17,0.2 ~ 0.4 mass parts polysorbate60 and 7.5 ~ 11 mass parts 25# transformer oil in reaction vessel successively, then by reaction vessel mixture rising temperature for dissolving mixing, solution B,
(2) to get in the step (1) of 5 ~ 10 mass parts and put into emulsification container together with obtained solution B solution A obtained with the step (1) of 85.43 ~ 104.54 mass parts in and carry out emulsification, after emulsification is even, namely obtain question response emulsion;
(3) band reaction emulsion obtained for step (2) is transferred in reaction vessel, stir, be heated to 60 ~ 65 DEG C, add initiator solution, described initiator solution is made up of 0.04 ~ 0.05 mass parts ammonium persulphate and 2 mass parts distilled water, agitator motor rotating speed is adjusted to 300r/min and stirs initiation, question response solution temperature rises to 70 DEG C, agitator motor rotating speed is adjusted to 1200r/min, the temperature of reaction soln controls below 100 DEG C by open cold radiator cooler, when temperature is down to 70 DEG C, agitator motor rotating speed is adjusted to 600r/min, after making reaction soln constant temperature continue reaction 1h at 80 DEG C, obtain oil well cement emulsion polymer water retaining.
Beneficial effect of the present invention is as follows:
1. not only liquid-phase product effective content is high for the water retaining obtained by the present invention, and product viscosity is little.
2. reaction soln is stable, side reaction is few preparing in water retaining process in the present invention, and reaction process is easy to control.
3. this patent adopts the oil well cement emulsion polymer water retaining that the method for letex polymerization synthesis concentration is larger, dosage controls at 1%-1.5% that (dosage is the per-cent relative to cement quality, namely every 100 grams of cement add the oil well cement emulsion polymer water retaining of the present invention of 1-1.5 gram), only need 1/5th of aqueous solution polymerization product dosage, greatly reduce use and transportation cost.
4. this patent selects 25# transformer oil as the oil phase of letex polymerization, and sintetics viscosity is low, emulsion-stabilizing, and can preserve 3 years and use properties is not any change, reaction process is easy to control.
5. compare solid aqueous solution polymkeric substance water retaining, oil well cement emulsion polymer water retaining of the present invention is liquid, and without the need to removing the operations such as oil phase, purification and oven dry in preparation process, technique is comparatively simple; And the shelf time is very long.
Embodiment
In order to be illustrated more clearly in the present invention, below in conjunction with preferred embodiment, the present invention is described further.It will be appreciated by those skilled in the art that specifically described content is illustrative and nonrestrictive, should not limit the scope of the invention with this below.
Embodiment 1:
(1) preparation of solution A: 190kg distilled water is dropped in reactor, open and stir, drop into 165kg2-acrylamide-2-methylpro panesulfonic acid, 21kg acrylamide, 2.2kg α-methacrylic acid, 0.2kgN successively again, N-methylene-bisacrylamide, 6.25kg MALEIC ANHYDRIDE, then material pH value is regulated to be 4-5 with the sodium hydroxide solution that the sodium hydroxide massfraction of 91.5kg is 40wt%, in pH value regulate process, control temperature is no more than 40 DEG C, for subsequent use as aqueous phase solution.
(2) preparation of solution B: drop into 10kg sorbester p17 successively in reactor, 1.3kg polysorbate60,49.3kg25# transformer oil be warming up to 60 ± 2 DEG C and dissolve mixing.
(3) emulsion polymerization process: 49.3kg solution B and 486.15kg solution A are transferred in reactor after emulsification evenly in emulsifying kettle, unlatching reactor stirs, material is warming up to 60-65 DEG C, add the initiator solution be mixed with by 0.2kg ammonium persulphate and 10kg distilled water, regulate agitator motor rotating speed to stir at 300r/min to cause, treat that temperature of charge rises to 70 DEG C, improve agitator motor speed to 1200 ± 2r/min, control material temperature below 100 DEG C, treat that temperature is down to 70 DEG C, regulate agitator motor rotating speed 600r/min, material constant temperature is made to continue reaction 1h at 80 DEG C, be down to less than 50 DEG C and namely obtain oil well cement emulsion polymer water retaining product, preserve and still can use for 3 years, use properties is without any change.This embodiment is most preferred embodiment, product viscosity is low, emulsion-stabilizing, liquid phase water retaining dosage can be reduced to 1.5%, and (dosage is the per-cent relative to cement quality, namely every 100 grams of cement add the oil well cement emulsion polymer water retaining of 1.5 grams), the level (liquids in general aqueous polymer water retaining dosage is 5%) of solid aqueous solution polymkeric substance water retaining dosage can be reached; Gained liquid product viscosities is 80MPas.
Embodiment 2:
(1) preparation of solution A: 190kg distilled water is dropped in reactor, open and stir, drop into 165kg2-acrylamide-2-methylpro panesulfonic acid, 21kg acrylamide, 2.2kg α-methacrylic acid, 0.2kgN successively again, N-methylene-bisacrylamide, 6.25kg MALEIC ANHYDRIDE, then material pH value is regulated to be 4-5 with the sodium hydroxide solution that the sodium hydroxide massfraction of 91.5kg is 40wt%, in pH regulator process, control temperature is no more than 40 DEG C, for subsequent use as aqueous phase solution.
(2) preparation of solution B: drop into 5kg sorbester p17 successively in reactor, 0.65kg polysorbate60,19kg25# transformer oil steam is warming up to 60 ± 2 DEG C and dissolves mixing.
(3) emulsion polymerization process: 24.65kg solution B and 486.15kg solution A are transferred in reactor after emulsification evenly in emulsifying kettle, unlatching reactor stirs, material is warming up to 60-65 DEG C, add the initiator solution be mixed with by 0.2kg ammonium persulphate and 10kg distilled water, regulate agitator motor rotating speed to stir at 300r/min to cause, treat that temperature of charge rises to 70 DEG C, improve agitator motor speed to 1200 ± 2r/min, control material temperature below 100 DEG C, treat that temperature is down to 70 DEG C, regulate agitator motor rotating speed 600r/min, material constant temperature is made to continue reaction 1h at 80 DEG C, obtain oil well cement emulsion polymer water retaining product, preserve and still can use for 3 years, use properties is without any change.It is that 2.0% (dosage is the per-cent relative to cement quality that this embodiment obtains product dosage, namely every 100 grams of cement add the oil well cement emulsion polymer water retaining of 2 grams), the level (liquids in general aqueous polymer water retaining dosage is 5%) of solid aqueous solution polymkeric substance water retaining dosage can be reached; Emulsion-stabilizing, viscosity is 123Pas.
Embodiment 3:
(1) preparation of solution A: the distilled water of 240kg is dropped in reactor, open and stir, drop into 165kg2-acrylamide-2-methylpro panesulfonic acid, 21kg acrylamide, 2.2kg α-methacrylic acid, 0.2kgN successively again, N-methylene-bisacrylamide, 6.25kg MALEIC ANHYDRIDE, then material pH value is regulated to be 4-5 with the sodium hydroxide solution that the sodium hydroxide massfraction of 91.5kg is 40wt%, in pH value regulate process, control temperature is no more than 40 DEG C, for subsequent use as aqueous phase solution.
(2) preparation of solution A: drop into 10kg sorbester p17 successively in reactor, 1.3kg polysorbate60,49.3kg25# transformer oil be warming up to 60 ± 2 DEG C and dissolve mixing.
(3) emulsion polymerization process: 49.3kg solution B and 526.15kg solution A are transferred in reactor after emulsification evenly in emulsifying kettle, unlatching reactor stirs, material is warming up to 60-65 DEG C, add the initiator solution be mixed with by 0.2kg ammonium persulphate and 10kg distilled water, regulate agitator motor rotating speed to stir at 300r/min to cause, treat that temperature of charge rises to 70 DEG C, improve agitator motor speed to 1200 ± 2r/min, control material temperature below 100 DEG C, treat that temperature is down to 70 DEG C, regulate agitator motor rotating speed 600r/min, material constant temperature is made to continue reaction 1h at 80 DEG C, obtain oil well cement emulsion polymer water retaining product, preserve and still can use for 3 years, use properties is without any change.It is 74mPas that this embodiment obtains product viscosity, dosage is that 2.0% (dosage is the per-cent relative to cement quality, namely every 100 grams of cement add the oil well cement emulsion polymer water retaining of 2 grams), the level (liquids in general aqueous polymer water retaining dosage is 5%) of solid aqueous solution polymkeric substance water retaining dosage can be reached; Emulsion-stabilizing, reaction process is more easy to control.
Embodiment 4
(1) preparation of solution A: the distilled water of 200kg is dropped in reactor, open and stir, drop into 165kg2-acrylamide-2-methylpro panesulfonic acid, 21.3kg acrylamide, 2.3kg α-methacrylic acid, 0.15kgN successively again, N-methylene-bisacrylamide, 6.6kg MALEIC ANHYDRIDE, then material pH value is regulated to be 4-5 with the sodium hydroxide solution that the sodium hydroxide massfraction of 94kg is 40wt%, in pH value regulate process, control temperature is no more than 40 DEG C, for subsequent use as aqueous phase solution.
(2) preparation of solution A: drop into 7.5kg sorbester p17 successively in reactor, 1.5kg polysorbate60,47.5kg25# transformer oil be warming up to 60 ± 2 DEG C and dissolve mixing.
(3) emulsion polymerization process: 56.5kg solution B and 489.35kg solution A are transferred in reactor after emulsification evenly in emulsifying kettle, unlatching reactor stirs, material is warming up to 60-65 DEG C, add the initiator solution be mixed with by 0.2kg ammonium persulphate and 10kg distilled water, regulate agitator motor rotating speed to stir at 300r/min to cause, treat that temperature of charge rises to 70 DEG C, improve agitator motor speed to 1200 ± 2r/min, control material temperature below 100 DEG C, treat that temperature is down to 70 DEG C, regulate agitator motor rotating speed 600r/min, material constant temperature is made to continue reaction 1h at 80 DEG C, obtain oil well cement emulsion polymer water retaining product, preserve and still can use for 3 years, use properties is without any change.It is 74mPas that this embodiment obtains product viscosity, dosage is that 1.5% (dosage is the per-cent relative to cement quality, namely every 100 grams of cement add the oil well cement emulsion polymer water retaining of 1.5 grams), the level (liquids in general aqueous polymer water retaining dosage is 5%) of solid aqueous solution polymkeric substance water retaining dosage can be reached.
Obviously; the above embodiment of the present invention is only for example of the present invention is clearly described; and be not the restriction to embodiments of the present invention; for those of ordinary skill in the field; can also make other changes in different forms on the basis of the above description; here cannot give exhaustive to all embodiments, every belong to technical scheme of the present invention the apparent change of extending out or variation be still in the row of protection scope of the present invention.
Claims (10)
1. a preparation method for oil well cement emulsion polymer water retaining, is characterized in that, comprises the steps:
(1) water, 2-acrylamide-2-methylpro panesulfonic acid, acrylamide, α-methacrylic acid, N,N methylene bis acrylamide, MALEIC ANHYDRIDE and pH value regulator are mixed with solution A; Tensio-active agent, emulsifying agent and 25# transformer oil are mixed with solution B;
(2) solution A that step (1) is obtained is put into the emulsification of emulsification container together with solution B, after emulsification evenly, obtain question response emulsion;
(3) transfer in reaction vessel by the question response emulsion that step (2) is obtained, stir, heat temperature raising, then adds initiator solution initiation reaction, can obtain oil well cement emulsion polymer water retaining after reaction terminates.
2. the preparation method of oil well cement emulsion polymer water retaining according to claim 1, it is characterized in that, in step (1), the compound method of solution A is: dropped into by water in reaction vessel, open and stir, then 2-acrylamide-2-methylpro panesulfonic acid, acrylamide, α-methacrylic acid, N is dropped into successively, N-methylene-bisacrylamide and MALEIC ANHYDRIDE, be then adjusted to 4 ~ 5 by pH value regulator by the pH value of mixture in reaction vessel.
3. the preparation method of oil well cement emulsion polymer water retaining according to claim 2, is characterized in that, the water of obtain solution A is distilled water or deionized water; PH value regulator is the mixture of potassium hydroxide solution or sodium hydroxide solution or potassium hydroxide solution and sodium hydroxide solution.
4. the preparation method of oil well cement emulsion polymer water retaining according to claim 3, it is characterized in that, the compound method of solution A is: dropped into by 34 ~ 88 mass parts distilled water in reaction vessel, open and stir, then 29 ~ 36 mass parts 2-acrylamide-2-methylpro panesulfonic acids are dropped into successively, 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 ANHYDRIDE, then with the sodium hydroxide solution of 17 ~ 20 mass parts, the pH value of mixture in reaction vessel is adjusted to 4 ~ 5, in the process that the pH value of mixture in reaction vessel is regulated, in reaction vessel, the temperature of mixture is less than or equal to 40 DEG C.
5. the preparation method of oil well cement emulsion polymer water retaining according to claim 4, is characterized in that, concentration of sodium hydroxide solution is 40wt%.
6. the preparation method of oil well cement emulsion polymer water retaining according to claim 1, it is characterized in that, in step (1), described tensio-active agent is one or both and two or more mixtures in polysorbas20, polysorbate40, polysorbate60 and tween 80, and described emulsifying agent is the mixture of span 20 or sorbester p17 or span 20 and sorbester p17.
7. the preparation method of oil well cement emulsion polymer water retaining according to claim 6, it is characterized in that, in step (1), the compound method of solution B is: in reaction vessel, drop into 1 ~ 2 mass parts sorbester p17,0.2 ~ 0.4 mass parts polysorbate60 and 7.5 ~ 11 mass parts 25# transformer oil successively, then by reaction vessel mixture rising temperature for dissolving mixing, solution B.
8. the preparation method of oil well cement emulsion polymer water retaining according to claim 1, is characterized in that, described initiator solution is made up of 0.04 ~ 0.05 mass parts ammonium persulphate and 2 mass parts distilled water.
9. the preparation method of oil well cement emulsion polymer water retaining according to claim 8, it is characterized in that, step (3) is: the question response emulsion that step (2) is obtained is transferred in reaction vessel, stir, be heated to 60 ~ 65 DEG C, add initiator solution, agitator motor rotating speed is adjusted to 300r/min and stirs initiation, question response solution temperature rises to 70 DEG C, agitator motor rotating speed is adjusted to 1200r/min, the temperature of reaction soln controls below 100 DEG C by open cold radiator cooler, when temperature is down to 70 DEG C, agitator motor rotating speed is adjusted to 600r/min, after making reaction soln constant temperature continue reaction 1h at 80 DEG C, obtain oil well cement emulsion polymer water retaining.
10., according to the preparation method of the arbitrary described oil well cement emulsion polymer water retaining of claim 1-9, it is characterized in that, comprise the steps:
(1) obtain solution A: 34 ~ 88 mass parts distilled water are dropped in reaction vessel, open and stir, then 29 ~ 36 mass parts 2-acrylamide-2-methylpro panesulfonic acids are dropped into successively, 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 ANHYDRIDE, then with the sodium hydroxide solution of 17 ~ 20 mass parts, the pH value of mixture in reaction vessel is adjusted to 4 ~ 5, in the process that the pH value of mixture in reaction vessel is regulated, in reaction vessel, the temperature of mixture is less than or equal to 40 DEG C, obtain solution B: drop into 1 ~ 2 mass parts sorbester p17,0.2 ~ 0.4 mass parts polysorbate60 and 7.5 ~ 11 mass parts 25# transformer oil in reaction vessel successively, then by reaction vessel mixture rising temperature for dissolving mixing, solution B,
(2) to get in the step (1) of 5 ~ 10 mass parts and put into emulsification container together with obtained solution B solution A obtained with the step (1) of 85.43 ~ 104.54 mass parts in and carry out emulsification, after emulsification is even, namely obtain question response emulsion;
(3) band reaction emulsion obtained for step (2) is transferred in reaction vessel, stir, be heated to 60 ~ 65 DEG C, add initiator solution, described initiator solution is made up of 0.04 ~ 0.05 mass parts ammonium persulphate and 2 mass parts distilled water, agitator motor rotating speed is adjusted to 300r/min and stirs initiation, question response solution temperature rises to 70 DEG C, agitator motor rotating speed is adjusted to 1200r/min, the temperature of reaction soln controls below 100 DEG C by open cold radiator cooler, when temperature is down to 70 DEG C, agitator motor rotating speed is adjusted to 600r/min, after making reaction soln constant temperature continue reaction 1h at 80 DEG C, obtain oil well cement emulsion polymer water retaining.
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