CN105176499A - Filtrate reducer capable of resisting high temperature and high-concentration salt and preparation method thereof - Google Patents
Filtrate reducer capable of resisting high temperature and high-concentration salt and preparation method thereof Download PDFInfo
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- CN105176499A CN105176499A CN201510510105.6A CN201510510105A CN105176499A CN 105176499 A CN105176499 A CN 105176499A CN 201510510105 A CN201510510105 A CN 201510510105A CN 105176499 A CN105176499 A CN 105176499A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
- C09K8/035—Organic additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
- C08F220/585—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine and containing other heteroatoms, e.g. 2-acrylamido-2-methylpropane sulfonic acid [AMPS]
Abstract
The invention discloses a filtrate reducer capable of resisting high temperature and high-concentration salt and used for a drilling fluid for oil and gas fields and a preparation method thereof. The filtrate reducer is prepared by subjecting three monomers consisting of N-vinyl pyrrolidone, 2-acrylamido-2-methylpropanesulfonate and N,N-dimethylacrylamide to radical copolymerization under the action of a redox initiator and then subjecting a copolymer obtained after radical copolymerization and a sodium hydroxide solution to neutralization. The filtrate reducer provided by the invention can substantially reduce the amount of filtrate loss and resist a high temperature of 220 DEG C and salinity of saturated salt water, and the high-temperature high-pressure filtration loss amount of the filtrate reducer is 10 ml after hot ageing of the filtrate reducer under the condition of a density of 2.3 SG at 220 DEG C for 16 h.
Description
Technical field
The present invention relates to a kind of high temperature resistance, anti-high salt concentration fluid loss agent, belong to drilling well oilfield technology field.
Background technology
In drilling process, due to the effect of pressure reduction, the moisture in drilling fluid inevitably passes through borehole wall leak-off in stratum, causes drilling fluid dehydration.Along with moisture enters stratum, in drilling fluid, clay particle is just attached on the borehole wall and forms " filter cake ", forms a filter cake borehole wall.Because the filter cake borehole wall is much finer and close than the original borehole wall, so it prevents the further dehydration of drilling fluid on the one hand, serve the effect of the protection borehole wall on the one hand.But in the process that the filter cake borehole wall is formed, the excess moisture of leak-off, filter cake is blocked up, and fine clay particle enters stratum etc. with moisture all can affect normal drilling well, and formation damages.The leak-off of drilling fluid and the leak-off of drilling fluid in drilling process that is formed in of filter cake are inevitable, and can form the filter cake protection borehole wall by leak-off.But drilling fluid filtration is excessive, easily causes shale expansion and cave in, causing hole instability.
Develop to deep for oil-gas exploration and development, drilling strata becomes increasingly complex, require more and more higher to the filtrate loss controllability of drilling fluid, Chinese scholars carries out modification to acrylamido copolymer, introduce new monomer and acrylamide copolymerization, prepare various fluid loss agent, as patent ZL201310185206.1 discloses one with acrylate, acrylamide for main monomer, glycidyl acrylate is cross-linking monomer, select water-soluble free radical initiator, under nitrogen existence condition, adopt the multipolymer that the method for letex polymerization is synthesized.
But in this type of prior art, what under the polymkeric substance of synthesis and ultra-high temperature condition, property of drilling fluid was safeguarded needs also there is gap.In order to overcome because reservoir pressure, temperature constantly raise, and high salt concentration is on the impact of the fluid loss agent of drilling fluid, causes filter loss to increase, and need provide a kind of high temperature resistance, anti-high salt concentration fluid loss agent.
Summary of the invention
The object of this invention is to provide a kind of high temperature resistance, anti-high salt concentration fluid loss agent, this fluid loss agent adopts NVP (NVP), 2-acrylamide-2-methylpro panesulfonic acid (AMPS), N, N-DMAA (NNDMA) three kinds of monomers are raw material, after redox initiator effect issues raw free radical copolymerization, the multipolymer obtained by copolymerization again and sodium hydroxide solution generation neutralization reaction obtain, this fluid loss agent, as high temperature resistant drilling fluids treatment agent, has stronger filtrate reducing effect and good heat and salinity tolerance ability.
The present invention also aims to the preparation method that above-mentioned a kind of fluid loss agent is provided.
Technical scheme of the present invention is as follows: a kind of high temperature resistance, anti-high salt concentration fluid loss agent, prepared by the feed composition of following parts by weight: NVP 100 ~ 150 parts, 2-acrylamide-2-methylpro panesulfonic acid 200 ~ 300 parts, N,N-DMAA 90 ~ 155 parts, redox initiator 0.5 ~ 3 part, 40 ~ 60 parts, sodium hydroxide, distilled water 500 ~ 700 parts.
Preferably, the quality proportioning of described NVP, 2-acrylamide-2-methylpro panesulfonic acid, N,N-DMAA three kinds of starting monomers is: 2.5:5:2.
Preferred further, described fluid loss agents is prepared by the feed composition of following quality proportioning: NVP 132g, 2-acrylamide-2-methylpro panesulfonic acid 249g, N,N-DMAA 119g, redox initiator 1g, sodium hydroxide 49.1g, distilled water 573.7ml.
In technical solution of the present invention, described redox initiator initiator system of ammonium persulfate.
In technical solution of the present invention, described sodium hydroxide is the sodium hydrate solid of massfraction 96%.
The preparation method of fluid loss agent of the present invention, is made up of following steps:
(1) get part distilled water and sodium hydroxide, be configured to the sodium hydroxide solution that massfraction is 30 ~ 45%; Distilled water under remainder, add in the reactor of liner temperature resistance tetrafluoroethylene, add NVP, 2-acrylamide-2-methylpro panesulfonic acid, N successively, N-DMAA, stirs 1 ~ 3 hour, raw material is fully dissolved, slow heating, make system temperature rise to 38 ~ 42 DEG C, insulation 5 ~ 10min, adds redox initiator;
In (2) 10 minutes, copolyreaction starts, exothermic heat of reaction, and make whole temperature of reaction system continue to rise to 90 ~ 95 DEG C by 38 ~ 42 DEG C in 1 hour, be then incubated 1 ~ 2 hour, Temperature fall, temperature is down to 50 DEG C, obtains multipolymer blob of viscose;
(3) multipolymer blob of viscose blob of viscose crusher in crushing is become micelle in small, broken bits, the sodium hydroxide solution that micelle in small, broken bits and step (1) configure is mixed, slowly fully stir, micelle in small, broken bits is thoroughly dissolved, system is warming up to 85 ~ 90 DEG C, carries out neutralization reaction 1.5 ~ 3 hours, obtains multipolymer sodium sulfonate micelle, multipolymer sodium sulfonate micelle in 105 DEG C of dryings, pulverizing, to obtain final product.
The preparation method of preferred fluid loss agent is made up of following steps:
(1) get distilled water 73.7ml, sodium hydroxide 49.1g, be configured to sodium hydroxide solution;
(2) distilled water 500ml is got, add in the reactor of liner temperature resistance tetrafluoroethylene, add NVP 132g, 2-acrylamide-2-methylpro panesulfonic acid 249g, N successively, N-DMAA 119g, stirs 2 hours, raw material is fully dissolved, slow heating, make system temperature rise to 40 DEG C, insulation, adds redox initiator 1g;
In (3) 10 minutes, copolyreaction starts, exothermic heat of reaction, and make whole system temperature continue to rise to 90 DEG C by 40 DEG C in 1 hour, be then incubated 1 hour, rear temperature progressively declines again, and after 40 minutes, temperature is down to 50 DEG C, obtains multipolymer blob of viscose;
(4) multipolymer blob of viscose blob of viscose crusher in crushing is become micelle in small, broken bits, micelle in small, broken bits is mixed with sodium hydroxide solution, slowly fully stir, micelle in small, broken bits is thoroughly dissolved, system is warming up to 90 DEG C, neutralization reaction 2 hours, obtains multipolymer sodium sulfonate micelle, multipolymer sodium sulfonate micelle in 105 DEG C of dryings, pulverizing, to obtain final product.
The present invention is as follows relative to the beneficial effect of prior art:
(1) while this fluid loss agent significantly can reduce filter loss, the high temperature reaching 220 DEG C can also be resisted, the salt concn of antisaturation salt solution;
(2) this fluid loss agent is under 2.3SG density, and 220 DEG C of heat roll 16 hours, and high temperature and high pre ssure filtration is 10ml.
Embodiment
Be described in further details the present invention below by embodiment, these embodiments are only used for the present invention is described, do not limit the scope of the invention.
Embodiment 1 adopts following formula: NVP 132g, 2-acrylamide-2-methylpro panesulfonic acid 249g, N,N-DMAA 119g, redox initiator ammonium persulphate 1g, sodium hydroxide 49.1g, distilled water 573.7ml; Prepare fluid loss agent of the present invention as follows:
(1) get distilled water 73.7ml, sodium hydroxide 49.1g, be configured to sodium hydroxide solution; Get distilled water 500ml, add in the reactor of liner temperature resistance tetrafluoroethylene, add 132gN-vinyl pyrrolidone, 249g2-acrylamide-2-methylpro panesulfonic acid, 119gN, N-DMAA, stirs 2 hours, raw material is fully dissolved, slow heating, make system temperature rise to 40 DEG C, insulation, adds 1g redox initiator ammonium persulphate;
In (2) 10 minutes, copolyreaction starts, exothermic heat of reaction, and make whole system temperature continue to rise to 90 DEG C by 40 DEG C in 1 hour, be then incubated 1 hour, rear temperature progressively declines again, and after 40 minutes, temperature is down to 50 DEG C, obtains multipolymer blob of viscose;
(3) multipolymer blob of viscose blob of viscose crusher in crushing is become micelle in small, broken bits, micelle in small, broken bits is mixed with sodium hydroxide solution, slowly fully stir, micelle in small, broken bits is thoroughly dissolved, system is warming up to 90 DEG C, neutralization reaction 2 hours, obtains multipolymer sodium sulfonate micelle, multipolymer sodium sulfonate micelle in 105 DEG C of dryings, pulverizing, to obtain final product.
The present embodiment obtains the detection of anti-fluid loss agents performance:
(1) measure its add fresh water slurry after filter loss: testing sequence is as follows: measure 350ml distilled water, adds 1g sodium bicarbonate (NaHCO when stirring at low speed
3), 35g Britain evaluates soil, and high-speed stirring 20 minutes, adds 1.75g fluid loss agent, then high-speed stirring 20 minutes, rolls 16 hours, be cooled to room temperature 180 DEG C of heat, and high-speed stirring 20 minutes, measures its API filtration;
(2) measure its add 4% salt slurries after filter loss: testing sequence is as follows: measure 350ml distilled water, add 14.0gNaCl, and high-speed stirring 20 minutes, this solution i.e. 4% salt solution.Accurately measure 350ml4% salt solution, add 1g sodium bicarbonate (NaHCO when stirring at low speed
3), 35g Britain evaluates soil, and high-speed stirring 20 minutes, adds 3.15g fluid loss agent, then high-speed stirring 20 minutes, rolls 16 hours, be cooled to room temperature 180 DEG C of heat, and high-speed stirring 20 minutes, measures its API filtration;
(3) measure its add saturated salt water slurry after filter loss: testing sequence is as follows: measure 350ml distilled water, add 122.5gNaCl, high-speed stirring 20 minutes, this solution is saturated brine, accurately measure 350ml saturated brine, add 1g sodium bicarbonate (NaHCO when stirring at low speed
3), 35g Britain evaluates soil, and high-speed stirring 20 minutes, adds 4.2g fluid loss agent, then high-speed stirring 20 minutes, rolls 16 hours, be cooled to room temperature 180 DEG C of heat, and high-speed stirring 20 minutes, measures its API filtration;
(4) measure it and add filter loss in 100%Weigh3 organic salt drilling fluid: testing sequence is as follows: measure 350ml distilled water, adds 1g sodium bicarbonate (NaHCO
3), 35g Britain evaluates soil, and high-speed stirring 20 minutes, adds 5.25g fluid loss agent, high-speed stirring 20 minutes, adds 350g organic salt Weigh3, and high-speed stirring 20 minutes rolls 16 hours 180 DEG C of heat, be cooled to room temperature, high-speed stirring 20 minutes, measures its API filtration.
After above-mentioned steps measures, the API filtration value of this fluid loss agent in fresh water slurry, 4% salt slurries, saturated salt water slurry, 100%Weigh3 organic salt drilling fluid is as follows:
。
Embodiment 2 adopts following formula: NVP 150 parts, 2-acrylamide-2-methylpro panesulfonic acid 300 parts, N,N-DMAA 120 parts, redox initiator ammonium persulphate 0.5 part, 40 parts, sodium hydroxide, distilled water 600 parts; Prepare fluid loss agent of the present invention according to the following steps:
(1) get part distilled water and sodium hydroxide, be configured to the sodium hydroxide solution that massfraction is 40%; Distilled water under remainder, add in the reactor of liner temperature resistance tetrafluoroethylene, add NVP, 2-acrylamide-2-methylpro panesulfonic acid, N successively, N-DMAA, stirs 3 hours, raw material is fully dissolved, slow heating, make system temperature rise to 42 DEG C, insulation 5min, adds redox initiator ammonium persulphate;
In (2) 10 minutes, copolyreaction starts, exothermic heat of reaction, and make whole temperature of reaction system continue to rise to 90 DEG C by 42 DEG C in 1 hour, be then incubated 1 hour, Temperature fall, temperature is down to 50 DEG C, obtains multipolymer blob of viscose;
(3) multipolymer blob of viscose blob of viscose crusher in crushing is become micelle in small, broken bits, the sodium hydroxide solution that micelle in small, broken bits and step (1) configure is mixed, slowly fully stir, micelle in small, broken bits is thoroughly dissolved, system is warming up to 85 DEG C, carries out neutralization reaction 3 hours, obtains multipolymer sodium sulfonate micelle, multipolymer sodium sulfonate micelle in 105 DEG C of dryings, pulverizing, to obtain final product.
Embodiment 3 adopts following formula: NVP 150 parts, 2-acrylamide-2-methylpro panesulfonic acid 300 parts, N,N-DMAA 155 parts, redox initiator ammonium persulphate 3 parts, 50 parts, sodium hydroxide, distilled water 580 parts; Prepare fluid loss agent of the present invention according to the following steps:
(1) get part distilled water and sodium hydroxide, be configured to the sodium hydroxide solution that massfraction is 30%; Distilled water under remainder, add in the reactor of liner temperature resistance tetrafluoroethylene, add NVP, 2-acrylamide-2-methylpro panesulfonic acid, N successively, N-DMAA, stirs 1 hour, raw material is fully dissolved, slow heating, make system temperature rise to 40 DEG C, insulation 10min, adds redox initiator ammonium persulphate;
In (2) 10 minutes, copolyreaction starts, exothermic heat of reaction, and make whole temperature of reaction system continue to rise to 92 DEG C by 40 DEG C in 1 hour, be then incubated 1 hour, Temperature fall, temperature is down to 50 DEG C, obtains multipolymer blob of viscose;
(3) multipolymer blob of viscose blob of viscose crusher in crushing is become micelle in small, broken bits, the sodium hydroxide solution that micelle in small, broken bits and step (1) configure is mixed, slowly fully stir, micelle in small, broken bits is thoroughly dissolved, system is warming up to 90 DEG C, carries out neutralization reaction 1.5 hours, obtains multipolymer sodium sulfonate micelle, multipolymer sodium sulfonate micelle in 105 DEG C of dryings, pulverizing, to obtain final product.
Embodiment 4 adopts following formula: NVP 100 parts, 2-acrylamide-2-methylpro panesulfonic acid 200 parts, N,N-DMAA 100 parts, redox initiator ammonium persulphate 1.8 parts, 60 parts, sodium hydroxide, distilled water 700 parts; Prepare fluid loss agent of the present invention according to the following steps:
(1) get part distilled water and sodium hydroxide, be configured to the sodium hydroxide solution that massfraction is 45%; Distilled water under remainder, add in the reactor of liner temperature resistance tetrafluoroethylene, add NVP, 2-acrylamide-2-methylpro panesulfonic acid, N successively, N-DMAA, stirs 2.5 hours, raw material is fully dissolved, slow heating, make system temperature rise to 38 DEG C, insulation 8min, adds redox initiator ammonium persulphate;
In (2) 10 minutes, copolyreaction starts, exothermic heat of reaction, and make whole temperature of reaction system continue to rise to 95 DEG C by 38 DEG C in 1 hour, be then incubated 1.5 hours, Temperature fall, temperature is down to 50 DEG C, obtains multipolymer blob of viscose;
(3) multipolymer blob of viscose blob of viscose crusher in crushing is become micelle in small, broken bits, the sodium hydroxide solution that micelle in small, broken bits and step (1) configure is mixed, slowly fully stir, micelle in small, broken bits is thoroughly dissolved, system is warming up to 88 DEG C, carries out neutralization reaction 3 hours, obtains multipolymer sodium sulfonate micelle, multipolymer sodium sulfonate micelle in 105 DEG C of dryings, pulverizing, to obtain final product.
Embodiment 5 adopts following formula: NVP 125 parts, 2-acrylamide-2-methylpro panesulfonic acid 280 parts, N,N-DMAA 90 parts, redox initiator ammonium persulphate 2.5 parts, 42 parts, sodium hydroxide, distilled water 500 parts; Prepare fluid loss agent of the present invention according to the following steps:
(1) get part distilled water and sodium hydroxide, be configured to the sodium hydroxide solution that massfraction is 42%; Distilled water under remainder, add in the reactor of liner temperature resistance tetrafluoroethylene, add NVP, 2-acrylamide-2-methylpro panesulfonic acid, N successively, N-DMAA, stirs 2 hours, raw material is fully dissolved, slow heating, make system temperature rise to 38 DEG C, insulation 10min, adds redox initiator ammonium persulphate;
In (2) 10 minutes, copolyreaction starts, exothermic heat of reaction, and make whole temperature of reaction system continue to rise to 90 DEG C by 38 DEG C in 1 hour, be then incubated 1.5 hours, Temperature fall, temperature is down to 50 DEG C, obtains multipolymer blob of viscose;
(3) multipolymer blob of viscose blob of viscose crusher in crushing is become micelle in small, broken bits, the sodium hydroxide solution that micelle in small, broken bits and step (1) configure is mixed, slowly fully stir, micelle in small, broken bits is thoroughly dissolved, system is warming up to 85 DEG C, carries out neutralization reaction 2.5 hours, obtains multipolymer sodium sulfonate micelle, multipolymer sodium sulfonate micelle in 105 DEG C of dryings, pulverizing, to obtain final product.
Claims (7)
1. a high temperature resistance, anti-high salt concentration fluid loss agent, it is characterized in that: prepared by the feed composition of following parts by weight: NVP 100 ~ 150 parts, 2-acrylamide-2-methylpro panesulfonic acid 200 ~ 300 parts, N,N-DMAA 90 ~ 155 parts, redox initiator 0.5 ~ 3 part, 40 ~ 60 parts, sodium hydroxide, distilled water 500 ~ 700 parts.
2. fluid loss agent as claimed in claim 1, is characterized in that: the quality proportioning of described NVP, 2-acrylamide-2-methylpro panesulfonic acid, N,N-DMAA three kinds of starting monomers is: 2.5:5:2.
3. fluid loss agent as claimed in claim 1, it is characterized in that: described fluid loss agent is prepared by the feed composition of following quality proportioning: NVP 132g, 2-acrylamide-2-methylpro panesulfonic acid 249g, N, N-DMAA 119g, redox initiator 1g, sodium hydroxide 49.1g, distilled water 573.7ml.
4. the fluid loss agent as described in claim 1 or 3, is characterized in that: described redox initiator is ammonium persulphate.
5. the fluid loss agent as described in claim 1 or 3, is characterized in that: described sodium hydroxide is the sodium hydrate solid of massfraction 96%.
6. the preparation method of fluid loss agent as claimed in claim 1, is characterized in that: be made up of following steps:
(1) get part distilled water and sodium hydroxide, be configured to the sodium hydroxide solution that massfraction is 30 ~ 45%; Distilled water under remainder, add in the reactor of liner temperature resistance tetrafluoroethylene, add NVP, 2-acrylamide-2-methylpro panesulfonic acid, N successively, N-DMAA, stirs 1 ~ 3 hour, raw material is fully dissolved, slow heating, make system temperature rise to 38 ~ 42 DEG C, insulation 5 ~ 10min, adds redox initiator;
In (2) 10 minutes, copolyreaction starts, exothermic heat of reaction, and make whole temperature of reaction system continue to rise to 90 ~ 95 DEG C by 38 ~ 42 DEG C in 1 hour, be then incubated 1 ~ 2 hour, Temperature fall, temperature is down to 50 DEG C, obtains multipolymer blob of viscose;
(3) multipolymer blob of viscose blob of viscose crusher in crushing is become micelle in small, broken bits, the sodium hydroxide solution that micelle in small, broken bits and step (1) configure is mixed, slowly fully stir, micelle in small, broken bits is thoroughly dissolved, system is warming up to 85 ~ 90 DEG C, carries out neutralization reaction 1.5 ~ 3 hours, obtains multipolymer sodium sulfonate micelle, multipolymer sodium sulfonate micelle in 105 DEG C of dryings, pulverizing, to obtain final product.
7. the preparation method of fluid loss agent as claimed in claim 3, is characterized in that: be made up of following steps:
(1) get distilled water 73.7ml, sodium hydroxide 49.1g, be mixed with sodium hydroxide solution;
(2) distilled water 500ml is got, add in the reactor of liner temperature resistance tetrafluoroethylene, add NVP 132g, 2-acrylamide-2-methylpro panesulfonic acid 249g, N successively, N-DMAA 119g, stirs 2 hours, raw material is fully dissolved, slow heating, make system temperature rise to 40 DEG C, insulation, adds redox initiator 1g;
In (3) 10 minutes, copolyreaction starts, exothermic heat of reaction, and make whole system temperature continue to rise to 90 DEG C by 40 DEG C in 1 hour, be then incubated 1 hour, rear temperature progressively declines again, and after 40 minutes, temperature is down to 50 DEG C, obtains multipolymer blob of viscose;
(4) multipolymer blob of viscose blob of viscose crusher in crushing is become micelle in small, broken bits, micelle in small, broken bits is mixed with sodium hydroxide solution, slowly fully stir, micelle in small, broken bits is thoroughly dissolved, system is warming up to 90 DEG C, neutralization reaction 2 hours, obtains multipolymer sodium sulfonate micelle, multipolymer sodium sulfonate micelle in 105 DEG C of dryings, pulverizing, to obtain final product.
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Application publication date: 20151223 |