CN103396515B - A kind of high temperature resistance treated starch fluid loss agent and preparation method thereof - Google Patents
A kind of high temperature resistance treated starch fluid loss agent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of high temperature resistance treated starch fluid loss agent and preparation method thereof, described treated starch fluid loss agent and preparation method are raw material by starch, phenolic compound, alkenyl amide and olefin sulfonic acid, oil-phase solution is external phase, nonionogenic tenside is emulsifying agent, and reduction substrate and hydrogen acceptor substrate katalysis under, reaction generate a kind of starch graft copolymer.Fluid loss agent temperature resistance provided by the invention can reach 175 DEG C, and has good anti-salt and anticalcium ability simultaneously, and its preparation method is simple, and reaction conditions gentleness is controlled, and grafting efficiency is high, and speed of response is fast, with low cost.
Description
Technical field
The present invention relates to fluid loss agent used in oil/gas drilling and preparation method thereof, particularly relate to treated starch fluid loss agent and preparation method thereof.
Background technology
Along with the continuous increase of world energy sources demand, exploitation deep formation hydrocarbon resources has become inevitable, and this just has higher requirement to drilling technology.Drilling Fluid is as integral part important in drilling technology, and the quality of its performance is directly connected to drilling quality and drilling cost, even drilling well success or failure.Under deep formation high-temperature and high-pressure conditions, the filtration property of drilling fluid is the integral part of drilling fluid over-all properties, and under high-temperature and high-pressure conditions, the control of drilling fluid filtration relies on the fluid loss agent of high temperature resistance to realize.Starch based fluid loss agent has asepsis environment-protecting, with low cost, source is wide, anti-calcium and anti-salt ability is strong, uses very early as filtrate reducer for drilling fluid.But if temperature is more than 120 DEG C, starch will lose efficacy because of high temperature degradation, thus greatly limit its use range.At present, the method improving the heat-resisting property of starch based fluid loss agent is mainly realized by graft copolymerization vinyl monomer and etherificate, but the temperature resistance ability of these starch fluid loss agents by modification in fresh-water drilling fluid is still difficult to breakthrough 140 DEG C, and domestic and international rare several can the treated starch fluid loss agent product of temperature resistance 140 DEG C, under its hot conditions, anti-calcium and anti-salt performance is poor.
Therefore, need to utilize new method of modifying to improve the high temperature resistance of starch based fluid loss agent, anti-salt and anticalcium ability, to adapt to the needs of high temperature deep well probing.
Summary of the invention
For solving the problems of the technologies described above, the object of this invention is to provide a kind of high temperature resistance treated starch fluid loss agent and preparation method thereof, described technical scheme is as follows:
A kind of high temperature resistance treated starch fluid loss agent, described treated starch fluid loss agent is raw material by starch, phenolic compound, alkenyl amide and olefin sulfonic acid, oil-phase solution is external phase, nonionogenic tenside is emulsifying agent, and reduction substrate and hydrogen acceptor substrate katalysis under, reaction generate a kind of starch graft copolymer.
Described starch is enzymolysis under the effect of α-amylase, obtains enzymatic degradation of starch, and described enzymolysis process comprises as follows:
In the starch taken, add distilled water, compound concentration is the starch milk of 20.0wt% ~ 50.0wt%, and is heated in the water-bath of 25 ~ 96 DEG C by starch milk;
Add α-amylase in starch milk after the heating, stir and evenly, be warming up to 105 ~ 118 DEG C after sustained reaction 60 ~ 120min, deactivation 60 ~ 120min obtains enzymatic degradation of starch emulsion.
A kind of preparation method of high temperature resistance treated starch fluid loss agent comprises:
Alkenyl amide and alkenyl sulphonate are dissolved in deionized water solvent, and regulate lysate pH to be 6.0 ~ 8.0 with NaOH or the KOH aqueous solution of 2.0wt%, obtaining concentration is 20.0wt% ~ 50.0wt% mixed monomer solution;
Join in reactor by oil-phase solution and nonionogenic tenside, being uniformly mixed and obtaining having oleophilic hydrophil balance value HLB scope is the emulsion of 7.0 ~ 9.0;
Enzymatic degradation of starch emulsion is joined in emulsion, and adds phenolic compound, biological enzyme and reduction substrate, stir and obtain the microemulsion that oil/water volume ratio is 2 ~ 5:1;
Microemulsion was slowly warming up to 20 ~ 86 DEG C in 0.5 ~ 3.0 hour, and the hydrogen acceptor substrate of to be 20.0wt% ~ 50.0wt% mixed monomer solution and molar weight by concentration be phenolic compound molar weight 0.2 ~ 1.0 times joins in microemulsion reaction system, react and obtain the thick product of high temperature resistance treated starch fluid loss agent in 1.0 ~ 3.0 hours, then described thick product is obtained high temperature resistance treated starch fluid loss agent after precipitation, washing, extracting, vacuum-drying.
Compared with prior art, one or more embodiment of the present invention can have the following advantages by tool:
The present invention is to provide a kind of novel high temperature resistance modified starch series fluid loss agent, first phenolic compound is incorporated in starch molecular structure, improve the heat-resisting property of modified starch series fluid loss agent by strengthening molecular rigidity, and anti-salt and anticalcium ability; And what preparation method adopted is conversed phase micro emulsion copolymerization method, and this preparation method is simple, and reaction conditions gentleness is controlled, speed of response is fast, and percentage of grafting is high, is applicable to industrial applications and promotes.
Other features and advantages of the present invention will be set forth in the following description, and, partly become apparent from specification sheets, or understand by implementing the present invention.Object of the present invention and other advantages realize by technology specifically noted in specification sheets, claims and obtain.
Embodiment
Easy understand, according to technical scheme of the present invention, do not changing under connotation of the present invention, one of ordinary skill in the art can propose multiple frame mode of the present invention and making method.Therefore following embodiment is only illustrating of technical scheme of the present invention, and should not be considered as of the present invention all or be considered as restriction or the restriction of technical solution of the present invention.
A kind of high temperature resistance treated starch fluid loss agent, described treated starch fluid loss agent is raw material by starch, phenolic compound, alkenyl amide and olefin sulfonic acid, oil-phase solution is external phase, nonionogenic tenside is emulsifying agent, and reduction substrate and hydrogen acceptor substrate katalysis under, reaction generate a kind of starch graft copolymer.
Above-mentioned starch is enzymolysis under the effect of α-amylase, obtains enzymatic degradation of starch, and described enzymolysis process comprises as follows:
In the starch taken, add distilled water, compound concentration is the starch milk of 20.0wt% ~ 50.0wt%, and is heated in the water-bath of 25 ~ 96 DEG C by starch milk;
Add α-amylase in starch milk after the heating, stir and evenly, be warming up to 105 ~ 118 DEG C after sustained reaction 60 ~ 120min, deactivation 60 ~ 120min obtains enzymatic degradation of starch emulsion.
Above-mentioned starch is one or more in cereal starch, potato starch and legume starch;
Above-mentioned phenolic compound is one or more in following chemical general formula species range,
Above-mentioned alkenyl amide is acrylamide, N, N-DMAA, N, one or more in N-acrylamide, N-ethylene vinyl amine, N-vinyl methylacetamide, N-vinyl ethyl acetamide, diacetone-acryloamide(DAA), N, N-methylene-bis third ethernamine, N hydroxymethyl acrylamide;
Above-mentioned olefin sulfonic acid is one or more among vinyl sulfonic acid, allyl sulphonic acid, styrene sulfonic acid, acryloyl-oxy butyl sulfonic acid, 2-acrylamido dodecyl sodium sulfonate, 2-acrylamido tetradecyl sulfonic acid, 2-acrylamido hexadecyl sulfonic acid, 2-acryloxy-2-methyl propane sulfonic acid, 2-acrylamide-2-methylpro panesulfonic acid.
R in above-mentioned phenolic compound chemical general formula
1, R
2, R
3, R
4, R
6and R
8for H, OH, CH
3, CF
3, C
2h
5, C
2f
5, NH
2, NHCH
3, N (CH
3)
2, OCH
3, NHCOCH
3, Cl, Br, I; R
5and R
7for N
+(CH
3)
3, NO
2, CN, CONH
2, SO
3h, SO
3na, SO
3k, CHO, COOH, COONa, COOK.
Above-mentioned starch is 5 ~ 10:1 with the molar mass ratio of phenolic compound;
The molar mass ratio of above-mentioned phenolic compound, alkenyl amide and olefin sulfonic acid is 1 ~ 5:2 ~ 10:3 ~ 15.
A preparation method for high temperature resistance treated starch fluid loss agent, comprising:
Alkenyl amide and alkenyl sulphonate are dissolved in deionized water solvent, and regulate lysate pH to be 6.0 ~ 8.0 with NaOH or the KOH aqueous solution of 2.0wt%, obtaining concentration is 20.0wt% ~ 50.0wt% mixed monomer solution;
Join in reactor by oil-phase solution and nonionogenic tenside, being uniformly mixed and obtaining having oleophilic hydrophil balance value HLB scope is the emulsion of 7.0 ~ 9.0;
Enzymatic degradation of starch emulsion is joined in emulsion, and adds phenolic compound, biological enzyme and reduction substrate, stir and obtain the microemulsion that oil/water volume ratio is 2 ~ 5:1;
Microemulsion was slowly warming up to 20 ~ 86 DEG C in 0.5 ~ 3.0 hour, and the hydrogen acceptor substrate of to be 20.0wt% ~ 50.0wt% mixed monomer solution and molar weight by concentration be phenolic compound molar weight 0.2 ~ 1.0 times joins in microemulsion reaction system, react and obtain the thick product of high temperature resistance treated starch fluid loss agent in 1.0 ~ 3.0 hours, then described thick product is obtained high temperature resistance treated starch fluid loss agent after precipitation, washing, extracting, vacuum-drying.
High temperature modified starch fluid loss agent preparation method will be resisted by following examples to be below described in detail:
Embodiment 1
40g W-Gum is added in the beaker that 100mL distilled water is housed, pour into after fully stirring into pasty state in reactor, heat in the water-bath of 65 DEG C.Under agitation condition, add 0.04g α-amylase, constant temperature keeps 120min, intensification oil bath temperature to 110 DEG C, and constant temperature keeps 60min, namely obtains enzymatic degradation of starch emulsion.
2-acrylamide-2-methylpro panesulfonic acid is made in water the solution of 15.0wt%, is neutralized to pH=6.0 by the KOH solution of 50.0wt%, dry to constant weight at being placed in vacuum drying oven 20 DEG C.
5.61 grams of acrylamides and 19.34g2-acrylamide-2-methylpro panesulfonic acid potassium are dissolved in the water of 60mL, regulates pH to 7.5 namely to obtain mixed monomer solution with the KOH aqueous solution of 2.0wt%.
In the reactor that temperature regulating device, reflux condensate device and constant pressure addition device are housed, add 400mL cyclohexane, add 35.0gSpan80 and 12.0gTween80 again, stir 30min, under agitation, enzymatic degradation of starch emulsion, 6.0g2,4-dihydroxy benzenes sulfonic acid potassium, 0.08g horseradish peroxidase and 0.96g methyl ethyl diketone is slowly added in reactor.In 1 hour, slowly raise the temperature to 50 DEG C of reaction system in reactor, and at the uniform velocity dropping mixed monomer solution and concentration are the H of 5.0wt% simultaneously
2o
210.0mL, in reaction system, continues reaction 3 hours, namely obtains the thick product of high temperature resistance treated starch fluid loss agent.
Filter after adding 350mL dehydrated alcohol precipitation, successively use each 3 times of washing with acetone product, be that the Glacial acetic acid-ethylene glycol mixed solvent of 3:2 is for extractant was to product Soxhlet extractor extracting 24 hours again with volume ratio, at 25 DEG C, vacuum-drying is to constant weight, namely obtain high temperature resistance treated starch fluid loss agent product, its molecular structure is as follows:
Embodiment 2
40g tapioca (flour) is added in the beaker that 40mL distilled water is housed, pour into after fully stirring into pasty state in reactor, heat in the water-bath of 96 DEG C, under agitation condition, add 0.008g α-amylase, constant temperature keeps 120min, intensification oil bath temperature to 118 DEG C, constant temperature keeps 60min, namely obtains enzymatic degradation of starch emulsion.
Styrene sulfonic acid is made in water the solution of 15.0wt%, is neutralized to pH=6.0 by the NaOH solution of 50.0wt%, dry to constant weight at being placed in vacuum drying oven 20 DEG C.
6.61gN, N-DMAA and 20.62g sodium p styrene sulfonate are dissolved in the water of 100mL, regulates pH to 7.0 to obtain mixed monomer solution with the NaOH aqueous solution of 2.0wt%.
In the reactor that temperature regulating device, reflux condensate device and constant pressure addition device are housed, add 480mL toluene, then add 26.91gSpan60 and 21.03gOP-10, stir 60min.Under agitation condition, in reactor, slowly add enzymatic degradation of starch emulsion, 4.20g pyrogallol, 0.06g soybean peroxidase and 1.2g methyl ethyl diketone.In 3 hours, slowly raise the temperature to 86 DEG C of reaction system in reactor, and at the uniform velocity dropping mixed monomer solution and concentration are the H of 5.0wt% simultaneously
2o
210.0mL, in reaction system, continues reaction 1 hour, namely obtains the thick product of high temperature resistance treated starch fluid loss agent.
Filter after adding 350mL dehydrated alcohol precipitation, successively use each 3 times of washing with acetone product, be that the Glacial acetic acid-ethylene glycol mixed solvent of 3:2 is for extractant was to product Soxhlet extractor extracting 24 hours again with volume ratio, at 25 DEG C, vacuum-drying is to constant weight, namely obtain high temperature resistance treated starch fluid loss agent product, its molecular structure is as follows:
Embodiment 3
40g wheat starch is added in the beaker that 160mL distilled water is housed, pour into after fully stirring into pasty state in reactor, heat in the water-bath of 25 DEG C, under agitation condition, add 0.2g α-amylase, constant temperature keeps 120min, intensification oil bath temperature to 105 DEG C, very surely keep 120min, namely obtain enzymatic degradation of starch emulsion.
2-acrylamide-2-methylpro panesulfonic acid is made in water the solution of 15.0wt%, is neutralized to pH=7.0 by the NaOH solution of 50.0wt%, dry to constant weight at being placed in vacuum drying oven 20 DEG C.
5.0gN-n-methylolacrylamide and 11.46g2-acrylamide-2-methylpro panesulfonic acid sodium are dissolved in the water of 50mL, regulates pH to 8.0 namely to obtain mixed monomer solution with the NaOH aqueous solution of 2.0wt%.
In the reactor that temperature regulating device, reflux condensate device and constant pressure addition device are housed, add 600mL o-Xylol, then add 62.52gSpan60 and 18.20gTween60, stir 90min.Under agitation condition, in reactor, slowly add enzymatic degradation of starch emulsion, 8.0g P-hydroxybenzoic acid sodium, 0.096g horseradish peroxidase and 1.5g methyl ethyl diketone.In 0.5 hour, slowly raise the temperature to 45 DEG C of reaction system in reactor, and at the uniform velocity dropping mixed monomer solution and concentration are the H of 5.0wt% simultaneously
2o
213.6mL is in reaction system.Continue reaction 3.0 hours, namely obtain the thick product of high temperature resistance treated starch fluid loss agent.
Filter after adding 350mL dehydrated alcohol precipitation, successively use each 3 times of washing with acetone product, be that the Glacial acetic acid-ethylene glycol mixed solvent of 3:2 is for extractant was to product Soxhlet extractor extracting 24 hours again with volume ratio, at 25 DEG C, vacuum-drying is to constant weight, namely obtain high temperature resistance treated starch fluid loss agent product, its molecular structure is as follows:
Embodiment 4
The heat-resisting property of treated starch fluid loss agent product, anti-salt contamination and anticalcium invade merit rating.Testing method: adopt ZB/TE13004-90: test procedure for drilling fluids
1, test in fresh water-based slurry
Fresh water-based is starched: stir in cup at height and add 400mL tap water, under constantly stirring, quantitatively add 16.0 calcium bentonites and 0.8gNa
2cO
3.Stir 20 minutes, at least stop twice therebetween, to scrape adhesion wilkinite on the wall, maintenance 24 hours in sealed vessel.
Treated starch-fresh-water drilling fluid system: quantitatively take treated starch fluid loss agent, is joined in fresh water-based slurry, maintenance 24 hours in sealed vessel after fully stirring.
Fresh water-based slurry and treated starch-fresh-water drilling fluid system high-speed stirring are loaded after 5 minutes in high temperature ageing tank, 175 DEG C are boiling hot 16 hours, and committing a breach of etiquette with press filtration in normal temperature measures the filter loss of drilling fluid with high pressure high temperature filter tester, its result is as following table 1:
Table 1
| Experiment slurry | 175 DEG C/16 hours |
| FL API | FL HTHP | |
| Fresh water-based is starched | 86.0 | Full leakage |
| Fresh water-based slurry+1.8wt% embodiment 1 sample | 13.2 | 28.4 |
| Fresh water-based slurry+2.5wt% embodiment 2 sample | 14.8 | 34.0 |
| Fresh water-based slurry+2.8wt% embodiment 2 sample | 13.8 | 29.6 |
| Fresh water-based slurry+2.8wt% embodiment 3 sample | 14.6 | 29.8 |
In table, FL
aPIpress filtration vector in-normal temperature; FL
hTHP-high temperature and high pre ssure filtration, measure temperature identical with corresponding aging temperature, test pressure is 3.5MPa.
2, test in the water base slurry of saturated salt
The water base slurry of saturated salt: stir in cup at height and add 400mL tap water, add 144.0g under constant agitation, 16.0g calcium bentonite and 0.8gNa
2cO
3.Stir 20 minutes, at least stop twice therebetween, to scrape adhesion wilkinite on the wall, maintenance 24 hours in sealed vessel.
Treated starch-saturated salt-water drilling fluid system: quantitatively take treated starch fluid loss agent, is joined in the water base slurry of saturated salt, maintenance 24 hours in sealed vessel after fully stirring.
Water base for saturated salt slurry and treated starch-saturated salt-water drilling fluid system high-speed stirring are loaded after 5 minutes in high temperature ageing tank, 175 DEG C are boiling hot 16 hours, and committing a breach of etiquette with press filtration in normal temperature measures the filter loss of drilling fluid with high pressure high temperature filter tester, its result is as following table 2:
Table 2
3, test in calcic base slurry
Calcic base is starched: stir in cup at height and add 400mL tap water, add 2.0gCaCl under constant agitation
2, 16.0g calcium bentonite and 0.8gNa
2cO
3.Stir 20 minutes, at least stop twice therebetween, to scrape adhesion wilkinite on the wall, maintenance 24 hours in sealed vessel.
Treated starch-calcic drilling fluid system; Quantitatively take treated starch fluid loss agent, joined in calcic base slurry, maintenance 24 hours in sealed vessel after fully stirring.
Calcic base slurry and treated starch-calcic drilling fluid system high-speed stirring are loaded after 5 minutes in high temperature ageing tank, 175 DEG C are boiling hot 16 hours, and committing a breach of etiquette with press filtration in normal temperature measures the filter loss of drilling fluid with high pressure high temperature filter tester, its result is as following table 3:
Table 3
Above test result shows, in treated starch-fresh-water drilling fluid system, after 175 DEG C of aging 16h, when the concentration of the treated starch fluid loss agent adding preparation in above-described embodiment 1 ~ 3 is respectively 1.8wt%, 2.5wt% and 2.8wt%, and can by the FL of drilling fluid
aPIbe reduced to below 15.0mL; When adding concentration and being respectively 1.8wt%, 2.8wt% and 2.8wt%, can by the FL of drilling fluid
hTHPbe reduced to below 30.0mL.Compare treated starch-fresh-water drilling fluid system, the appropriate high temperature resistance treated starch that improves is at treated starch-saturated salt-water drilling fluid system and treated starch-calcic (0.5wt%CaCl
2) dosage of drilling fluid system, effectively can reduce the filter loss of drilling fluid system.It can be said that bright, the temperature resistance ability of the heat resisting fluid loss reducing agent that this patent provides can reach 175 DEG C, and has good anti-salt and anticalcium ability.Therefore, this fluid loss agent product uses under being suitable for the geologic condition of deep-well, the high temperature of ultra deep well, high salt or high calcium.
The principal feature of high temperature resistant anti-calcium and anti-salt rigidity fluid loss agent can be drawn: starch structure unit, introduce phenyl ring as rigid radical from above embodiment, reduce the attached effect of desorption under high temperature that fluid loss agent molecule causes because of thermal motion, improve treated starch fluid loss agent performance under the high temperature conditions, and anti-salt and anticalcium ability.In addition, in the order of addition of synthesis material, take the expedite that the preferential and phenolic compound of starch structure unit reacts, thus the Sauerstoffatom in starch structure unit is directly connected with the carbon atom on phenyl ring in phenolic compound, lonely on Sauerstoffatom to produce p-to the π-electron on p electronics and phenyl ring pi-conjugated, thus improve the thermostability of molecular entities.In addition, conversed phase micro emulsion copolymerization method impels the free radical in reaction system steadily to generate fast, improves stability and the speed of reaction of polyreaction, and its reaction conditions gentleness is controlled, and grafting efficiency is high.
Although the embodiment disclosed by the present invention is as above, the embodiment that described content just adopts for the ease of understanding the present invention, and be not used to limit the present invention.Technician in any the technical field of the invention; under the prerequisite not departing from the spirit and scope disclosed by the present invention; any amendment and change can be done what implement in form and in details; but scope of patent protection of the present invention, the scope that still must define with appending claims is as the criterion.
Claims (5)
1. a high temperature resistance treated starch fluid loss agent, it is characterized in that, described treated starch fluid loss agent is raw material by starch, phenolic compound, alkenyl amide and olefin sulfonic acid, oil-phase solution is external phase, nonionogenic tenside is emulsifying agent, and reduction substrate and hydrogen acceptor substrate katalysis under, reaction generate a kind of starch graft copolymer;
Described starch is enzymolysis under the effect of α-amylase, obtains enzymatic degradation of starch, and described enzymolysis process comprises as follows:
In the starch taken, add distilled water, compound concentration is the starch milk of 20.0wt% ~ 50.0wt%, and is heated in the water-bath of 25 ~ 96 DEG C by starch milk;
Add α-amylase in starch milk after the heating, stir and evenly, be warming up to 105 ~ 118 DEG C after sustained reaction 60 ~ 120min, deactivation 60 ~ 120min obtains enzymatic degradation of starch emulsion;
Enzymatic degradation of starch emulsion is joined in emulsion, and adds phenolic compound, biological enzyme and reduction substrate, stir and obtain the microemulsion that oil/water volume ratio is 2 ~ 5: 1; Described biological enzyme is horseradish peroxidase or soybean peroxidase;
Described starch is 5 ~ 10: 1 with the molar mass ratio of phenolic compound;
The molar mass ratio of described phenolic compound, alkenyl amide and olefin sulfonic acid is 1 ~ 5: 2 ~ 10: 3 ~ 15;
Described reduction substrate is methyl ethyl diketone; Described hydrogen acceptor substrate is H
2o
2.
2. high temperature resistance treated starch fluid loss agent according to claim 1, is characterized in that,
Described starch is one or more in cereal starch, potato starch and legume starch;
Described phenolic compound is one or more in following chemical general formula species range,
Described alkenyl amide is acrylamide, N, N-DMAA, N, one or more in N-acrylamide, N-ethylene vinyl amine, N-vinyl methylacetamide, N-vinyl ethyl acetamide, diacetone-acryloamide(DAA), N, N-methylene-bis third ethernamine, N hydroxymethyl acrylamide;
Described olefin sulfonic acid is one or more among vinyl sulfonic acid, allyl sulphonic acid, styrene sulfonic acid, acryloyl-oxy butyl sulfonic acid, 2-acrylamido dodecyl sodium sulfonate, 2-acrylamido tetradecyl sulfonic acid, 2-acrylamido hexadecyl sulfonic acid, 2-acryloxy-2-methyl propane sulfonic acid, 2-acrylamide-2-methylpro panesulfonic acid;
R in described phenolic compound chemical general formula
1, R
2, R
3, R
4, R
6and R
8for H, OH, CH
3, CF
3, C
2h
5, C
2f
5, NH
2, NHCH
3, N (CH
3)
2, OCH
3, NHCOCH
3, Cl, Br, I; R
5and R
7for N
+(CH
3)
3, NO
2, CN, CONH
2, SO
3h, SO
3na, SO
3k, CHO, COOH, COONa, COOK.
3. the preparation method of high temperature resistance treated starch fluid loss agent according to claim 1, it is characterized in that, described method comprises:
Alkenyl amide and alkenyl sulphonate are dissolved in deionized water solvent, and regulate lysate pH to be 6.0 ~ 8.0 with NaOH or the KOH aqueous solution of 2.0wt%, obtaining concentration is 20.0wt% ~ 50.0wt% mixed monomer solution;
Join in reactor by oil-phase solution and nonionogenic tenside, being uniformly mixed and obtaining having oleophilic hydrophil balance value HLB scope is the emulsion of 7.0 ~ 9.0;
Enzymatic degradation of starch emulsion is joined in emulsion, and adds phenolic compound, biological enzyme and reduction substrate, stir and obtain the microemulsion that oil/water volume ratio is 2 ~ 5: 1;
Microemulsion was slowly warming up to 20 ~ 86 DEG C in 0.5 ~ 3.0 hour, and the hydrogen acceptor substrate of to be 20.0wt% ~ 50.0wt% mixed monomer solution and molar weight by concentration be phenolic compound molar weight 0.2 ~ 1.0 times joins in microemulsion reaction system, react and obtain the thick product of high temperature resistance treated starch fluid loss agent in 1.0 ~ 3.0 hours, then described thick product is obtained high temperature resistance treated starch fluid loss agent after precipitation, washing, extracting, vacuum-drying.
4. the preparation method of high temperature resistance treated starch fluid loss agent according to claim 3, is characterized in that,
Described alkenyl sulphonate is solution olefin sulfonic acid being configured in water 15.0wt%, and is neutralized to pH=6.0 ~ 7.0 by the KOH solution of 50.0wt%, dries to constant weight and obtain at being placed in vacuum drying oven 20 DEG C;
The concentration of described nonionogenic tenside in oil-phase solution is 10.0wt% ~ 20.0wt%;
The concentration of described biological enzyme in microemulsion is 0.005wt% ~ 0.05wt%, and the molar weight of reduction substrate is 0.05 ~ 0.2 times of alkenyl amide, olefin sulfonic acid and phenolic compound integral molar quantity.
5. the preparation method of high temperature resistance treated starch fluid loss agent according to claim 3, is characterized in that,
Described oil-phase solution is one or more in benzene, toluene, o-Xylol, silicone oil, white oil, kerosene, normal heptane, cyclohexane, normal hexane, octane-iso;
Described nonionogenic tenside is one or more in Determination of Polyoxyethylene Non-ionic Surfactants, polyol-based non-ionic surfactant, alkylol amide type nonionogenic tenside.
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| CN114163568B (en) * | 2020-09-11 | 2023-12-12 | 中国石油化工股份有限公司 | Modified starch filtrate reducer and preparation method and application thereof |
| CN114437296A (en) * | 2020-10-31 | 2022-05-06 | 中国石油天然气股份有限公司 | Filtrate reducer and preparation method thereof |
| CN112175593B (en) * | 2020-11-02 | 2022-08-16 | 中国石油化工股份有限公司 | High-temperature-resistant drilling fluid and preparation method thereof |
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