CN107353373B - A kind of preparation method of drilling fluid sulfomethylated humic acid potassium graft polymers fluid loss additive - Google Patents

A kind of preparation method of drilling fluid sulfomethylated humic acid potassium graft polymers fluid loss additive Download PDF

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CN107353373B
CN107353373B CN201710714840.8A CN201710714840A CN107353373B CN 107353373 B CN107353373 B CN 107353373B CN 201710714840 A CN201710714840 A CN 201710714840A CN 107353373 B CN107353373 B CN 107353373B
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parts
fluid loss
loss additive
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graft polymers
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CN107353373A (en
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鲍荣
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Civil Rights Dongxing Mud Material Co., Ltd.
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Civil Rights Dongxing Mud Material Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F289/00Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/02Well-drilling compositions
    • C09K8/03Specific additives for general use in well-drilling compositions
    • C09K8/035Organic additives

Abstract

The invention discloses a kind of drilling fluid preparation methods of sulfomethylated humic acid potassium graft polymers fluid loss additive, with potassium humate, acrylamide, alkyl acrylic, 2- acrylamide-2-methylpro panesulfonic acid, n-vinyl pyrrolidone etc. is raw material, heat resisting fluid loss reducing agent is prepared by aqueous solution polymerization method, it synthesizes optimum condition are as follows: 30 ~ 50 parts of potassium humate, 15 ~ 25 parts of acrylamide, 5 ~ 15 parts of alkyl acrylic, 10 ~ 20 parts of 2- acrylamide-2-methylpro panesulfonic acid, 5 ~ 15 parts of n-vinyl pyrrolidone.The present invention causes monomer by redox initiator and polymerization reaction occurs, obtain a kind of macromolecular graft polymers fluid loss additive, the product has good filtrate loss controllability in fresh water, saturated brine and compound salt-water drilling fluid, is resistant to 200 DEG C of high temperature, easy to use.

Description

A kind of preparation of drilling fluid sulfomethylated humic acid potassium graft polymers fluid loss additive Method
Technical field
The present invention relates to filtrate reducer for drilling fluid preparation field, in particular to a kind of drilling fluid is connect with sulfomethylated humic acid potassium The preparation method of branch polymer filtrate reducer.
Background technique
The loss of drilling fluid is not only resulted in when drilling fluid filtration is excessive, can also cause borehole well instability, cave-in, dirt Contaminate the various problems such as reservoir.Fluid loss additive is one of maximum material of drillng operation dosage, and suitable drop is added in drilling fluid Fluid loss agents can reach good filtrate reducing effect.Once heat resisting fluid loss reducing agent is degraded in drilling fluid, drilling fluid resists Warm nature, which declines to a great extent, to cause drilling fluid rheology to be deteriorated, drilling fluid flocculation and delamination, or even the pernicious leak-off of appearance, mud cake thicken The problems such as, cause the various accidents such as bit freezing, burying, well slough.Common sulfonated phenol formaldehyde resin class fluid loss additive domestic at present and sulphur It is good to change walchowite filtration reduction effect, is resistant to 180 DEG C of high temperature, but dosage is larger, and is glutinous in the presence of having in salt water when in use Degree loss, is easy the defects of being polluted by high valence ion, seriously limits its scope of application.
In addition with the increasing of oil extraction, many oil fields all enter high temperature deep layer oil-producing region, and exploitation difficulty is increasingly Greatly, partial mining area requirement fluid loss additive is resistant to 200 DEG C or more high temperature.Temperature-resistant and anti-salt type polymerize species fluid loss additive in oil field In exploitation have very big application potential, the present invention develop one kind can fluid loss additive resistant to high temperatures and salt resistance, can solve Certainly drilling fluid filtration problems of too during deep reservoir oil-gas mining provides new breakthrough for the exploitation of high temperature Deep Oil And Gas Exploration Mouthful.
Summary of the invention
The purpose of the present invention is to provide a kind of drilling fluid systems of sulfomethylated humic acid potassium graft polymers fluid loss additive Preparation Method, the fluid loss additive have good filtrate loss controllability in fresh water, saturated brine and compound salt-water drilling fluid, are resistant to 200 DEG C of high temperature, it is easy to use.
A kind of preparation method of drilling fluid heat resisting fluid loss reducing agent, it is characterised in that method includes the following steps:
1) 60 ~ 100 parts of deionized waters are added in the reaction kettle equipped with 30 ~ 50 parts of potassium humates, after dissolution is stirred at room temperature, PH to 10 ~ 11 is adjusted with alkaline reagent, 6 ~ 10 parts by weight of formaldehyde, 6 ~ 10 parts by weight sulfonating agent sodium hydrogensulfites are then added, stir It mixes and is warming up to 70 ~ 75 DEG C, cool down after reacting 3 ~ 4h;
2) by 15 ~ 25 parts of acrylamides, 5 ~ 15 parts of alkyl acrylics, 10 ~ 20 parts of 2- acrylamido -2- methyl-prop sulphurs Reaction kettle in step 1) is added after being dissolved in 70 ~ 150 parts of deionized waters in acid, 5 ~ 15 parts of n-vinyl pyrrolidone, stirs 0.5h, 0.13 ~ 0.25 part of initiation auxiliary agent lactic acid-chromium base bentonite clay material, heating, by 0.27 ~ 0.5 initiator (persulfuric acid are added simultaneously Sodium, sodium hydrogensulfite) wiring solution-forming, it is slowly alternately added in reaction kettle, time for adding 0.5h, 55 ~ 60 after being added dropwise DEG C heat preservation 4h, discharging, cooling obtain sulfomethylated humic acid potassium graft polymers fluid loss additive.
The utility model has the advantages that the present invention provides a kind of preparation of drilling fluid sulfomethylated humic acid potassium graft polymers fluid loss additive Method, the fluid loss additive saline-alkaline tolerance is strong, and raw material relatively easily obtains, and process, which joined, during the preparation process causes auxiliary agent cream Acid-chromium base bentonite clay material is a kind of high-efficiency activated substance, has surprising catalytic performance, is conducive to synthetic sample mistake The polymerization of monomer in journey, within the required range by molecular chain length control.With acrylamide, alkyl acrylic, 2- acrylamide Base -2- methyl propane sulfonic acid, the product that n-vinyl pyrrolidone is principal monomer synthesis, heat and salinity tolerance ability is prominent, and its Drilling fluid filtration can be greatly lowered in the dosage of low concentration in drilling fluid.
Specific embodiment
Embodiment 1
100 parts of deionized waters are added in the reaction kettle equipped with 50 parts of potassium humates, after dissolution is stirred at room temperature, are tried with alkalinity Agent adjusts pH to 10 ~ 11, and 10 parts by weight of formaldehyde, 10 parts by weight sulfonating agent sodium hydrogensulfites are then added, and stirring is warming up to 70 ~ 75 DEG C, cool down after reacting 3 ~ 4h,
By 25 parts of acrylamides, 5 parts of alkyl acrylics, 10 parts of 2- acrylamide-2-methylpro panesulfonic acids, 10 parts of N- ethylene Reaction kettle in step 1) is added after being dissolved in 100 parts of deionized waters in base pyrrolidones, stirs 0.5h, while 0.2 part of initiation is added Auxiliary agent lactic acid-chromium base bentonite clay material, heating, by 0.4 part of initiator (sodium peroxydisulfate, sodium hydrogensulfite, n sodium peroxydisulfate: n Sodium sulfite=1.3:1) wiring solution-forming, it is slowly alternately added in reaction kettle, time for adding 0.5h, 55 ~ 60 after being added dropwise DEG C heat preservation 4h, discharging, cooling obtain sulfomethylated humic acid potassium graft polymers fluid loss additive.
Above-mentioned lactic acid-chromium base bentonite clay material the preparation method is as follows:
7.08 parts of chromic nitrates, 18.91 parts of zinc nitrates, 7.35 parts of aluminum nitrates and 5.68 parts of ferric nitrates are dissolved in 100 by step 1 Mixing salt solution is obtained in part water;5.35 parts of sodium hydroxides and 2.84 parts of sodium carbonate are dissolved in 50 parts, mixing alkali soluble is configured to Mixed ammonium/alkali solutions are slowly dropped in the mixing salt solution being vigorously stirred by liquid, stop being added dropwise after salt-mixture precipitates completely mixed Aqueous slkali is closed, washing filtering after taking bottom sediment to stir crystallization at 70 DEG C for 24 hours, drying for standby;
Step 2 evaporates excessive hydrochloric acid after sufficiently reacting 36 parts of neodymia with 4 parts of mixed in hydrochloric acid, be added excessive water, then plus Enter ammonium hydroxide and precipitated completely to rare earth, filters, be washed to no chloride ion, obtain neodymium hydroxide, neodymium hydroxide is mixed with excessive water, Suspension is obtained, is heated to that lactic acid aqueous solution insulation reaction 5h is added after 60 DEG C while stirring, product mistake is precipitated in evaporation excessive water Filter be dried to obtain lactic acid neodymium compound, after lactic acid neodymium compound is mixed with product in step 1 addition 50 parts of sodium bentonites into Row is mediated and obtains lactic acid-chromium base bentonite clay material.Embodiment 2
Identical with embodiment 1, difference is: 30 parts of potassium humate of addition, 60 parts of deionized water, 6 parts of formaldehyde, and sulfurous 6 parts of sour hydrogen sodium;15 parts of acrylamide of addition, 10 parts of alkyl acrylic, 15 parts of 2- acrylamide-2-methylpro panesulfonic acid, N- second 15 parts of vinyl pyrrolidone are dissolved in 110 parts of deionized waters, and 0.17 part of initiation auxiliary agent lactic acid-chromium base bentonite clay material is added, 0.34 part of initiator.
Embodiment 3
Identical with embodiment 1, difference is: 30 parts of potassium humate of addition, 60 parts of deionized water, 6 parts of formaldehyde, and sulfurous 6 parts of sour hydrogen sodium;15 parts of acrylamide of addition, 15 parts of alkyl acrylic, 15 parts of 2- acrylamide-2-methylpro panesulfonic acid, N- second 5 parts of vinyl pyrrolidone are dissolved in 100 parts of deionized waters, are added 0.16 part of initiation auxiliary agent lactic acid-chromium base bentonite clay material, and 0.32 Part initiator.
Embodiment 4
Identical with embodiment 1, difference is: 35 parts of potassium humate of addition, 70 parts of deionized water, 7 parts of formaldehyde, and sulfurous 7 parts of sour hydrogen sodium;15 parts of acrylamide of addition, 5 parts of alkyl acrylic, 20 parts of 2- acrylamide-2-methylpro panesulfonic acid, N- ethylene 10 parts of base pyrrolidones are dissolved in 100 parts of deionized waters, are added 0.17 part of initiation auxiliary agent lactic acid-chromium base bentonite clay material, and 0.34 Part initiator.
Embodiment 5
Identical with embodiment 1, difference is: 40 parts of potassium humate of addition, 80 parts of deionized water, 8 parts of formaldehyde, and sulfurous 8 parts of sour hydrogen sodium;20 parts of acrylamide of addition, 5 parts of alkyl acrylic, 15 parts of 2- acrylamide-2-methylpro panesulfonic acid, N- ethylene 10 parts of base pyrrolidones are dissolved in 100 parts of deionized waters, are added 0.18 part of initiation auxiliary agent lactic acid-chromium base bentonite clay material, and 0.36 Part initiator.
Embodiment 6
Identical with embodiment 1, difference is: 40 parts of potassium humate of addition, 80 parts of deionized water, 8 parts of formaldehyde, and sulfurous 8 parts of sour hydrogen sodium;20 parts of acrylamide of addition, 10 parts of alkyl acrylic, 15 parts of 2- acrylamide-2-methylpro panesulfonic acid, N- second 5 parts of vinyl pyrrolidone are dissolved in 100 parts of deionized waters, are added 0.18 part of initiation auxiliary agent lactic acid-chromium base bentonite clay material, and 0.36 Part initiator.
Embodiment 7
Identical with embodiment 1, difference is: 45 parts of potassium humate of addition, 90 parts of deionized water, 9 parts of formaldehyde, and sulfurous 9 parts of sour hydrogen sodium;20 parts of acrylamide of addition, 5 parts of alkyl acrylic, 15 parts of 2- acrylamide-2-methylpro panesulfonic acid, N- ethylene 15 parts of base pyrrolidones are dissolved in 110 parts of deionized waters, are added 0.2 part of initiation auxiliary agent lactic acid-chromium base bentonite clay material, and 0.4 part Initiator.
Embodiment 8
Identical with embodiment 1, difference is: 50 parts of potassium humate of addition, 100 parts of deionized water, 10 parts of formaldehyde, sub- 10 parts of sodium bisulfate;25 parts of acrylamide of addition, 5 parts of alkyl acrylic, 15 parts of 2- acrylamide-2-methylpro panesulfonic acid, N- 5 parts of vinyl pyrrolidone are dissolved in 100 parts of deionized waters, are added 0.2 part of initiation auxiliary agent lactic acid-chromium base bentonite clay material, and 0.4 Part initiator.
Embodiment 9
Identical with embodiment 1, difference is: 45 parts of potassium humate of addition, 90 parts of deionized water, 9 parts of formaldehyde, and sulfurous 9 parts of sour hydrogen sodium;25 parts of acrylamide of addition, 5 parts of alkyl acrylic, 15 parts of 2- acrylamide-2-methylpro panesulfonic acid, N- ethylene 15 parts of base pyrrolidones are dissolved in 120 parts of deionized waters, are added 0.21 part of initiation auxiliary agent lactic acid-chromium base bentonite clay material, and 0.42 Part initiator.
Comparative example 1
Identical with embodiment 1, difference is, is only added without and causes auxiliary agent lactic acid-chromium base bentonite clay material.
Comparative example 2
Identical with embodiment 1, difference is, the initiation auxiliary agent being only added is not lactic acid-chromium base bentonite material The sodium bentonite of material but routine.
Comparative example 3
Identical with embodiment 1, difference is: only preparing and is added without chromic nitrate when causing auxiliary agent.
Comparative example 4
Identical with embodiment 1, difference is: only preparing and 8.05 parts of chromic nitrates, 9.82 parts are added when causing auxiliary agent Zinc nitrate, 8.75 parts of aluminum nitrates and 4.04 parts of ferric nitrates.
Comparative example 5
2- acrylamide-2-methylpro panesulfonic acid is replaced with into p-methyl benzenesulfonic acid, remaining is identical with embodiment 1.
Comparative example 6
With embodiment 6, only it is added without and causes auxiliary agent lactic acid-chromium base bentonite clay material.
Comparative example 7
Identical with 1 process of embodiment, difference is, is added without potassium humate.
Comparative example 8
Identical with 1 process of embodiment, difference is, is added without alkaline reagent, pH 7.
The drilling fluid that the present embodiment prepares is carried out with sulfomethylated humic acid potassium graft polymers fluid loss additive below Performance evaluation, the specific steps are as follows:
1, fluid loss additive filtrate loss controllability evaluation result
Base slurry is prepared: being measured the tap water of about 10L with graduated cylinder, and is heated to 60 DEG C, soil paste swelling is removed in preparation Native 400g is slowly added into hot water, is stirred when adding native, the fully dispersed uniformly rear addition 20gNa of bentonite2CO3Stir 30min After conserve it is spare for 24 hours.
Experiment slurry is prepared and test: blank sample is used as using base slurry, be separately added into base is starched embodiment 1 ~ 9 and comparative example 1 ~ Fluid loss additive sample is added fluid loss additive class sample is base slurry weight 2% as test specimens in 6 in base slurry.
Filter loss test: base is starched and is tested slurry and measures API filtration, high temperature and pressure leak-off after heat rolling 16h at 200 DEG C Amount (high temperature and pressure fluid loss measuring temperature is its heat rolling temperature), test data is shown in Table 1.
Table 1 is filtration reduction evaluation result
As shown in Table 1, base slurry filter loss after 2% embodiment sample heat at 200 DEG C rolls 16h is added in base slurry different journeys Degree ground reduces, and the API filtration of base slurry is generally down to 10.6 ~ 17.8ml from 25.5ml, and high temperature and high pressure filter loss is dropped from 73.0ml To 20.3 ~ 28.4ml.In particular embodiment 1 synthesized fluid loss additive its have excellent performance, API filtration is down to 4.2ml, high temperature High filter pressing loss is down to 10.5ml, it is seen that raw material is produced with the performance for comparing sulfomethylated humic acid potassium graft polymers fluid loss additive Raw tremendous influence, when raw material proportioning reaches optimal combination in embodiment 1, filtrate reducing effect reaches best.In addition comparative example 1 ~ 5 Illustrate that the comparison fluid loss additive performance of matching of the bentonitic addition of the initiation auxiliary agent lactic acid-chromium baseization and formula is affected.
Comparative example 7-8 illustrates that the adjusting of potassium humate and raw material ph influence also very greatly product overall performance.
2, fluid loss additive temperature resistance evaluation result
Sample to be tested is prepared and test: take 400ml clear water, the sample prepared in embodiment 1 be added, 200 DEG C, 220 DEG C, Its rheological parameter is surveyed after heat rolling 16h at 240 DEG C, it is the 2% of clear water weight that fluid loss additive class sample, which is added,.
Table 2 is heat rolling temperature to fluid loss additive aqueous solution rheology impact
As can be seen from Table 2, with the raising of heat rolling temperature, the solution viscosity of fluid loss additive declines with shear force.? At 240 DEG C after heat rolling, the AV and PV of fluid loss additive aqueous solution decline by a big margin, but fluid loss additive is not degradable, water Solution still has certain viscosity, illustrates that the fluid loss additive temperature resistance is excellent, still there is certain temperature resistance at 240 DEG C.
3, fluid loss additive Assessment on Salt
Sample to be tested is prepared and test: taking 400ml drilling well liquid-based to starch, the fluid loss additive sample prepared in 2% embodiment 1 is added After high-speed stirred is thoroughly dispersed in drilling fluid to fluid loss additive, a certain amount of salt, test drilling fluid rheology and filter is added in product Vector, the salt of addition are the mass percent of drilling well liquid-based slurry.Drilling fluid heat rolling 16h at 200 DEG C is recycled after test, is surveyed Rheological characteristic, API filtration and the high temperature and high pressure filter loss of test drilling well liquid.
Table 3 is fluid loss additive salt-resistance (NaCl) evaluation
Table 4 is fluid loss additive salt-resistance (CaCl2) evaluation
By table 3, table 4 it is found that the 20%NaCl drilling well liquid-based slurry API filtration that fluid loss additive in the present invention is added is only 6.8ml, high temperature and high pressure filter loss 36.3ml, and in the 1%CaCl that fluid loss additive in of the invention is added2Drilling well liquid-based starches API filter Vector is only 7.2ml, high temperature and high pressure filter loss 35.6ml, illustrates that fluid loss additive has good salt-resistance in the present invention, is one The preferable salt resistance fluid loss additive of kind.

Claims (8)

1. a kind of drilling fluid preparation method of sulfomethylated humic acid potassium graft polymers fluid loss additive, it is characterised in that this method The following steps are included:
1) 60 ~ 100 parts of deionized waters are added in the reaction kettle equipped with 30 ~ 50 parts of potassium humates, after dissolution is stirred at room temperature, use alkali Property reagent adjust pH to 10 ~ 11, then be added 6 ~ 10 parts by weight of formaldehyde, 6 ~ 10 parts by weight sulfonating agent sodium hydrogensulfites, stirring rise Temperature cools down after reacting 3 ~ 4h to 70 ~ 75 DEG C;
2) by 15 ~ 25 parts of acrylamides, 5 ~ 15 parts of alkyl acrylics, 10 ~ 20 parts of 2- acrylamide-2-methylpro panesulfonic acids, 5 ~ Reaction kettle in step 1) is added after being dissolved in 70 ~ 150 parts of deionized waters in 15 parts of n-vinyl pyrrolidone, stirs 0.5h, simultaneously 0.13 ~ 0.25 part of initiation auxiliary agent lactic acid-chromium base bentonite clay material, heating, by 0.27 ~ 0.5 part of sodium peroxydisulfate and sulfurous is added The initiator that sour hydrogen sodium is made into, is slowly alternately added in reaction kettle, time for adding 0.5h, protects after being added dropwise at 55 ~ 60 DEG C Warm 4h, discharging, cooling obtain sulfomethylated humic acid potassium graft polymers fluid loss additive.
2. the preparation side of a kind of drilling fluid sulfomethylated humic acid potassium graft polymers fluid loss additive according to claim 1 Method, it is characterised in that step 1) neutral and alkali reagent is one of sodium hydroxide, potassium hydroxide or a variety of.
3. the preparation side of a kind of drilling fluid sulfomethylated humic acid potassium graft polymers fluid loss additive according to claim 1 Method, it is characterised in that potassium humate in step 1), formaldehyde, sodium hydrogensulfite, deionized water mass ratio be 5:1:1:2.
4. the preparation side of a kind of drilling fluid sulfomethylated humic acid potassium graft polymers fluid loss additive according to claim 1 Method, it is characterised in that ratio of initiator n sodium peroxydisulfate in step 2: n sodium sulfite=1.3:1.
5. the preparation side of a kind of drilling fluid sulfomethylated humic acid potassium graft polymers fluid loss additive according to claim 1 Method, it is characterised in that mixing speed is 100 ~ 150r/min in step 1), and mixing speed is 300 ~ 400r/min in step 2.
6. the preparation side of a kind of drilling fluid sulfomethylated humic acid potassium graft polymers fluid loss additive according to claim 1 Method, it is characterised in that reaction kettle of the step 1) into step 2 is ceramic electric heating reaction kettle.
7. the preparation side of a kind of drilling fluid sulfomethylated humic acid potassium graft polymers fluid loss additive according to claim 1 Method, it is characterised in that the polymer filtrate reducer weight average molecular weight is 90 ~ 1,400,000.
8. the preparation side of a kind of drilling fluid sulfomethylated humic acid potassium graft polymers fluid loss additive according to claim 1 Method, it is characterised in that the lactic acid-chromium base bentonite clay material the preparation method is as follows:
7.08 parts of chromic nitrates, 18.91 parts of zinc nitrates, 7.35 parts of aluminum nitrates and 5.68 parts of ferric nitrates are dissolved in 100 parts of water by step 1 In obtain mixing salt solution, 5.35 parts of sodium hydroxides and 2.84 parts of sodium carbonate are dissolved in 50 parts, mixed ammonium/alkali solutions are configured to, will Mixed ammonium/alkali solutions are slowly dropped in the mixing salt solution being vigorously stirred, and stop that mixing alkali soluble is added dropwise after salt-mixture precipitates completely Liquid, washing filtering after taking bottom sediment to stir crystallization at 70 DEG C for 24 hours, drying for standby;
Step 2 evaporates excessive hydrochloric acid after sufficiently reacting 36 parts of neodymia with 4 parts of mixed in hydrochloric acid, excessive water is added, adds ammonia Water precipitates completely to rare earth, and filtering is washed to no chloride ion, obtains neodymium hydroxide, neodymium hydroxide is mixed with excessive water, is obtained Suspension is heated to that lactic acid aqueous solution insulation reaction 5h is added after 60 DEG C while stirring, and evaporation excessive water precipitation product, which is crossed, to be filtered dry It is dry to obtain lactic acid neodymium compound, 50 parts of sodium bentonites are added after lactic acid neodymium compound is mixed with product in step 1 and pinch Conjunction obtains lactic acid-chromium base bentonite clay material.
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CN108822812A (en) * 2018-07-25 2018-11-16 佛山陵朝新材料有限公司 A kind of preparation method of salt tolerant high heat stability fluid loss additive
CN111139039B (en) * 2018-11-02 2022-06-10 中国石油化工股份有限公司 Sulfonated phenolic resin graft modified polymer filtrate reducer and preparation method thereof
CN111139042B (en) * 2018-11-02 2022-06-10 中国石油化工股份有限公司 Resin modified polymer fluid loss agent based on degradation and preparation method thereof
CN110564381B (en) * 2019-09-28 2021-07-20 重庆威能钻井助剂有限公司 Composite filtrate reducer for drilling fluid and preparation method thereof
CN110591667B (en) * 2019-09-29 2021-07-20 重庆威能钻井助剂有限公司 High-temperature-resistant fluid loss additive for drilling fluid and preparation method thereof

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