CN114605576A - Preparation method of polyacrylamide potassium salt for drilling fluid - Google Patents
Preparation method of polyacrylamide potassium salt for drilling fluid Download PDFInfo
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- CN114605576A CN114605576A CN202210282269.8A CN202210282269A CN114605576A CN 114605576 A CN114605576 A CN 114605576A CN 202210282269 A CN202210282269 A CN 202210282269A CN 114605576 A CN114605576 A CN 114605576A
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- 229920002401 polyacrylamide Polymers 0.000 title claims abstract description 48
- 238000005553 drilling Methods 0.000 title claims abstract description 27
- 239000012530 fluid Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 title description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 35
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 34
- 239000002245 particle Substances 0.000 claims abstract description 25
- 239000000084 colloidal system Substances 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 22
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000003999 initiator Substances 0.000 claims abstract description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 15
- 239000001103 potassium chloride Substances 0.000 claims abstract description 14
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 14
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004202 carbamide Substances 0.000 claims abstract description 13
- 239000002131 composite material Substances 0.000 claims abstract description 13
- 230000007062 hydrolysis Effects 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims abstract description 9
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 7
- 230000032683 aging Effects 0.000 claims abstract description 5
- 238000004090 dissolution Methods 0.000 claims abstract description 5
- 230000000977 initiatory effect Effects 0.000 claims abstract description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 21
- 229910052700 potassium Inorganic materials 0.000 claims description 21
- 239000011591 potassium Substances 0.000 claims description 21
- 239000003638 chemical reducing agent Substances 0.000 claims description 11
- 239000007800 oxidant agent Substances 0.000 claims description 11
- 150000003839 salts Chemical class 0.000 claims description 11
- 239000003112 inhibitor Substances 0.000 claims description 9
- 230000001590 oxidative effect Effects 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 229940010514 ammonium ferrous sulfate Drugs 0.000 claims description 6
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000012986 chain transfer agent Substances 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 3
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical group FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 2
- 239000004280 Sodium formate Substances 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 238000005469 granulation Methods 0.000 claims description 2
- 230000003179 granulation Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 claims description 2
- 235000019254 sodium formate Nutrition 0.000 claims description 2
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims 2
- 238000007254 oxidation reaction Methods 0.000 claims 2
- VEDJYNSRAXFGMJ-UHFFFAOYSA-N azanium;2-methyl-2-oxidooxypropane Chemical compound [NH4+].CC(C)(C)O[O-] VEDJYNSRAXFGMJ-UHFFFAOYSA-N 0.000 claims 1
- 238000012216 screening Methods 0.000 abstract description 2
- 239000002265 redox agent Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 34
- 239000003292 glue Substances 0.000 description 15
- 239000000047 product Substances 0.000 description 13
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 10
- 239000000178 monomer Substances 0.000 description 9
- 238000007334 copolymerization reaction Methods 0.000 description 7
- VAPQAGMSICPBKJ-UHFFFAOYSA-N 2-nitroacridine Chemical compound C1=CC=CC2=CC3=CC([N+](=O)[O-])=CC=C3N=C21 VAPQAGMSICPBKJ-UHFFFAOYSA-N 0.000 description 5
- UFQDKRWQSFLPQY-UHFFFAOYSA-N 4,5-dihydro-1h-imidazol-3-ium;chloride Chemical compound Cl.C1CN=CN1 UFQDKRWQSFLPQY-UHFFFAOYSA-N 0.000 description 5
- -1 amidine hydrochloride Chemical class 0.000 description 5
- 238000010009 beating Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- IMBKASBLAKCLEM-UHFFFAOYSA-L ferrous ammonium sulfate (anhydrous) Chemical compound [NH4+].[NH4+].[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O IMBKASBLAKCLEM-UHFFFAOYSA-L 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 230000003301 hydrolyzing effect Effects 0.000 description 4
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 230000033116 oxidation-reduction process Effects 0.000 description 2
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 229910001414 potassium ion Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920005614 potassium polyacrylate Polymers 0.000 description 1
- UIIIBRHUICCMAI-UHFFFAOYSA-N prop-2-ene-1-sulfonic acid Chemical compound OS(=O)(=O)CC=C UIIIBRHUICCMAI-UHFFFAOYSA-N 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- NLVXSWCKKBEXTG-UHFFFAOYSA-N vinylsulfonic acid Chemical compound OS(=O)(=O)C=C NLVXSWCKKBEXTG-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C08F120/00—Homopolymers 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
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/52—Amides or imides
- C08F120/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F120/56—Acrylamide; Methacrylamide
-
- 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
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
-
- 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
- C08F8/00—Chemical modification by after-treatment
- C08F8/42—Introducing metal atoms or metal-containing groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/21—Urea; Derivatives thereof, e.g. biuret
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention relates to a preparation method of polyacrylamide sylvite for drilling fluid, which comprises the following steps: adding an acrylamide solution and a urea solution into deionized water for uniform dissolution; conveying the solution to a reaction kettle with a nitrogen protection device; respectively adding a redox agent and a composite initiator into the reaction kettle for polymerization initiation; after the reaction temperature reaches the highest temperature, aging at high temperature to obtain a rubber block; and crushing the rubber block to obtain colloid particles, dripping a potassium hydroxide solution into the colloid particles, conveying the colloid particles to a hydrolyzer for hydrolysis, granulating and drying the hydrolyzed colloid particles, and grinding and screening the colloid particles into a powdery or granular product, namely polyacrylamide sylvite. The method can increase the dissolving speed, shorten the dissolving time and improve the field use efficiency.
Description
Technical Field
The invention belongs to the field of petroleum development, and particularly relates to a preparation method of polyacrylamide potassium salt for drilling fluid.
Background
In the process of oil and gas drilling, in the process of using water-based drilling fluid, the wall of a shale stratum is easy to absorb water and expand, so that the wall of a well is unstable, the well collapses, and meanwhile, cuttings are also easy to absorb water and expand, so that complex downhole problems such as drilling resistance, drill jamming, torque increase, pump holding and the like are caused, even a drill drop or a whole well is scrapped. The shale inhibitors commonly used in the market at present comprise inorganic ionic inhibitors such as potassium chloride, polyammonium inhibitors, polyether amine inhibitors, natural product modified inhibitors, copolymer inhibitors and the like.
The potassium polyacrylamide can ensure that the product has better capability of inhibiting hydration and dispersion of clay and cuttings, control stratum slurrying and keep good anti-collapse effect, the high viscosity of the potassium polyacrylamide can effectively generate the effects of coating and suspending drilling cuttings, and simultaneously the potassium ions can exchange ions with other ions in the stratum to form a layer of film on the hole wall to prevent water in the drilling fluid from entering the stratum to achieve the effect of inhibiting hydration expansion, thereby reducing the accidents in the hole such as hole shrinkage and drilling, and the like and playing a role of stabilizing the hole wall.
The potassium polyacrylamide in the current market is mostly prepared by a copolymerization method, wherein the copolymerization method comprises the steps of neutralizing a potassium hydroxide solution and an acrylic acid solution to be neutral, producing a potassium acrylate solution, then uniformly mixing the potassium acrylate solution and the acrylamide solution, adding a catalyst to generate a colloid, drying, grinding and screening into granular products. According to the process, a large amount of heat is generated in the neutralization process of potassium hydroxide and acrylic acid, so that the temperature in the batching tank is increased, cooling equipment is required to be started to reduce the temperature in the production process, the energy consumption is high, and meanwhile, the reactivity ratios of a potassium acrylate monomer and an acrylamide monomer generated by neutralization in the free radical polymerization process are different, so that the acrylamide reaction rate is high, the potassium acrylate reaction rate is low, the crosslinking is easy, and the reaction is terminated. Resulting in uneven charge of polymer high molecular chain produced by copolymerization and low and long molecular chain linearity. The concrete characteristics are that the molecular weight is not high and is not more than 1800 ten thousand, the water solubility is poor, the solution viscosity is low, and the application dosage is large.
The literature reports (Cheng Bo, Liu Peng City, Wang Bright, synthesis of high molecular weight salt-resistant polyacrylamide potassium salt, Anhui chemical industry, volume 46, 6) that a high molecular weight polyacrylamide potassium salt product is prepared by using Acrylamide (AM), 2-acrylamide-2-methylpropanesulfonic Acid (AMPS) and potassium acrylate as raw materials and adopting a low-temperature composite initiator. The molecular weight of the polyacrylamide sylvite prepared by the method can only reach 1800 ten thousand at most, the water solubility is poor, and the viscosity is not high under high shear rate.
In chinese patent (CN 111978464 a, potassium polyacrylamide, its preparation method and application), acrylamide monomers, sulfonic acid monomers and acrylonitrile monomers are added with potassium hydroxide as an auxiliary agent, persulfate as an initiator and a surfactant to react under the protection of nitrogen gas to obtain a semi-finished product of potassium polyacrylamide, which is then crushed, dried and sieved to obtain a finished product. The patent also adopts a copolymerization method, potassium hydroxide is taken as an auxiliary agent in advance, added into a monomer, reacts with a sulfonic acid monomer to generate potassium sulfonate, and then undergoes free radical copolymerization with acrylamide under the initiation of an initiator persulfate to generate polyacrylamide potassium salt, and the sulfonic acid monomer listed in the patent is: one of 2-acrylamide-2-methyl butane sulfonic acid, allyl sulfonic acid and vinyl sulfonic acid, the monomer has a larger molecular structure, is difficult to polymerize, has a lower reaction rate compared with acrylamide, is easy to terminate the reaction by self-polymerization, and the obtained product also has the defect of a copolymerization method.
The inhibition effect of the polyacrylamide potassium salt in the drilling fluid is mainly realized by the high viscosity of the polymer solution and the proper potassium content, the viscosity of the polymer solution is related to the molecular weight of the polymer, the higher the molecular weight is, the higher the solution viscosity is, the potassium content can be adjusted by the hydrolysis degree, the higher or lower the hydrolysis degree is, the molecular weight of the polymer is reduced, and the optimal use effect of the polyacrylamide potassium salt must be realized by searching the proper range of the hydrolysis degree.
Disclosure of Invention
The invention provides a preparation method of polyacrylamide sylvite for drilling fluid, which can increase the dissolution speed, shorten the dissolution time and improve the field use efficiency.
The invention adopts the technical scheme that the preparation method of the polyacrylamide sylvite for the drilling fluid is characterized by comprising the following steps of:
1) adding an acrylamide solution and a urea solution into deionized water for uniform dissolution, adjusting the pH value of the solution to 6.0-7.0 by using a pH regulator, and cooling to 0-5 ℃;
2) conveying the solution with the adjusted pH value to a reaction kettle with a nitrogen protection device, and introducing nitrogen for 30-40 minutes;
3) respectively adding an oxidation-reduction agent and a composite initiator into a reaction kettle for polymerization initiation, adjusting the dosage of the oxidation-reduction agent and the composite initiator, and controlling the polymerization reaction time to be 1-5 h;
4) after the reaction temperature reaches the highest temperature, aging for 30-60 minutes at the high temperature to obtain a rubber block;
5) taking out the gel block, weighing, crushing by a granulator to obtain colloid particles with the particle size of less than 5.0mm, then dropwise adding a potassium hydroxide solution into the colloid particles, uniformly stirring, conveying the colloid particles to a hydrolyzer for hydrolysis, adjusting the temperature of the hydrolyzer and the time of materials in the hydrolyzer to ensure full hydrolysis, feeding the hydrolyzed colloid particles into a second granulator for granulation, drying by drying equipment, grinding and sieving into powdery or granular product polyacrylamide sylvite with the molecular weight: more than or equal to 2500 ten thousand, the hydrolysis degree is 30-38%, and the potassium content is more than or equal to 12%.
Further, the solution before pH value adjustment is composed of the following raw materials in parts by weight: deionized water: 74-77 parts; the concentration of the acrylamide solution is 50%, and the dosage is as follows: 23-26 parts; the concentration of the urea solution is 25%, and the dosage is as follows: 0.1 to 0.3 portion.
Further, the oxidant and the reducing agent are tert-butyl hydroperoxide-ferrous ammonium sulfate, and the dosage of the oxidant is as follows: 0.002-0.004 portion, the dosage ratio of the reducing agent to the oxidizing agent is: 2:1.
Further, the composite initiator is one or more of azobisisobutyramidine hydrochloride, azobisisobutyronitrile and azobisisoheptonitrile, and the dosage of the initiator is as follows: 0.002-0.06 portion.
Further, the chain transfer agent is sodium hypophosphite or sodium formate, and the adding amount of the chain transfer agent is as follows: 0 to 0.02 portion.
Further, the pH regulator is one of acetic acid, phosphoric acid, sulfuric acid and hydrochloric acid.
Further, the concentration of the potassium hydroxide solution added dropwise was: 48-50%, the addition amount is: 10-16% of the weight of the colloid.
Further, the temperature of the hydrolyzer is 70-90 ℃, and the hydrolysis time is as follows: 1-4 h.
A potassium polyacrylamide salt for drilling fluid is used as coating inhibitor.
The invention adopts post-hydrolysis method to produce polyacrylamide sylvite, acrylamide monomer is homopolymerized to generate polyacrylamide colloid, then liquid potassium hydroxide solution is added at higher temperature, partial post-hydrolysis amide groups are carboxylic acid groups, potassium ions are carried on high molecular chains, the monomer only contains acrylamide, and the reaction rate is consistent, so that the longer molecular chains can be formed in the homopolymerization process by controlling the amount of catalyst, the molecular weight can reach 2500 ten thousands, the post-hydrolysis degree can be more accurately controlled by adding the potassium hydroxide solution into the colloid in a dropwise manner, the charge distribution on the colloid after post-hydrolysis is more uniform, meanwhile, the post-hydrolysis speed can be accelerated by utilizing the high temperature of the polyacrylamide colloid after homopolymerization, and the energy consumption is saved. The potassium polyacrylamide obtained by the method has better linear viscosity and high shear rate viscosity. The urea solution is added into the acrylamide monomer solution, so that the urea does not participate in polymerization reaction, but the urea solution is extremely easy to dissolve in water due to small molecules, and can be uniformly distributed among polyacrylamide macromolecules, so that when the final finished product, namely the granular or powdery polyacrylamide potassium salt product, is dissolved, the dissolving speed can be increased, the dissolving time can be shortened, and the field use efficiency can be improved. The release of ammonia gas in the post-hydrolysis process can be effectively reduced by controlling the pH value of the homopolymerization solution within the range of 6.0-7.0.
Detailed Description
The following examples are further illustrated.
Example 1:
a preparation method of polyacrylamide potassium salt for drilling fluid comprises the following steps:
1) adding 23 parts of 50% acrylamide solution and 0.1 part of 25% urea solution into 77 parts of deionized water, uniformly dissolving, adjusting the pH value to 6.0 by using acetic acid, and cooling to 5 ℃;
2) conveying the adjusted solution into a glass reaction kettle, and introducing nitrogen for 30 minutes; adding 0.002 part of azodiisobutyl imidazoline hydrochloride as a composite initiator and 0.02 part of azodiisobutyl amidine hydrochloride into a reactor, and adding 0.002 part of tert-butyl hydroperoxide as an oxidant and 0.004 part of ammonium ferrous sulfate as a reducing agent; continuing introducing nitrogen for 5 minutes, stopping introducing nitrogen until the temperature is not increased any more, reacting for 4 hours, and aging for 30 minutes at the temperature to obtain a transparent elastic rubber block;
3) taking out the glue blocks, weighing, beating the glue into particles with the particle diameter of less than 5mm by using a granulator, then adding 48% of potassium hydroxide solution with the mass of 10% of the glue, uniformly stirring, then putting into a hydrolyzer, setting the temperature of the hydrolyzer to be 70 ℃, hydrolyzing for 4h, crushing the hydrolyzed glue by using the granulator again, drying, wherein the drying temperature is not more than 100 ℃, drying until the moisture content is less than 10%, grinding, and sieving by using a sieve with the diameter of 0.9mm to obtain the polyacrylamide sylvite product.
Example 2:
a preparation method of polyacrylamide potassium salt for drilling fluid comprises the following steps:
1) adding 25 parts of 50% acrylamide solution and 0.2 part of 25% urea solution into 75 parts of deionized water, uniformly dissolving, adjusting the pH value to 6.5 by using acetic acid, and cooling to 2 ℃;
2) conveying the adjusted solution into a glass reaction kettle, and introducing nitrogen for 30 minutes; adding 0.002 part of azodiisobutyl imidazoline hydrochloride as a composite initiator and 0.02 part of azodiisobutyl amidine hydrochloride into a reactor, and adding 0.002 part of tert-butyl hydroperoxide as an oxidant and 0.004 part of ammonium ferrous sulfate as a reducing agent; continuing introducing nitrogen for 5 minutes, stopping introducing nitrogen until the temperature is not increased any more, and reacting for 3 hours; aging at the temperature for 50 minutes to obtain a transparent elastic rubber block;
3) taking out the rubber block, weighing, beating the rubber block into particles with the particle diameter of less than 5mm by using a granulator, adding 48% of potassium hydroxide solution with the mass of 13% of the rubber, uniformly stirring, and putting into a hydrolyzer, wherein the temperature of the hydrolyzer is set to be 80 ℃, and the hydrolysis time is set to be 2 hours; crushing the hydrolyzed colloid again by a granulator, drying until the drying temperature is not more than 100 ℃, drying until the moisture content is less than 10%, grinding, sieving by a sieve with the diameter of 0.9mm, and obtaining the polyacrylamide sylvite product.
Example 3:
a preparation method of polyacrylamide potassium salt for drilling fluid comprises the following steps:
1) adding 26 parts of 50% acrylamide solution and 0.3 part of 25% urea solution into 74 parts of deionized water, uniformly dissolving, adjusting the pH value to 7.0 by using acetic acid, and cooling to 0 ℃;
2) the solution was transferred to a glass reaction vessel and nitrogen was purged for 30 minutes. 0.002 part of azodiisobutyl imidazoline hydrochloride as a composite initiator and 0.02 part of azodiisobutyl amidine hydrochloride are added into a reactor, and 0.002 part of tert-butyl hydroperoxide as an oxidant and 0.004 part of ammonium ferrous sulfate as a reducing agent are added into the reactor. After nitrogen introduction is continued for 5 minutes, the reaction is stopped until the temperature is not increased any more, the reaction time is 3 hours, and the mixture is aged for 50 minutes at the temperature. Obtaining the transparent elastic rubber block.
3) Taking out the glue blocks, weighing, beating the glue into particles with the particle diameter of less than 5mm by using a granulator, then adding 48% of potassium hydroxide solution with the mass of 16% of the glue, uniformly stirring, then putting into a hydrolyzer, setting the temperature of the hydrolyzer to be 90 ℃, hydrolyzing for 1h, crushing the hydrolyzed glue by using the granulator again, drying, wherein the drying temperature is not more than 100 ℃, drying until the moisture content is less than 10%, grinding, and sieving by using a sieve with the diameter of 0.9mm to obtain the polyacrylamide sylvite product.
Comparative example 1:
1) adding 26 parts of 50% acrylamide solution and 0.3 part of 25% urea solution into 74 parts of deionized water, uniformly dissolving, adjusting the pH value to 7.0 by using acetic acid, and cooling to 0 ℃;
2) the solution was transferred to a glass reaction vessel and nitrogen was purged for 30 minutes. 0.002 part of azodiisobutyl imidazoline hydrochloride as a composite initiator and 0.02 part of azodiisobutyl amidine hydrochloride are added into a reactor, and 0.002 part of tert-butyl hydroperoxide as an oxidant and 0.004 part of ammonium ferrous sulfate as a reducing agent are added into the reactor. After nitrogen introduction is continued for 5 minutes, the reaction is stopped until the temperature is not increased any more, the reaction time is 3 hours, and the mixture is aged for 50 minutes at the temperature. Obtaining transparent elastic rubber blocks;
3) taking out the glue blocks, weighing, beating the glue into particles with the particle diameter of less than 5mm by using a granulator, then adding 48% of potassium hydroxide solution with the mass of 20% of the glue, uniformly stirring, then putting the mixture into a hydrolyzer, hydrolyzing for 2 hours at normal temperature, crushing the hydrolyzed glue by using the granulator again, drying the crushed glue until the drying temperature is not more than 100 ℃, grinding the crushed glue until the moisture content is less than 10%, and sieving the ground glue by using a sieve with the diameter of 0.9mm to obtain the polyacrylamide sylvite product.
Comparative example 2:
1) adding 26 parts of 50% acrylamide solution and 0.3 part of 25% urea solution into 74 parts of deionized water, uniformly dissolving, adjusting the pH value to 7.0 by using acetic acid, and cooling to 0 ℃;
2) the solution was transferred to a glass reaction vessel and nitrogen was purged for 30 minutes. 0.002 part of azodiisobutyl imidazoline hydrochloride as a composite initiator and 0.02 part of azodiisobutyl amidine hydrochloride are added into a reactor, and 0.002 part of tert-butyl hydroperoxide as an oxidant and 0.004 part of ammonium ferrous sulfate as a reducing agent are added into the reactor. And stopping introducing nitrogen for 5 minutes, and reacting for 3 hours when the temperature is not increased any more. Aged at this temperature for 50 minutes. Obtaining transparent elastic rubber blocks;
3) taking out the rubber block, weighing, beating the rubber block into particles with the particle diameter less than 5mm by using a granulator, then adding 48% of potassium hydroxide solution with the mass of 20% of the rubber, uniformly stirring, putting into a hydrolyzer, and hydrolyzing for 2h at 100 ℃. Crushing the hydrolyzed colloid again by a granulator, drying until the drying temperature is not more than 100 ℃, drying until the moisture content is less than 10%, grinding, sieving by a sieve with the diameter of 0.9mm, and sieving to obtain the polyacrylamide potassium salt product.
Comparative examples 3, 4:
the commercially available polyacrylamide potassium salt A (medium petroleum) and B (Anhui Tianrun) were used for comparison.
And (3) performance testing:
the potassium polyacrylamide salts obtained in examples 1 to 3 were prepared according to the oil industry standards: SY/T5946-2019 polyacrylamide potassium salt used as coating inhibitor for drilling fluid and enterprise standard Q/321283GJQ35-2021, and the test results are shown in table 1:
from the above analysis results, it can be known that the molecular weight of the polyacrylamide potassium salt prepared by the present invention can reach more than 2500 ten thousand, the examples 1-3 effectively control the concentration and temperature of potassium hydroxide added into the colloid, compared with the comparative example 1 without the concentration of potassium hydroxide and the post-hydrolysis temperature control, the molecular weight is only 1/2 of the examples 1-3, the viscosity is only 1/3 of the examples 1-3, compared with the comparative example 2 with the concentration of potassium hydroxide added and the post-hydrolysis temperature control being nearly beyond the examples 1-3, but the difference in molecular weight still reaches 1/3, and the viscosity only reaches 1/2, so that it can be clearly found that the concentration and temperature of potassium hydroxide added into the colloid of the examples 1-3 can be effectively controlled, the molecular weight and viscosity can be better improved, particularly preferred is example 2, which provides a higher viscosity of aqueous solution at the same level. Meanwhile, the expansion reduction rate of the rock core line can also show that the potassium polyacrylate prepared by the post-hydrolysis method has higher molecular linearity, better linearity and high shear rate viscosity than those prepared by the copolymerization method.
The above examples are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereto. Any insubstantial changes and substitutions made by those skilled in the art based on the present invention are intended to be covered by the claims.
Claims (9)
1. A preparation method of polyacrylamide sylvite for drilling fluid is characterized by comprising the following steps: the method comprises the following steps:
adding an acrylamide solution and a urea solution into deionized water for uniform dissolution, adjusting the pH value of the solution to 6.0-7.0 by using a pH regulator, and cooling to 0-5 ℃;
conveying the solution with the adjusted pH value to a reaction kettle with a nitrogen protection device, and introducing nitrogen for 30-40 minutes;
respectively adding an oxidation reducing agent and a composite initiator into a reaction kettle for polymerization initiation, adjusting the dosage of the oxidation reducing agent and the composite initiator, and controlling the polymerization reaction time to be 1-5 h;
after the reaction temperature reaches the highest temperature, aging for 30-60 minutes at the high temperature to obtain a rubber block;
taking out the gel block, weighing, crushing by a granulator to obtain colloid particles with the particle size of less than 5.0mm, then dropwise adding a potassium hydroxide solution into the colloid particles, uniformly stirring, conveying the colloid particles to a hydrolyzer for hydrolysis, adjusting the temperature of the hydrolyzer and the time of materials in the hydrolyzer to ensure full hydrolysis, feeding the hydrolyzed colloid particles into a second granulator for granulation, drying by drying equipment, grinding and sieving into powdery or granular product polyacrylamide sylvite with the molecular weight: more than or equal to 2500 ten thousand, the hydrolysis degree is 30-38%, and the potassium content is more than or equal to 12%.
2. The preparation method of the potassium polyacrylamide salt for the drilling fluid, which is disclosed by claim 1, is characterized by comprising the following steps of: the solution before pH value adjustment is composed of the following raw materials in parts by weight: deionized water: 74-77 parts; the concentration of the acrylamide solution is 50%, and the dosage is as follows: 23-26 parts; the concentration of the urea solution is 25%, and the dosage is as follows: 0.1 to 0.3 portion.
3. The preparation method of the potassium polyacrylamide salt for the drilling fluid, which is disclosed by claim 1, is characterized by comprising the following steps of: the oxidant and the reducer are tert-butyl hydroperoxide-ammonium ferrous sulfate, and the dosage of the oxidant is as follows: 0.002-0.004 portion, the dosage ratio of the reducing agent to the oxidizing agent is: 2:1.
4. The preparation method of the potassium polyacrylamide salt for the drilling fluid, which is disclosed by claim 1, is characterized by comprising the following steps of: the composite initiator is one or more of azobisisobutyramidine hydrochloride, azobisisobutyronitrile and azobisisoheptonitrile, and the dosage of the initiator is as follows: 0.002-0.06 portion.
5. The preparation method of the potassium polyacrylamide salt for the drilling fluid, which is disclosed by claim 1, is characterized by comprising the following steps of: the chain transfer agent is sodium hypophosphite or sodium formate, and the adding amount of the chain transfer agent is as follows: 0 to 0.02 portion.
6. The preparation method of the potassium polyacrylamide salt for the drilling fluid, which is disclosed by claim 1, is characterized by comprising the following steps of: the pH regulator is one of acetic acid, phosphoric acid, sulfuric acid and hydrochloric acid.
7. The preparation method of the potassium polyacrylamide salt for the drilling fluid, which is disclosed by claim 1, is characterized by comprising the following steps of: the concentration of the dropwise added potassium hydroxide solution is as follows: 48-50%, the addition amount is: 10-16% of the weight of the colloid.
8. The preparation method of the potassium polyacrylamide salt for the drilling fluid, which is disclosed by claim 1, is characterized by comprising the following steps of: the temperature of the hydrolyzer is 70-90 ℃, and the hydrolysis time is as follows: 1-4 h.
9. A potassium polyacrylamide salt for drilling fluid is used as coating inhibitor.
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| CN115353585A (en) * | 2022-09-26 | 2022-11-18 | 河南金马石油科技有限责任公司 | Preparation method of polyacrylamide potassium salt coating inhibitor for drilling fluid |
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| CN115353585A (en) * | 2022-09-26 | 2022-11-18 | 河南金马石油科技有限责任公司 | Preparation method of polyacrylamide potassium salt coating inhibitor for drilling fluid |
| CN115353585B (en) * | 2022-09-26 | 2023-10-27 | 河南金马石油科技有限责任公司 | Preparation method of polyacrylamide potassium salt coating inhibitor for drilling fluid |
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