CN115353585A - Preparation method of polyacrylamide potassium salt coating inhibitor for drilling fluid - Google Patents
Preparation method of polyacrylamide potassium salt coating inhibitor for drilling fluid Download PDFInfo
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- CN115353585A CN115353585A CN202211176525.1A CN202211176525A CN115353585A CN 115353585 A CN115353585 A CN 115353585A CN 202211176525 A CN202211176525 A CN 202211176525A CN 115353585 A CN115353585 A CN 115353585A
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- drilling fluid
- polyacrylamide
- potassium salt
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- acrylamide monomer
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- 239000003112 inhibitor Substances 0.000 title claims abstract description 54
- 239000011248 coating agent Substances 0.000 title claims abstract description 46
- 238000000576 coating method Methods 0.000 title claims abstract description 46
- 229920002401 polyacrylamide Polymers 0.000 title claims abstract description 43
- 238000005553 drilling Methods 0.000 title claims abstract description 39
- 239000012530 fluid Substances 0.000 title claims abstract description 39
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- 239000000376 reactant Substances 0.000 claims abstract description 15
- 239000007864 aqueous solution Substances 0.000 claims abstract description 13
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 13
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004202 carbamide Substances 0.000 claims abstract description 11
- 230000007062 hydrolysis Effects 0.000 claims abstract description 11
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000012966 redox initiator Substances 0.000 claims abstract description 7
- 229960001484 edetic acid Drugs 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical group [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 22
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 14
- 235000015497 potassium bicarbonate Nutrition 0.000 claims description 12
- 239000011736 potassium bicarbonate Substances 0.000 claims description 12
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 12
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 12
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 11
- 235000011181 potassium carbonates Nutrition 0.000 claims description 11
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 7
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 7
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 7
- 239000003638 chemical reducing agent Substances 0.000 claims description 7
- 239000007800 oxidant agent Substances 0.000 claims description 7
- 229910052700 potassium Inorganic materials 0.000 claims description 7
- 239000011591 potassium Substances 0.000 claims description 7
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 7
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 4
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical group [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical group [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- 235000010265 sodium sulphite Nutrition 0.000 claims description 2
- 238000006116 polymerization reaction Methods 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 5
- 230000005764 inhibitory process Effects 0.000 abstract description 4
- 230000001276 controlling effect Effects 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- 230000001105 regulatory effect Effects 0.000 abstract description 3
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 abstract 1
- 235000011164 potassium chloride Nutrition 0.000 abstract 1
- 239000001103 potassium chloride Substances 0.000 abstract 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 21
- 239000000243 solution Substances 0.000 description 10
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 8
- 229960003975 potassium Drugs 0.000 description 6
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 5
- 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
- 230000008569 process Effects 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 238000007873 sieving Methods 0.000 description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 description 4
- 239000001569 carbon dioxide Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 238000007334 copolymerization reaction Methods 0.000 description 4
- 210000003298 dental enamel Anatomy 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 230000006872 improvement Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000011435 rock Substances 0.000 description 2
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical class [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 1
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 description 1
- 101100161752 Mus musculus Acot11 gene Proteins 0.000 description 1
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229940086066 potassium hydrogencarbonate Drugs 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/08—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing carbon dioxide
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
- C09K8/035—Organic additives
-
- 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
- C09K8/04—Aqueous well-drilling compositions
- C09K8/14—Clay-containing compositions
- C09K8/18—Clay-containing compositions characterised by the organic compounds
- C09K8/22—Synthetic organic compounds
- C09K8/24—Polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/02—CO2-releasing, e.g. NaHCO3 and citric acid
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/24—Homopolymers or copolymers of amides or imides
- C08J2333/26—Homopolymers or copolymers of acrylamide or methacrylamide
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- Chemical & Material Sciences (AREA)
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Medicinal Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention belongs to the technical field of oil field drilling fluid treating agents, and particularly relates to a preparation method of a polyacrylamide potassium salt coating inhibitor for drilling fluid. The preparation method provided by the invention comprises the following steps: (1) Uniformly stirring and mixing an aqueous solution of an acrylamide monomer, a hydrolytic agent, ethylene diamine tetraacetic acid and urea, adding a redox initiator to the mixture for stirring reaction at a set temperature of 20-40 ℃ under the protection of nitrogen, stopping stirring when the temperature of a reaction system is 2-3 ℃ higher than the set temperature, transferring the obtained reactant, and continuously reacting for 5-7 hours to obtain a spongy product; (2) Crushing, drying and crushing the spongy product to obtain the sponge. The invention adopts a simple hydrolysis polymerization method, can achieve the purposes of comprehensively regulating and controlling the molecular weight, the inhibition effect and the water solubility of the product, and greatly meets the industrial requirements of the polyacrylamide sylvite coating inhibitor for the drilling fluid.
Description
Technical Field
The invention belongs to the technical field of oil field drilling fluid treating agents, and particularly relates to a preparation method of a polyacrylamide potassium salt coating inhibitor for drilling fluid.
Background
Along with the continuous deepening of the development of domestic oil and gas reservoirs, higher requirements are put forward on the quality of the drilling fluid treating agent. The coating inhibitor for the drilling fluid is one of more important treating agents in the using process of the drilling fluid, and has the functions of coating rock debris, inhibiting expansion of shale and clay and stabilizing a well wall.
The polyacrylamide potassium salt coating inhibitor is a mature inhibitor for the drilling fluid at present, and is widely applied to the drilling fluid at present. The existing preparation method of the polyacrylamide potassium salt coating inhibitor generally adopts a method of copolymerization of acrylamide and potassium acrylate, and specifically comprises the steps of dissolving potassium hydroxide into a solution, neutralizing the solution with acrylic acid to generate a potassium acrylate solution, adding solid acrylamide to dissolve uniformly, and adding a redox initiator to perform polymerization reaction to obtain the polyacrylamide potassium salt coating inhibitor. However, the polyacrylamide potassium salt product obtained by the method has low molecular weight and relatively poor coating inhibition capability, and has the problems of easy agglomeration and poor solubility, so that the further application of the polyacrylamide potassium salt product in the drilling fluid is limited.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing a potassium polyacrylamide salt coating inhibitor for drilling fluid, which adopts a simple hydrolysis polymerization method, and can obtain a coating inhibitor with high molecular weight, excellent inhibition capability and excellent water solubility.
In order to achieve the aim, the preparation method of the polyacrylamide potassium salt coating inhibitor for the drilling fluid provided by the invention comprises the following steps:
(1) Uniformly stirring and mixing an aqueous solution of an acrylamide monomer, a hydrolytic agent, ethylene diamine tetraacetic acid and urea, adding a redox initiator to carry out stirring reaction at a set temperature of 20-40 ℃ under the protection of nitrogen, stopping stirring when the temperature of a reaction system is 2-3 ℃ higher than the set temperature, transferring the obtained reactant, and carrying out open standing reaction for 5-7 hours to obtain a spongy product;
(2) Crushing, drying and crushing the spongy product to obtain a polyacrylamide potassium salt coating inhibitor for the drilling fluid;
wherein, in the aqueous solution of the acrylamide monomer, the mass concentration of the acrylamide monomer is 30-40%; the hydrolytic agent is potassium carbonate and potassium bicarbonate with the mass ratio of 1: (2-3); the dosage of the hydrolytic agent is 35 to 40 percent of the mass of the acrylamide monomer.
The preparation method of the polyacrylamide potassium salt coating inhibitor for the drilling fluid comprises the steps of simultaneously preparing the polyacrylamide potassium salt by taking a monomer solution, a hydrolytic agent, disodium ethylene diamine tetraacetate and urea as a composite system, wherein under the combined action of an initiator and the hydrolytic agent, the raw material system can synchronously carry out polymerization and hydrolysis processes, the chain extension polymerization process is easier to control, and the hydrolysis process is more uniform, so that the water solubility of the product is ensured while the product is endowed with higher molecular weight, the purposes of comprehensively regulating and controlling the molecular weight, the inhibition effect and the water solubility of the product are achieved, and the industrial requirement of the polyacrylamide potassium salt coating inhibitor for the drilling fluid is greatly met.
According to the preparation method, potassium carbonate and potassium bicarbonate are used as the composite hydrolytic agent, and generally, the stronger the alkalinity of the hydrolytic agent is, the better the hydrolytic effect is. The invention adopts potassium carbonate and potassium bicarbonate, and the mass ratio is 1: the mixture of (2) to (3) is relatively weak in alkalinity as a hydrolyzing agent, and the hydrolyzing agent can lower the pH of the polymerization system at the initial stage of the reaction, and facilitates the progress of the polymerization reaction. After the polymerization is carried out to a certain degree, potassium bicarbonate can gradually release water and carbon dioxide due to pyrolysis to generate potassium carbonate, so that the pH value of the system is increased, and the hydrolysis reaction is promoted, therefore, the invention can realize the comprehensive regulation and control of the polymerization and hydrolysis degree. In addition, the invention adopts high-content potassium bicarbonate, carbon dioxide can be released in the decomposition process, the carbon dioxide can take away part of heat, the system temperature is reduced, the product is prevented from being cohered, holes can be left after the carbon dioxide is released, the spongy product shape is obtained, and the improvement of the product solubility is promoted.
Furthermore, the invention adds the complexing of the disodium salt of the ethylenediaminetetraacetic acid to remove metal ions in the aqueous solution, and simultaneously plays a role in further improving the molecular weight of the polymer and the water solubility of the product. Preferably, the amount of the disodium ethylene diamine tetraacetate is 0.10-0.20% of the mass of water used in the acrylamide monomer aqueous solution.
In the polymerization system, in order to further improve the mixing uniformity of the composite system, thereby ensuring the balance of polymerization and hydrolysis processes and finally realizing the comprehensive improvement of the molecular weight and water-soluble effect of the product, the invention further increases urea to improve the molecular weight of the polymer and the water-soluble effect of the product. Preferably, the amount of urea is 3.5 to 4.0% by mass of the acrylamide monomer.
After the redox initiator is added, the composite system of the invention simultaneously carries out polymerization and hydrolysis reaction, thereby comprehensively regulating and controlling the molecular weight and the water-soluble effect of the product. Preferably, the redox initiator consists of an oxidizing agent and a reducing agent, wherein the using amount of the oxidizing agent is 0.07-0.15% of the mass of the acrylamide monomer, and the using amount of the reducing agent is 0.07-0.15% of the mass of the acrylamide monomer.
The present invention is not particularly limited in the kind of the specific oxidizing agent and reducing agent, as long as the requirements for aqueous solution copolymerization can be satisfied. Further preferably, the oxidant is potassium persulfate or ammonium persulfate; the reducing agent is sodium sulfite or sodium bisulfite.
After the reaction in the step (1), the spongy product is obtained, and can be pre-crushed and dried by adopting a conventional treatment method, and then crushed and sieved. Preferably, the drying temperature is 70-85 ℃. More preferably, the mesh number used for the sieving is 30 to 50 mesh, and more preferably 40 mesh.
The preparation method of the polyacrylamide potassium salt coating inhibitor for the drilling fluid provided by the invention has the advantages of simple steps and low cost, and is suitable for industrial production. Experimental results show that the polyacrylamide potassium salt coating inhibitor prepared by the preparation method has the intrinsic viscosity of over 10.4, the water solubility of the product is good, the hydrolysis degree is 30.05-32.58%, the dissolution time in water is only 255-260 s at the concentration of 0.5%, the expansion reduction rate of a rock core wire is 81-85%, and the requirement of SY/T5946-2019 on the minimum technical index of the coating inhibitor for the drilling fluid is far exceeded.
Detailed Description
The following examples are provided to illustrate the preparation of the potassium polyacrylamide coating inhibitor for drilling fluid of the present invention, but they should not be construed as limiting the scope of the present invention.
Example 1
The preparation method of the polyacrylamide potassium salt coating inhibitor for the drilling fluid comprises the following specific steps:
(1) 100g of an acrylamide monomer aqueous solution with the mass concentration of 40% (prepared by adding 40g of acrylamide into 60g of deionized water), 4.0g of potassium carbonate, 10.0g of potassium bicarbonate, 1.5g of urea and 0.06g of ethylene diamine tetraacetic acid (EDTA-2 Na) are respectively added into a clean four-mouth bottle, stirring is carried out for 30min to be completely dissolved, then the system is controlled to set the temperature at 30 ℃, nitrogen is introduced to drive oxygen for 30min, and 2.0mL of ammonium persulfate with the mass concentration of 2.5% and 2.0mL of sodium bisulfite with the mass concentration of 2.5% are added under the protection of nitrogen to carry out stirring reaction. Recording the system temperature, stopping stirring when the system temperature is 2-3 ℃ higher than the set temperature, pouring the reactant into an enamel cup, and standing and reacting for 6 hours in an open manner to obtain a spongy reactant;
(2) And crushing the spongy reactant, drying for 10h at 80 ℃, and then crushing and sieving by a 40-mesh sieve to obtain the polyacrylamide potassium salt coated inhibitor product for the drilling fluid in the embodiment 1.
Example 2
The preparation method of the polyacrylamide potassium salt coating inhibitor for the drilling fluid comprises the following specific steps:
(1) 100g of an acrylamide monomer aqueous solution with the mass concentration of 40%, 5.0g of potassium carbonate, 10.0g of potassium bicarbonate, 1.5g of urea and 0.06g of ethylene diamine tetraacetic acid (EDTA-2 Na) are respectively added into a clean four-mouth bottle, stirring is carried out for 30min to be completely dissolved, then the system is controlled to have the set temperature of 30 ℃, nitrogen is introduced to drive oxygen for 30min, and 1.6mL of ammonium persulfate with the mass concentration of 2.5% and 1.6mL of sodium bisulfite with the mass concentration of 2.5% are added under the protection of nitrogen to carry out stirring reaction. Recording the system temperature, stopping stirring when the system temperature is 2-3 ℃ higher than the set temperature, pouring the reactant into an enamel cup, and standing and reacting for 6 hours in an open manner to obtain a spongy reactant;
(2) And crushing the spongy reactant, drying for 10h at 80 ℃, and then crushing and sieving by a 40-mesh sieve to obtain the polyacrylamide potassium salt coated inhibitor product for the drilling fluid in the embodiment 2.
Example 3
The preparation method of the polyacrylamide potassium salt coated inhibitor for the drilling fluid comprises the following specific steps:
(1) 100g of an acrylamide monomer aqueous solution with the mass concentration of 40%, 4.0g of potassium carbonate, 12.0g of potassium bicarbonate, 1.5g of urea and 0.06g of disodium ethylene diamine tetraacetate (EDTA-2 Na) are respectively added into a clean four-mouth bottle, the mixture is stirred for 30min to be completely dissolved, then the system is controlled to have the set temperature of 30 ℃, nitrogen is introduced to drive oxygen for 30min, and 1.3mL of ammonium persulfate with the mass concentration of 2.5% and 1.3mL of sodium bisulfite with the mass concentration of 2.5% are added under the protection of nitrogen to carry out stirring reaction. Recording the system temperature, stopping stirring when the system temperature is higher than the set temperature by 2-3 ℃, pouring the reactant into an enamel cup, and standing and reacting for 6 hours in an open manner to obtain a spongy reactant;
(2) And crushing the spongy reactant, drying for 10h at 80 ℃, and then crushing and sieving by a 40-mesh sieve to obtain the polyacrylamide potassium salt coated inhibitor product for the drilling fluid in the embodiment 3.
Comparative example 1
The preparation method of the polyacrylamide potassium salt coated inhibitor for drilling fluid in the comparative example 1 is a copolymerization method generally adopted in the prior art. The method takes potassium hydroxide, acrylic acid and acrylamide as raw materials and comprises the following specific steps:
(1) In a 500mL beaker, 220mL of deionized water was added, followed by 19.5g of potassium hydroxide, which was dissolved by stirring, and after cooling to room temperature, 22.6g of acrylic acid was added, and the reaction was stirred to complete the reaction to a homogeneous potassium acrylate solution. The reaction equation is CH 2 ＝CH-COOH+KOH＝＝CH 2 ＝CH-COOK+H 2 O；
(2) Adding 75g of acrylamide into the potassium acrylate solution, stirring and dissolving completely, and adjusting the pH value of the system to 8.0 by using a potassium hydroxide aqueous solution;
(3) Pouring the mixed solution of the potassium acrylate and the acrylamide obtained in the step (2) into a clean and dry four-mouth bottle, then placing the bottle into a water bath kettle, installing a stirrer, a thermometer and a nitrogen inlet pipe, stirring to raise the temperature of the system to 30 ℃, introducing nitrogen for 30min, under the protection of stirring and nitrogen, firstly adding 2.5mL of 5% sodium bisulfite solution, then adding 2.5mL of 5% ammonium persulfate solution for reaction, recording the temperature of the system, stopping stirring when the temperature of the system is higher than the set temperature of 2-3 ℃, pouring the reactant into an enamel cup, and continuing the reaction for 6h to obtain a gel-like reactant;
(4) And crushing the gel-like reactant, drying at 80 ℃ for 10h, and then crushing and sieving by a 40-mesh sieve to obtain the polyacrylamide potassium salt coated inhibitor product for the drilling fluid in the comparative example 1.
Comparative example 2
The preparation method of the polyacrylamide potassium salt coated inhibitor for drilling fluid in the comparative example 2 is a copolymerization method. The method takes potassium hydroxide, acrylic acid and acrylamide as raw materials, and the specific steps are basically the same as those of comparative example 1, and only differ from the raw materials in terms of the amount. In this comparative example, the amount of deionized water in step (1) was 180mL, potassium hydroxide was 15.7g, and acrylic acid was 18.4g; in the step (2), 60g of acrylamide is obtained; in the step (3), the dosage of the sodium bisulfite solution and the ammonium persulfate solution is 2.1mL.
Comparative example 3
The potassium polyacrylamide salt coating inhibitor of this comparative example is prepared by the same method as that of the coating inhibitor of example 1, and is prepared by a polymerization hydrolysis method, with the only difference that: the coating inhibitor of this comparative example was prepared without the addition of urea and EDTA-2Na.
Comparative example 4
The potassium polyacrylamide salt coating inhibitor of this comparative example was prepared in substantially the same manner as the coating inhibitor of example 1, except that: the coating inhibitor of this comparative example was prepared without adding potassium bicarbonate while increasing the amount of potassium carbonate to 14.0g.
Comparative example 5
The potassium polyacrylamide salt coating inhibitor of this comparative example was prepared in substantially the same manner as the coating inhibitor of example 1, except that: the coating inhibitor of this comparative example was prepared without adding potassium carbonate while increasing the amount of potassium bicarbonate to 14.0g.
Comparative example 6
The potassium polyacrylamide salt coating inhibitor of this comparative example was prepared in substantially the same manner as the coating inhibitor of example 1, except that: in the preparation of the coating inhibitor of this comparative example, the amounts of potassium carbonate and potassium hydrogencarbonate were adjusted to 7.0g each.
Examples of the experiments
The polyacrylamide potassium salt coating inhibitor prepared in the above examples 1 to 3 and comparative examples 1 to 6 was subjected to performance tests, and the test indexes include moisture content, purity, intrinsic viscosity, degree of hydrolysis, and K + Content, core linear expansion rate and 0.5 percent concentration are stirred for completely dissolving in water. In the above indexes, the time for stirring and dissolving the coating inhibitor with the concentration of 0.5% in water is the time for stirring and dissolving the coating inhibitor with the same mass in water to prepare the liquid with the mass concentration of 0.5%, and the test methods of the other indexes are performed according to the petroleum industry standard 'SY/T5946-2019 coating inhibitor polyacrylamide potassium salt for drilling fluid'. As a result, theAs shown in table 1.
TABLE 1 main Performance test results of Polyacrylamide Potassium salt coating inhibitor
As can be seen from Table 1, compared with the comparative example, under the condition that the water content, the purity, the hydrolysis degree and the potassium ion content of the product are all similar, the intrinsic viscosity of the polyacrylamide potassium salt coated inhibitor product for the drilling fluid prepared by the preparation method is 1-3 units higher than that of the product prepared by the existing method, the linear expansion reduction rate of the core is increased by 4% -28%, the adding amount of 0.5% in distilled water is increased, and the dissolving time is at least shortened by more than 10s under the same stirring condition.
Claims (6)
1. A preparation method of a polyacrylamide potassium salt coating inhibitor for drilling fluid is characterized by comprising the following steps:
(1) Uniformly stirring and mixing an aqueous solution of an acrylamide monomer, a hydrolytic agent, ethylene diamine tetraacetic acid and urea, adding a redox initiator to carry out stirring reaction at a set temperature of 20-40 ℃ under the protection of nitrogen, stopping stirring when the temperature of a reaction system is 2-3 ℃ higher than the set temperature, transferring the obtained reactant, and carrying out open standing reaction for 5-7 hours to obtain a spongy product;
(2) Crushing, drying and crushing the spongy product to obtain the polyacrylamide potassium salt coating inhibitor for the drilling fluid;
wherein in the aqueous solution of the acrylamide monomer, the mass concentration of the acrylamide monomer is 30-40%; the hydrolysis agent is potassium carbonate and potassium bicarbonate with the mass ratio of 1: (2-3); the dosage of the hydrolytic agent is 35 to 40 percent of the mass of the acrylamide monomer.
2. The method for preparing the polyacrylamide potassium salt coating inhibitor for the drilling fluid as claimed in claim 1, wherein the dosage of the disodium ethylene diamine tetraacetate is 0.10-0.20% of the mass of water used in the acrylamide monomer aqueous solution.
3. The method for preparing the polyacrylamide potassium salt coating inhibitor for the drilling fluid as claimed in claim 1, wherein the dosage of the urea is 3.5-4.0% of the mass of the acrylamide monomer.
4. The preparation method of the potassium polyacrylamide coating inhibitor for drilling fluid as claimed in claim 1, wherein the redox initiator consists of an oxidizing agent and a reducing agent, the amount of the oxidizing agent is 0.07-0.15% of the mass of the acrylamide monomer, and the amount of the reducing agent is 0.07-0.15% of the mass of the acrylamide monomer.
5. The preparation method of the polyacrylamide potassium salt coating inhibitor for the drilling fluid as claimed in claim 1, wherein the oxidant is potassium persulfate or ammonium persulfate; the reducing agent is sodium sulfite or sodium bisulfite.
6. The preparation method of the polyacrylamide potassium salt coated inhibitor for drilling fluid as claimed in claim 1, wherein in the step (2), the drying temperature is 70-85 ℃.
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| CN104619750A (en) * | 2012-09-12 | 2015-05-13 | 埃科莱布美国股份有限公司 | Process for preparing water soluble polymers with no insoluble gels and low levels of residual monomers |
| CN111620973A (en) * | 2017-05-19 | 2020-09-04 | 黄叶芳 | Preparation method of instant anionic high-molecular-weight polyacrylamide |
| CN114605576A (en) * | 2022-03-22 | 2022-06-10 | 爱森（中国）絮凝剂有限公司 | Preparation method of polyacrylamide potassium salt for drilling fluid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| GB903368A (en) * | 1959-05-06 | 1962-08-15 | Dow Chemical Co | Process for the production of a water-soluble polymer |
| CN1542027A (en) * | 2003-04-29 | 2004-11-03 | 许振举 | Method for preparing high molecular weight polyacrylamide dried powder |
| CN104619750A (en) * | 2012-09-12 | 2015-05-13 | 埃科莱布美国股份有限公司 | Process for preparing water soluble polymers with no insoluble gels and low levels of residual monomers |
| CN102977243A (en) * | 2012-11-24 | 2013-03-20 | 山东宝莫生物化工股份有限公司 | Method for producing high-hydrolysis polyacrylamide through homopolymerization cohydrolysis |
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