WO2022099460A1 - Method for preparing filtrate reducer cst-kh570-am - Google Patents
Method for preparing filtrate reducer cst-kh570-am Download PDFInfo
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- WO2022099460A1 WO2022099460A1 PCT/CN2020/127816 CN2020127816W WO2022099460A1 WO 2022099460 A1 WO2022099460 A1 WO 2022099460A1 CN 2020127816 W CN2020127816 W CN 2020127816W WO 2022099460 A1 WO2022099460 A1 WO 2022099460A1
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- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title abstract description 10
- 239000000706 filtrate Substances 0.000 title abstract description 8
- 229920002472 Starch Polymers 0.000 claims abstract description 34
- 239000008107 starch Substances 0.000 claims abstract description 34
- 235000019698 starch Nutrition 0.000 claims abstract description 33
- 238000003756 stirring Methods 0.000 claims abstract description 30
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000839 emulsion Substances 0.000 claims abstract description 16
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 14
- 239000000047 product Substances 0.000 claims abstract description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 12
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 235000019253 formic acid Nutrition 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 claims abstract description 6
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims abstract description 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims abstract description 6
- 238000010907 mechanical stirring Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract 2
- 238000002360 preparation method Methods 0.000 claims description 21
- 238000005485 electric heating Methods 0.000 claims description 10
- 240000003183 Manihot esculenta Species 0.000 claims description 5
- 239000012065 filter cake Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 3
- 230000000977 initiatory effect Effects 0.000 claims 1
- 239000008367 deionised water Substances 0.000 abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 abstract description 5
- 238000000944 Soxhlet extraction Methods 0.000 abstract description 3
- 230000001603 reducing effect Effects 0.000 abstract description 3
- 150000003839 salts Chemical class 0.000 abstract description 3
- 241000658379 Manihot esculenta subsp. esculenta Species 0.000 abstract 1
- 238000007664 blowing Methods 0.000 abstract 1
- 238000000227 grinding Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000007873 sieving Methods 0.000 abstract 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000003999 initiator Substances 0.000 description 5
- 239000000178 monomer Substances 0.000 description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 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
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000015784 hyperosmotic salinity response Effects 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229920000881 Modified starch Polymers 0.000 description 1
- 239000004368 Modified starch Substances 0.000 description 1
- UKXNHSTVFQAPCA-UHFFFAOYSA-N [Si].C[Si](N[Si](C)(C)C)(C)C Chemical compound [Si].C[Si](N[Si](C)(C)C)(C)C UKXNHSTVFQAPCA-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 125000003342 alkenyl group Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000006266 etherification reaction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 229920000578 graft copolymer Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 235000019426 modified starch Nutrition 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 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
- 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
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F230/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal
- C08F230/04—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal
- C08F230/08—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal containing silicon
-
- 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
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
-
- 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
Definitions
- the invention relates to a preparation method of a fluid loss reducing agent CSt-KH570-AM.
- Starch is a widely available, inexpensive, renewable and degradable biomass resource. After being modified by etherification, cross-linking, grafting and other methods, starch can be used as a fluid loss control agent for oilfield drilling fluids, and is suitable for brine and saturated brine systems. Grafted copolymerized starch is formed by grafting monomers to starch molecules through covalent bonds under the action of initiators. It has both salt resistance and certain temperature resistance of starch substances. research hotspots.
- Silicone monomers and their polymers have the advantages of low surface tension, low glass transition temperature, good permeability and good temperature resistance.
- Some researchers have studied, in the organic solvent of N,N-dimethylformamide, ⁇ -methacryloyloxypropyltrimethoxysilane (KH570) and other monomers are synthesized by free radical copolymerization. Silicone copolymer fluid loss reducer with good fluid loss and temperature resistance properties.
- the synthesis method has harsh reaction conditions and needs to be carried out in an organic solvent, which is liable to cause environmental pollution.
- the purpose of the present invention is to provide a preparation method of fluid loss reducer CSt-KH570-AM.
- a preparation method of fluid loss reducer CSt-KH570-AM comprising the steps of: adding 15-25 parts of tapioca starch and 60-70 parts of deionized water to a three-necked flask equipped with an electric stirring paddle and an inlet/outlet pipe, Place the three-necked flask in a constant temperature water bath, stir the starch emulsion evenly and heat it to 74-76°C for gelatinization for 40-50min, then adjust the starch emulsion to 44-46°C, add 20-30 parts of AM, and mechanically stir for 25-35min , add formic acid dropwise to adjust the pH of the solution to 4.1-4.3, then add 11-13 parts of KH570, stir evenly, pass nitrogen protection, add 4-6 parts of ammonium persulfate and 7-9 parts of sodium bisulfite as initiators, stir After reaction for 3.5-4.5h, suction filtration, wash the filter cake with absolute ethanol for 5 times to obtain a white product; put the product in an electric heating
- the starch emulsion is uniformly stirred and heated to 75° C. for gelatinization for 45 minutes.
- the starch emulsion is adjusted to 45°C.
- formic acid is added dropwise to adjust the pH of the solution to 4.2.
- the reaction is stirred for 4 hours and then filtered with suction.
- the product is dried in an electric heating blast drying oven at 50° C. for 48 hours to a constant weight.
- Soxhlet extraction is performed with acetone for 10 hours.
- the method is simple, fast and easy to operate, and the prepared fluid loss reducing agent CSt-KH570-AM has excellent fluid loss reducing property, salt tolerance and temperature resistance.
- a preparation method of fluid loss reducer CSt-KH570-AM comprising the steps of: adding 20 parts of tapioca starch and 65 parts of deionized water to a three-necked flask equipped with an electric stirring paddle and an inlet/outlet pipe, placing the three-necked flask in the three-necked flask In a constant temperature water bath, stir the starch emulsion evenly and heat it to 75°C for gelatinization for 45min, then adjust the starch emulsion to 45°C, add 25 parts of AM, stir mechanically for 30min, add dropwise formic acid to adjust the pH of the solution to 4.2, and then add 12 parts KH570, after stirring evenly, pass nitrogen protection, add 5 parts of ammonium persulfate and 8 parts of sodium bisulfite as initiators, stir and react for 4 hours, filter with suction, wash the filter cake with absolute ethanol for 5 times to obtain a white product; Place in an electric heating blast drying oven at 50°C to dry for 48h to
- a preparation method of fluid loss reducer CSt-KH570-AM comprising the steps of: adding 15 parts of tapioca starch and 60 parts of deionized water to a three-necked flask equipped with an electric stirring paddle and an inlet/outlet pipe, placing the three-necked flask in the three-necked flask In a constant temperature water bath, stir the starch emulsion evenly and heat it to 74°C for gelatinization for 40min, then adjust the starch emulsion to 44°C, add 20 parts of AM, stir mechanically for 25min, add dropwise formic acid to adjust the pH of the solution to 4.1, and then add 11 parts KH570, after stirring evenly, pass nitrogen protection, add 4 parts of ammonium persulfate and 7 parts of sodium bisulfite as initiators, stir and react for 3.5h, filter with suction, wash the filter cake with absolute ethanol for 5 times to obtain a white product; The product was dried in an electric heating blast drying oven at 45°C for
- a preparation method of fluid loss reducer CSt-KH570-AM comprising the steps of: adding 25 parts of tapioca starch and 70 parts of deionized water to a three-necked flask equipped with an electric stirring paddle and an inlet/outlet pipe, placing the three-necked flask in the three-necked flask In a constant temperature water bath, stir the starch emulsion evenly and heat it to 76°C for gelatinization for 50min, then adjust the starch emulsion to 46°C, add 30 parts of AM, stir mechanically for 35min, add dropwise formic acid to adjust the pH of the solution to 4.3, and then add 13 parts KH570, after stirring evenly, pass nitrogen protection, add 6 parts of ammonium persulfate and 9 parts of sodium bisulfite as initiators, stir and react for 4.5 hours, filter with suction, wash the filter cake with absolute ethanol 5 times to obtain a white product; The product was dried in an electric heating blast drying oven at 55°C for 49
- the method is simple, fast and easy to operate, and the prepared fluid loss reducing agent CSt-KH570-AM has excellent fluid loss reducing property, salt tolerance and temperature resistance.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Dispersion Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Graft Or Block Polymers (AREA)
Abstract
A method for preparing filtrate reducer CSt-KH570-AM, the method comprising the following steps: adding cassava starch and deionized water to a three-neck flask equipped with an electric stirring paddle and an air inlet/outlet pipe, placing the three-neck flask in a thermostatic water bath, stirring the starch emulsion until uniform, heating same to 74-76ºC and gelatinizing same for 40-50 min, then adjusting the starch emulsion to 44-46ºC, adding AM, performing mechanical stirring, then adding formic acid dropwise to adjust the pH of the solution to 4.1-4.3, followed by the addition of KH570, stirring same until uniform, then introducing nitrogen for protection, adding ammonium persulfate and sodium bisulfite, stirring same for 3.5-4.5 h, followed by suction filtrating, and washing same with absolute ethanol five times to obtain a white product; and drying the product to a constant weight, grinding same, sieving same through a 100-mesh sieve, then performing Soxhlet extraction thereof with acetone, and leaving an insoluble part in an electrothermal blowing drying oven and drying same to a constant weight to obtain the filtrate reducer. The filtrate reducer prepared by the method has an excellent filtrate reducing property, salt resistance and temperature resistance.
Description
本发明涉及一种降滤失剂CSt-KH570-AM的制备方法。The invention relates to a preparation method of a fluid loss reducing agent CSt-KH570-AM.
淀粉是一种来源广泛、价格低廉、可再生及可降解的生物质资源。淀粉经醚化、交联、接枝等方法改性后可用作油田钻井液降滤失剂，适用于盐水及饱和盐水体系。接枝共聚淀粉是单体在引发剂作用下经共价键接枝到淀粉分子上所形成的，既有淀粉类物质的抗盐性，又有一定抗温性，是目前淀粉类降滤失剂的研究热点。国内的研究人员用丙烯酰胺(AM)、丙烯酸(AA)、丙烯腈(AN)等单体与淀粉接枝共聚形成烯基类多元淀粉接枝共聚物降滤失剂，具有一定的降滤失、抗温、抗盐和抗钙污染能力，但总体来看此类接枝淀粉的抗温性能不够理想。为更好地提高淀粉类降滤失剂抗温性，有研究人员利用无机硅对淀粉进行改性合成抗温性能良好的无机硅改性淀粉降滤失剂，也有利用有机硅(六甲基二硅氮烷)对醚化淀粉进一步改性制备出了抗高温的有机硅淀粉降滤失剂，但是这些方法仍存在着合成工艺复杂、生产成本高等问题。Starch is a widely available, inexpensive, renewable and degradable biomass resource. After being modified by etherification, cross-linking, grafting and other methods, starch can be used as a fluid loss control agent for oilfield drilling fluids, and is suitable for brine and saturated brine systems. Grafted copolymerized starch is formed by grafting monomers to starch molecules through covalent bonds under the action of initiators. It has both salt resistance and certain temperature resistance of starch substances. research hotspots. Domestic researchers use acrylamide (AM), acrylic acid (AA), acrylonitrile (AN) and other monomers to graft and copolymerize with starch to form an alkenyl multi-starch graft copolymer filtrate reducer, which has a certain filtration loss control. , temperature resistance, salt resistance and calcium pollution resistance, but in general, the temperature resistance of this kind of grafted starch is not ideal. In order to better improve the temperature resistance of starch filtrate reducers, some researchers used inorganic silicon to modify starch to synthesize inorganic silicon modified starch filtrate reducers with good temperature resistance, and some researchers also used organic silicon (hexamethyl) Disilazane) further modified etherified starch to prepare high temperature resistant organosilicon starch fluid loss reducer, but these methods still have the problems of complex synthesis process and high production cost.
有机硅单体及其聚合物具有低表面张力、低玻璃化温度、良好的渗透率及耐温性能好等优点。有学者研究，在N,N-二甲基甲酰胺这种有机溶剂中，将γ-甲基丙烯酰氧基丙基三甲氧基硅烷(KH570)与其他单体通过自由基共聚反应，合成了具有良好降滤失及抗温性能的有机硅共聚物降滤失剂。但该合成方法反应条件苛刻且需要在有机溶剂中进行，易造成环境污染。Silicone monomers and their polymers have the advantages of low surface tension, low glass transition temperature, good permeability and good temperature resistance. Some scholars have studied, in the organic solvent of N,N-dimethylformamide, γ-methacryloyloxypropyltrimethoxysilane (KH570) and other monomers are synthesized by free radical copolymerization. Silicone copolymer fluid loss reducer with good fluid loss and temperature resistance properties. However, the synthesis method has harsh reaction conditions and needs to be carried out in an organic solvent, which is liable to cause environmental pollution.
发明内容SUMMARY OF THE INVENTION
本发明的目的在于提供一种降滤失剂CSt-KH570-AM的制备方法。The purpose of the present invention is to provide a preparation method of fluid loss reducer CSt-KH570-AM.
本发明通过下面技术方案实现：The present invention is achieved through the following technical solutions:
一种降滤失剂CSt-KH570-AM的制备方法，包括如下步骤：在装有电动搅拌桨、进/出气管的三口烧瓶中加入15-25份木薯淀粉和60-70份去离子水，将三口烧瓶置于恒温水浴锅中，将淀粉乳液搅拌均匀并加热到74-76℃糊化40-50min，然后调节淀粉乳液至44-46℃，加入20-30份AM，机械搅拌25-35min，滴加甲酸调节溶液pH至4.1-4.3，再加入11-13份KH570，搅拌均匀后，通氮气保护，加入4-6份过硫酸铵及7-9份亚硫酸氢钠作引发剂，搅拌反应3.5-4.5h后抽滤，用无水乙醇洗涤滤饼5次，得白色产品；将产品置于45-55℃的电热鼓风干燥箱中干燥47-49h至恒重，研磨，过100目筛，用丙酮索氏提取9-11h，留取不可溶部分置于45-55℃的电热鼓风干燥箱中干燥47-49h至恒重即得；各原料均为重量份。A preparation method of fluid loss reducer CSt-KH570-AM, comprising the steps of: adding 15-25 parts of tapioca starch and 60-70 parts of deionized water to a three-necked flask equipped with an electric stirring paddle and an inlet/outlet pipe, Place the three-necked flask in a constant temperature water bath, stir the starch emulsion evenly and heat it to 74-76°C for gelatinization for 40-50min, then adjust the starch emulsion to 44-46°C, add 20-30 parts of AM, and mechanically stir for 25-35min , add formic acid dropwise to adjust the pH of the solution to 4.1-4.3, then add 11-13 parts of KH570, stir evenly, pass nitrogen protection, add 4-6 parts of ammonium persulfate and 7-9 parts of sodium bisulfite as initiators, stir After reaction for 3.5-4.5h, suction filtration, wash the filter cake with absolute ethanol for 5 times to obtain a white product; put the product in an electric heating blast drying oven at 45-55℃ to dry for 47-49h to constant weight, grind, and pass 100 Mesh sieve, Soxhlet extraction with acetone for 9-11h, and the insoluble part was placed in an electric heating blast drying oven at 45-55°C to dry for 47-49h to constant weight; each raw material was in parts by weight.
优选地，所述的制备方法中，将淀粉乳液搅拌均匀并加热到75℃糊化45min。Preferably, in the preparation method, the starch emulsion is uniformly stirred and heated to 75° C. for gelatinization for 45 minutes.
优选地，所述的制备方法中，调节淀粉乳液至45℃。Preferably, in the preparation method, the starch emulsion is adjusted to 45°C.
优选地，所述的制备方法中，机械搅拌30min。Preferably, in the preparation method, mechanical stirring is performed for 30 min.
优选地，所述的制备方法中，滴加甲酸调节溶液pH至4.2。Preferably, in the preparation method, formic acid is added dropwise to adjust the pH of the solution to 4.2.
优选地，所述的制备方法中，搅拌反应4h后抽滤。Preferably, in the preparation method, the reaction is stirred for 4 hours and then filtered with suction.
优选地，所述的制备方法中，将产品置于50℃的电热鼓风干燥箱中干燥48h至恒重。Preferably, in the preparation method, the product is dried in an electric heating blast drying oven at 50° C. for 48 hours to a constant weight.
优选地，所述的制备方法中，用丙酮索氏提取10h。Preferably, in the preparation method, Soxhlet extraction is performed with acetone for 10 hours.
本发明技术效果：Technical effect of the present invention:
该方法简便、快捷、易操作，制备的降滤失剂CSt-KH570-AM具有优异的降滤失性、耐盐性和抗温性。The method is simple, fast and easy to operate, and the prepared fluid loss reducing agent CSt-KH570-AM has excellent fluid loss reducing property, salt tolerance and temperature resistance.
下面结合实施例具体介绍本发明的实质性内容。The substantive content of the present invention will be specifically described below with reference to the embodiments.
实施例1Example 1
一种降滤失剂CSt-KH570-AM的制备方法，包括如下步骤：在装有电动搅拌桨、进/出气管的三口烧瓶中加入20份木薯淀粉和65份去离子水，将三口烧瓶置于恒温水浴锅中，将淀粉乳液搅拌均匀并加热到75℃糊化45min，然后调节淀粉乳液至45℃，加入25份AM，机械搅拌30min，滴加甲酸调节溶液pH至4.2，再加入12份KH570，搅拌均匀后，通氮气保护，加入5份过硫酸铵及8份亚硫酸氢钠作引发剂，搅拌反应4h后抽滤，用无水乙醇洗涤滤饼5次，得白色产品；将产品置于50℃的电热鼓风干燥箱中干燥48h至恒重，研磨，过100目筛，用丙酮索氏提取10h，留取不可溶部分置于50℃的电热鼓风干燥箱中干燥48h至恒重即得；各原料均为重量份。A preparation method of fluid loss reducer CSt-KH570-AM, comprising the steps of: adding 20 parts of tapioca starch and 65 parts of deionized water to a three-necked flask equipped with an electric stirring paddle and an inlet/outlet pipe, placing the three-necked flask in the three-necked flask In a constant temperature water bath, stir the starch emulsion evenly and heat it to 75°C for gelatinization for 45min, then adjust the starch emulsion to 45°C, add 25 parts of AM, stir mechanically for 30min, add dropwise formic acid to adjust the pH of the solution to 4.2, and then add 12 parts KH570, after stirring evenly, pass nitrogen protection, add 5 parts of ammonium persulfate and 8 parts of sodium bisulfite as initiators, stir and react for 4 hours, filter with suction, wash the filter cake with absolute ethanol for 5 times to obtain a white product; Place in an electric heating blast drying oven at 50°C to dry for 48h to constant weight, grind, pass through a 100-mesh sieve, extract with acetone Soxhlet for 10h, and store the insoluble part in an electric heating blast drying oven at 50°C for 48h to Constant weight is obtained; all raw materials are in parts by weight.
实施例2Example 2
一种降滤失剂CSt-KH570-AM的制备方法，包括如下步骤：在装有电动搅拌桨、进/出气管的三口烧瓶中加入15份木薯淀粉和60份去离子水，将三口烧瓶置于恒温水浴锅中，将淀粉乳液搅拌均匀并加热到74℃糊化40min，然后调节淀粉乳液至44℃，加入20份AM，机械搅拌25min，滴加甲酸调节溶液pH至4.1，再加入11份KH570，搅拌均匀后，通氮气保护，加入4份过硫酸铵及7份亚硫酸氢钠作引发剂，搅拌反应3.5h后抽滤，用无水乙醇洗涤滤饼5次，得白色产品；将产品置于45℃的电热鼓风干燥箱中干燥47h至恒重，研磨，过100目筛，用丙酮索氏提取9h，留取不可溶部分置于45℃的电热鼓风干燥箱中干燥47h至恒重即得；各原料均为重量份。A preparation method of fluid loss reducer CSt-KH570-AM, comprising the steps of: adding 15 parts of tapioca starch and 60 parts of deionized water to a three-necked flask equipped with an electric stirring paddle and an inlet/outlet pipe, placing the three-necked flask in the three-necked flask In a constant temperature water bath, stir the starch emulsion evenly and heat it to 74°C for gelatinization for 40min, then adjust the starch emulsion to 44°C, add 20 parts of AM, stir mechanically for 25min, add dropwise formic acid to adjust the pH of the solution to 4.1, and then add 11 parts KH570, after stirring evenly, pass nitrogen protection, add 4 parts of ammonium persulfate and 7 parts of sodium bisulfite as initiators, stir and react for 3.5h, filter with suction, wash the filter cake with absolute ethanol for 5 times to obtain a white product; The product was dried in an electric heating blast drying oven at 45°C for 47 hours to constant weight, ground, passed through a 100-mesh sieve, and extracted with acetone for 9 hours. to constant weight; all raw materials are in parts by weight.
实施例3Example 3
一种降滤失剂CSt-KH570-AM的制备方法，包括如下步骤：在装有电动搅拌桨、进/出气管的三口烧瓶中加入25份木薯淀粉和70份去离子水，将三口烧瓶置于恒温水浴锅中，将淀粉乳液搅拌均匀并加热到76℃糊化50min，然后调节淀粉乳液至46℃，加入30份AM，机械搅拌35min，滴加甲酸调节溶液pH至4.3，再加入13份KH570，搅拌均匀后，通氮气保护，加入6份过硫酸铵及9份亚硫酸氢钠作引发剂，搅拌反应4.5h后抽滤，用无水乙醇洗涤滤饼5次，得白色产品；将产品置于55℃的电热鼓风干燥箱中干燥49h至恒重，研磨，过100目筛，用丙酮索氏提取11h，留取不可溶部分置于55℃的电热鼓风干燥箱中干燥49h至恒重即得；各原料均为重量份。A preparation method of fluid loss reducer CSt-KH570-AM, comprising the steps of: adding 25 parts of tapioca starch and 70 parts of deionized water to a three-necked flask equipped with an electric stirring paddle and an inlet/outlet pipe, placing the three-necked flask in the three-necked flask In a constant temperature water bath, stir the starch emulsion evenly and heat it to 76°C for gelatinization for 50min, then adjust the starch emulsion to 46°C, add 30 parts of AM, stir mechanically for 35min, add dropwise formic acid to adjust the pH of the solution to 4.3, and then add 13 parts KH570, after stirring evenly, pass nitrogen protection, add 6 parts of ammonium persulfate and 9 parts of sodium bisulfite as initiators, stir and react for 4.5 hours, filter with suction, wash the filter cake with absolute ethanol 5 times to obtain a white product; The product was dried in an electric heating blast drying oven at 55°C for 49 hours to constant weight, ground, passed through a 100-mesh sieve, extracted with acetone Soxhlet for 11 hours, and the insoluble part was kept in an electric heating blast drying oven at 55°C for 49 hours. to a constant weight; all raw materials are in parts by weight.
该方法简便、快捷、易操作，制备的降滤失剂CSt-KH570-AM具有优异的降滤失性、耐盐性和抗温性。The method is simple, fast and easy to operate, and the prepared fluid loss reducing agent CSt-KH570-AM has excellent fluid loss reducing property, salt tolerance and temperature resistance.
Claims (8)
- 一种降滤失剂CSt-KH570-AM的制备方法，其特征在于包括如下步骤：在装有电动搅拌桨、进/出气管的三口烧瓶中加入15-25份木薯淀粉和60-70份去离子水，将三口烧瓶置于恒温水浴锅中，将淀粉乳液搅拌均匀并加热到74-76℃糊化40-50min，然后调节淀粉乳液至44-46℃，加入20-30份AM，机械搅拌25-35min，滴加甲酸调节溶液pH至4.1-4.3，再加入11-13份KH570，搅拌均匀后，通氮气保护，加入4-6份过硫酸铵及7-9份亚硫酸氢钠作引发剂，搅拌反应3.5-4.5h后抽滤，用无水乙醇洗涤滤饼5次，得白色产品；将产品置于45-55℃的电热鼓风干燥箱中干燥47-49h至恒重，研磨，过100目筛，用丙酮索氏提取9-11h，留取不可溶部分置于45-55℃的电热鼓风干燥箱中干燥47-49h至恒重即得；各原料均为重量份。A preparation method of fluid loss reducer CSt-KH570-AM, which is characterized by comprising the steps of: adding 15-25 parts of tapioca starch and 60-70 parts to a three-necked flask equipped with an electric stirring paddle and an inlet/outlet pipe Ionized water, place the three-necked flask in a constant temperature water bath, stir the starch emulsion evenly and heat it to 74-76°C for gelatinization for 40-50min, then adjust the starch emulsion to 44-46°C, add 20-30 parts of AM, mechanically stir 25-35min, add formic acid dropwise to adjust the pH of the solution to 4.1-4.3, then add 11-13 parts of KH570, stir evenly, pass nitrogen protection, add 4-6 parts of ammonium persulfate and 7-9 parts of sodium bisulfite for initiation After stirring and reacting for 3.5-4.5 hours, suction filtration, and washing the filter cake with absolute ethanol for 5 times to obtain a white product; the product was placed in an electric heating blast drying oven at 45-55 °C to dry for 47-49 hours to constant weight, and ground. , passed through a 100-mesh sieve, extracted with acetone Soxhlet for 9-11 hours, and the insoluble part was placed in an electric blast drying oven at 45-55°C to dry for 47-49 hours to constant weight; each raw material was in parts by weight.
- 根据权利要求1所述的制备方法，其特征在于：将淀粉乳液搅拌均匀并加热到75℃糊化45min。The preparation method according to claim 1, wherein the starch emulsion is stirred evenly and heated to 75° C. for gelatinization for 45 minutes.
- 根据权利要求1所述的制备方法，其特征在于：调节淀粉乳液至45℃。The preparation method according to claim 1, wherein the starch emulsion is adjusted to 45°C.
- 根据权利要求1所述的制备方法，其特征在于：机械搅拌30min。The preparation method according to claim 1 is characterized in that: mechanical stirring is 30min.
- 根据权利要求1所述的制备方法，其特征在于：滴加甲酸调节溶液pH至4.2。The preparation method according to claim 1 is characterized in that: formic acid is added dropwise to adjust the pH of the solution to 4.2.
- 根据权利要求1所述的制备方法，其特征在于：搅拌反应4h后抽滤。The preparation method according to claim 1 is characterized in that: suction filtration after stirring reaction for 4h.
- 根据权利要求1所述的制备方法，其特征在于：将产品置于50℃的电热鼓风干燥箱中干燥48h至恒重。The preparation method according to claim 1, wherein the product is dried in an electric heating blast drying oven at 50°C for 48 hours to a constant weight.
- 根据权利要求1所述的制备方法，其特征在于：用丙酮索氏提取10h。The preparation method according to claim 1 is characterized in that: extracting with acetone Soxhlet for 10h.
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| CN115975112A (en) * | 2022-11-29 | 2023-04-18 | 中国石油大学(华东) | High-temperature-resistant organic silicon crosslinked starch fluid loss agent and preparation method and application thereof |
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