CN102303872B - Preparation method of high-property organic bentonite - Google Patents
Preparation method of high-property organic bentonite Download PDFInfo
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Abstract
The invention belongs to the technical field of petrochemical industry and relates to a preparation method of high-property organic bentonite for an oil-based drilling liquid. The preparation method comprises the following steps: dissolving 50-70 parts of sodium-based bentonite dry material in 600-900 parts of deionized water so as to form a suspension system a; mixing and dissolving 15-30 parts of quaternary ammonium salt organic modifier in 100-300 parts of solvent so as to form a homogenous system b; dissolving 10-15 parts of intercalation agent in 100-150 parts of solvent so as to form a homogenous system c; adding a solution b in the suspension system a, and reacting for 1-2 hours at the temperature of 70-90 DGE C so as to form a homogenous system d; adding a solution c in the suspension system d, and reacting for 1-2 hours at the temperature of 70-90 DGE C; and cooling a product to room temperature, washing off redundant ions in the product, filtering, and finally, drying a solid product in the vacuum environment at the temperature of 60-80 DEG C, smashing and screening so as to obtain the product high-property organic bentonite. By using the method provided by the invention, the property of the organic bentonite can be greatly improved, and the high-quality organic bentonite is prepared, thereby being beneficial to improvement of rheological behavior and debris carrying capability of a drilling liquid.
Description
Technical field
The invention belongs to the petrochemical technology field, relate to drilling fluid organophilic clay technical field, be specifically related to a kind of high-performance method for preparing organobentonite.
Background technology
Wilkinite is as main moisture clay pit, molecular formula: Na take montmorillonite
x(H
2O)
4(Al
2-XMg
0.83) Si
4O
10) (OH)
2, because it has special character, as: swelling, cohesiveness, adsorptivity, catalytic, thixotropy, suspension and cationic exchange etc. are applied to various fields.China's bentonite ore resource is very abundant, content is only second to the U.S., occupy the second place of the world, but to its deep processing and utilization far away from abroad, be in the Application and Development stage at initial stage always, just carried out in recent years the research work of wilkinite deep processing and utilization, organobentonite is exactly one of fine product of wilkinite deep processing.Organobentonite has good dispersiveness, adds dissolubility and emulsifying property because it has the characteristic of hydrophobic oleophylic in organic solvent. and be widely used in the industrial circles such as petroleum drilling, paint, printing ink, high temperature grease, makeup, casting, agricultural chemicals as anti-sedimentation agent, viscosifying agent, tackifier and suspension agent etc.
Organobentonite is the most basic oleophylic colloid in the oil base drilling fluid, both can improve viscosity and the shear force of mud in oil base drilling fluid, can reduce again the filter loss of oil base drilling fluid, so organophilic clay is indispensable additive in the oil base drilling fluid.Organophilic clay mainly works to increase glutinous carrying in drilling fluid cuts, and the quality of its performance will directly affect rheological and the large rock-carrying ability of drilling fluid.Drilling fluid in the market is with the gelation of organophilic clay in white oil or diesel oil and increase and glutinous carry that to cut effect generally relatively poor, and therefore the preparation with organophilic clay is studied to oil base drilling fluid.
Summary of the invention
The objective of the invention is to propose a kind of employing organic modifiers and intercalator and prepare high-performance bentonite method.
The inventive method can improve bentonite interlamellar spacing and rheological property significantly, makes superior in quality organobentonite, is conducive to improve rheological and the large rock-carrying ability of oil base drilling fluid.
Main technical schemes of the present invention is: the preparation method is as follows:
(1) 50～70 parts sodium bentonite siccative is dissolved in 600～900 parts the deionized water, high-speed stirring forms suspension system a;
(2) 15～30 parts of quaternary amine organic modifiers is miscible in 100～300 parts of solvents, stirring and dissolving forms homogeneous system b;
(3) 10～15 parts of intercalators are dissolved in 100～150 parts of solvents, stirring and dissolving forms homogeneous system c;
(4) under whipped state, solution b is joined rapidly among the suspension system a, 70～90 ℃ of reactions 1-2 hour, form homogeneous system d;
(5) under whipped state, solution c is added rapidly among the suspension system d, 70～90 ℃ of reactions 1-2 hour;
The product that obtains in the step (5) is cooled to room temperature, and unnecessary ion in the flush away product filters, and is then that the solid product of gained is dry under 60～80 ℃ of vacuum environments, pulverizes 200 mesh sieves, namely obtains the organobentonite product.
Usually, described quaternary amine organic modifiers is the quaternary amine between carbon chain lengths C12～C18, a kind of such as tetradecyl trimethyl ammonium chloride, palmityl trimethyl ammonium chloride, cetyl pyridinium, octadecyl trimethyl ammonium chloride, stearyl dimethyl benzyl ammonium chloride etc.; Add-on is 80～120% molar equivalents of sodium bentonite cation exchange capacity.
Described intercalator is a kind of in hexanolactam, fatty alcohol-polyoxyethylene ether AEO, the octadecyl Soxylat A 25-7.
Described solvent is deionized water or dehydrated alcohol.
Adopt the organobentonite main component of the inventive method preparation as follows:
(1) the high-quality sodium bentonite is 50～70 parts
(2) the quaternary amine organic modifiers is 20～30 parts
(3) intercalator is 10～15 parts
(4) water is 700～1300 parts
Above-mentioned sodium bentonite is pulverulent mixture, montmorillonite weight percentage 85～100%, and its cation exchange capacity (CEC) is 100～300mmol/100g, colloid index 350-500 ml/15g, expansion capacity 85-95 ml/g.
Embodiment:Further specify content of the present invention below in conjunction with embodiment:
Embodiment 1: 50 parts sodium base soil are distributed in 700 parts of deionized waters, and high-speed stirring obtains stable suspension, and the pH value to 7 of adjustment suspension ~ 8 are for subsequent use; 20 parts of palmityl trimethyl ammonium chlorides are dissolved in 300 parts of deionized waters, stir, make it to become the solution for standby of clear.10 parts of hexanolactams are dissolved in 100 parts of deionized waters, stir, make it to become the solution for standby of clear.Under the high-speed stirring state, palmityl trimethyl ammonium chloride solution is added to rapidly in the suspension, reaction is 1.5 hours in the time of 75 ℃, continues to add caprolactam solution, stirring reaction 1 hour.Product is cooled to room temperature, repeatedly removes Cl remaining in the product with deionized water
-, filter, the organobentonite of preparation in 70 ℃ of vacuum-dryings, pulverizing and cross 200 mesh sieves, is namely obtained the organobentonite product.
Embodiment 2: 60 parts sodium base soil are distributed in 800 parts of deionized waters, and high-speed stirring obtains stable suspension, and the pH value to 7 of adjustment suspension ~ 8 are for subsequent use; 22 parts of octadecyl trimethyl ammonium chloride are dissolved in 200 parts of ethanol, stir, make it to become the solution for standby of clear.11 parts of AEO are dissolved in 100 parts of deionized waters, stir, make it to become the solution for standby of clear.Under the high-speed stirring state, octadecyl trimethyl ammonium chloride solution is added to rapidly in the suspension, reaction is 1.5 hours in the time of 70 ℃, continues to add AEO solution, stirring reaction 1 hour.Product is cooled to room temperature, repeatedly removes Cl remaining in the product with deionized water
-, filter, the organobentonite of preparation in 75 ℃ of vacuum-dryings, pulverizing and cross 200 mesh sieves, is namely obtained the organobentonite product.
Embodiment 3: 65 parts sodium base soil are distributed in 800 parts of deionized waters, and high-speed stirring obtains stable suspension, and the pH value to 7 of adjustment suspension ~ 8 are for subsequent use; 24.8 parts of stearyl dimethyl benzyl ammonium chlorides are dissolved in 200 parts of ethanol, stir, make it to become the solution for standby of clear.10.5 parts of octadecyl Soxylat A 25-7s are dissolved in 100 parts of deionized waters, stir, make it to become the solution for standby of clear.Under the high-speed stirring state, stearyl dimethyl benzyl ammonium chloride solution is added to rapidly in the suspension, reaction is 1.5 hours in the time of 70 ℃, continues to add octadecyl polyoxyethylene ethereal solution, reacts 1 hour.Product is cooled to room temperature, repeatedly removes Cl remaining in the product with deionized water
-, filter, the organobentonite of preparation in 70 ℃ of vacuum-dryings, pulverizing and cross 200 mesh sieves, is namely obtained the organobentonite product.
The organobentonite performance is carried out interlamellar spacing and rheological is estimated:
(1) interlamellar spacing test: adopt x-ray powder diffraction instrument, according to the Bragg equation: (wherein d is interlamellar spacing to 2dsin2 θ=n λ, θ is input angle, λ=0.1540nm, wavelength for incident ray, n is diffraction progression, gets 1) can calculate sodium bentonite and bentonite interlamellar spacing d (001).
(2) rheological (normal temperature): take by weighing the organophilic clay of 10.5 g, pour into 350ml0 is housed
#The height of diesel oil stirs in the cup, stirs 10 min under the 3000r/min condition, makes its dispersion, and then high-speed stirring 10 min under 11000r/min measure apparent viscosity, plastic viscosity and yield values under 25 ℃.
Evaluation result is as follows:
Can be found out by above-mentioned data: its interlamellar spacing of organobentonite of this forwarding method preparation is higher, and good rheological property is arranged in diesel oil.
Claims (3)
1. high-performance method for preparing organobentonite is characterized in that carrying out according to the method for being prepared as follows: (1) is dissolved in 50～70 parts sodium bentonite siccative in 600～900 parts the deionized water, and high-speed stirring forms suspension system a; (2) 15～30 parts of quaternary amine organic modifiers is miscible in 100～300 parts of solvents, stirring and dissolving forms homogeneous system b; (3) 10～15 parts of intercalators are dissolved in 100～150 parts of solvents, stirring and dissolving forms homogeneous system c; (4) under whipped state, solution b is joined rapidly among the suspension system a, 70～90 ℃ of reactions 1-2 hour, form homogeneous system d; (5) under whipped state, solution c is added rapidly among the suspension system d, 70～90 ℃ of reactions 1-2 hour;
The product that obtains in the step (5) is cooled to room temperature, and unnecessary ion in the flush away product filters, and is then that the solid product of gained is dry under 60～80 ℃ of vacuum environments, pulverizes 200 mesh sieves, namely obtains the organophilic clay product;
Described intercalator is a kind of in hexanolactam, fatty alcohol-polyoxyethylene ether AEO, the octadecyl Soxylat A 25-7; Solvent is deionized water or dehydrated alcohol.
2. according to preparation method claimed in claim 1, it is characterized in that the quaternary amine organic modifiers is a kind of in palmityl trimethyl ammonium chloride, cetyl pyridinium, octadecyl trimethyl ammonium chloride, the stearyl dimethyl benzyl ammonium chloride, add-on is 80～120% molar equivalents of sodium bentonite cation exchange capacity.
3. according to preparation method claimed in claim 1, it is characterized in that the organophilic clay main component that adopts the method to make is as follows:
(1) the high-quality sodium bentonite is 50～70 parts
(2) the quaternary amine organic modifiers is 15～30 parts
(3) intercalator is 10～15 parts
(4) water is 600～1300 parts
Above-mentioned sodium bentonite is pulverulent mixture, montmorillonite weight percentage 85～100%, and its cation exchange capacity (CEC) is 100～300mmol/100g, colloid index 350-500ml/15g, expansion capacity 85-95ml/g.
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| CN103936021A (en) * | 2014-04-04 | 2014-07-23 | 浙江工业大学 | Method for preparing organobentonite with low viscosity and high settling resistance |
| CN105733529A (en) * | 2014-12-11 | 2016-07-06 | 中国石油化工股份有限公司 | Method for preparing organobentonite for white oil based drilling fluid |
| CN106542536A (en) * | 2015-09-16 | 2017-03-29 | 中国石油化工股份有限公司 | A kind of high-performance oil-based drilling fluid method for preparing organobentonite |
| CA2998756A1 (en) * | 2015-09-18 | 2017-03-23 | Bfp Management, Llc | Synthetic agricultural product |
| CN106634892A (en) * | 2016-08-26 | 2017-05-10 | 潍坊天福化学科技有限公司 | High-temperature-resistant drilling organic soil and preparation method thereof |
| CN106701734A (en) * | 2017-02-08 | 2017-05-24 | 光合强化（北京）生物科技有限公司 | Modified bentonite adsorbent for fixing benzene degrading bacterium |
| CN109704353A (en) * | 2017-10-25 | 2019-05-03 | 中国石油化工股份有限公司 | Oil resistant base drilling fluid method for preparing organobentonite |
| CN110527500A (en) * | 2018-05-24 | 2019-12-03 | 中国石油化工股份有限公司 | White oil base drilling fluid method for preparing organobentonite |
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| CN110105930B (en) * | 2019-04-23 | 2021-05-07 | 上海勃利燃气设备有限公司 | Bentonite drilling fluid and preparation method thereof |
| CN110844915B (en) * | 2019-11-22 | 2021-08-03 | 浙江康百欣新材料有限公司 | Modified organic bentonite and preparation method and application thereof |
| CN111748326B (en) * | 2020-06-22 | 2022-11-22 | 中国石油天然气集团有限公司 | Cutting agent for biodiesel-based drilling fluid and preparation method thereof |
| CN113336238B (en) * | 2021-06-22 | 2023-11-17 | 中石化南京化工研究院有限公司 | Preparation method of organic soil for high-temperature-resistant water-in-oil drilling fluid |
| CN118496828B (en) * | 2024-07-19 | 2024-10-25 | 淄博联技化工有限公司 | Composite modified organic bentonite and preparation method and application thereof |
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| CN1052094A (en) * | 1989-11-30 | 1991-06-12 | 中国石油化工总公司石油化工科学研究院 | Organic bentonite gelatinizer and preparation method thereof |
| JP2722177B2 (en) * | 1994-12-20 | 1998-03-04 | 豊順鉱業株式会社 | Method for activating clay and its product |
| CN101624515B (en) * | 2009-08-05 | 2013-03-06 | 湖北汉科新技术股份有限公司 | Organic clay with high jellification rate in white oil and preparation method thereof |
| CN101870476A (en) * | 2010-05-14 | 2010-10-27 | 淄博联技化工有限公司 | Method for producing temperature-resistant organically modified bentonite |
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Address after: Liuhe District of Nanjing City, Jiangsu province 210048 geguan Road No. 699 Patentee after: CHINA PETROCHEMICAL Corp. Patentee after: SINOPEC NANJING CHEMICAL RESEARCH INSTITUTE Co.,Ltd. Address before: Liuhe District of Nanjing City, Jiangsu province 210048 geguan Road No. 699 Patentee before: CHINA PETROCHEMICAL Corp. Patentee before: Nanhua Group Research Institute |