CN103145140A - Preparation method of modified organic bentonite - Google Patents
Preparation method of modified organic bentonite Download PDFInfo
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- CN103145140A CN103145140A CN2013100345125A CN201310034512A CN103145140A CN 103145140 A CN103145140 A CN 103145140A CN 2013100345125 A CN2013100345125 A CN 2013100345125A CN 201310034512 A CN201310034512 A CN 201310034512A CN 103145140 A CN103145140 A CN 103145140A
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- bentonite
- sodium bentonite
- organic modified
- modified organic
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- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 229910000278 bentonite Inorganic materials 0.000 title abstract description 16
- 239000000440 bentonite Substances 0.000 title abstract description 16
- ONCZQWJXONKSMM-UHFFFAOYSA-N dialuminum;disodium;oxygen(2-);silicon(4+);hydrate Chemical compound O.[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Na+].[Na+].[Al+3].[Al+3].[Si+4].[Si+4].[Si+4].[Si+4] ONCZQWJXONKSMM-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229940080314 sodium bentonite Drugs 0.000 claims abstract description 47
- 229910000280 sodium bentonite Inorganic materials 0.000 claims abstract description 47
- 239000000725 suspension Substances 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- ZORQXIQZAOLNGE-UHFFFAOYSA-N 1,1-difluorocyclohexane Chemical compound FC1(F)CCCCC1 ZORQXIQZAOLNGE-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229940035049 sorbitan monooleate Drugs 0.000 claims abstract description 13
- 235000011069 sorbitan monooleate Nutrition 0.000 claims abstract description 13
- 239000001593 sorbitan monooleate Substances 0.000 claims abstract description 13
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 230000010355 oscillation Effects 0.000 claims abstract description 7
- 239000008267 milk Substances 0.000 claims description 14
- 210000004080 milk Anatomy 0.000 claims description 14
- 235000013336 milk Nutrition 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 229940092782 bentonite Drugs 0.000 abstract description 15
- 238000005553 drilling Methods 0.000 abstract description 10
- 238000002441 X-ray diffraction Methods 0.000 abstract description 6
- 239000011229 interlayer Substances 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 239000012530 fluid Substances 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract 3
- 238000004026 adhesive bonding Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 11
- 229910052901 montmorillonite Inorganic materials 0.000 description 8
- 241000282326 Felis catus Species 0.000 description 7
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical group O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 6
- 239000010410 layer Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000003921 oil Substances 0.000 description 5
- 239000004033 plastic Substances 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 238000013461 design Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000009830 intercalation Methods 0.000 description 3
- 230000002687 intercalation Effects 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- 241000446313 Lamella Species 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000032798 delamination Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000012747 synergistic agent Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
Images
Abstract
The invention relates to a preparation method of modified organic bentonite. The preparation method of the modified organic bentonite includes the following steps: (1), water is added to sodium bentonite and stirred to obtain sodium bentonite suspension liquid; (2), at room temperature, cetyl trimethyl ammonium bromide is dissolved in water, and then sorbitan monooleate is added to the liquid cetyl trimethyl ammonium bromide to obtain lactescence; and (3), the obtained sodium bentonite suspension liquid and the lactescence are mixed to carry out a constant temperature oscillation reaction, are cooled to the room temperature, and are centrifuged, washed, dried, smashed and filtered by a sieve to obtain the modified organic bentonite. An X-ray diffraction (XRD) spectrogram of products displays that the interlayer spacing expanding value of the prepared modified organic bentonite reaches 2.0-3.5nm, and the modified organic bentonite has better compatibility compared with organic substances. The modified organic bentonite is used as annexing agent of white oil-based drilling fluid, and the gluing rate can be improved to 95%-100%.
Description
Technical field
The present invention relates to a kind of novel preparation method for bentonite, particularly a kind of preparation method of organic modified bentonite.
Background technology
Wilkinite has another name called otaylite, amargosite, polynite etc., is by tuff or other volcanic rock alteration and a kind of pillared layered compound of forming under the effect of alkaline water.Its main component is montmorillonite, wherein contains SiO
2, Al
2O
3, Fe
2O
3, FeO, MgO, CaO, Na
2O, K
2O, TiO
2, H
2O。Montmorillonite is a kind of silico-aluminate of two dimensional surface stratiform structure, it is formed alternately by tetrahedron and octahedra tetrahedron (T) and the octahedral sheet (O) that forms respectively, the topmost structural unit of montmorillonite is the 2:1 layer, i.e. T-O-T layer that octahedral sheet forms of two tetrahedral sheet folders.Tetrahedral sheet is take silicon-oxy tetrahedron as main, wherein coordination Si
4+By Al
3+, Fe
3+The plasma displacement.Octahedron is comprised of six Sauerstoffatoms or hydroxide radical, and central ion is mainly the Al of hexa-coordinate
3+, it can be by Fe
3+, Fe
2+, Mg
2+, Li
+Deng replacement.When the positively charged ion in octahedron, tetrahedron is replaced at a low price, make primary structure increase the negative charge of equivalent, the compensation of interlayer Liquidity limit is arranged.Form electric dipole between the positively charged ion between montmorillonite layer and crystal skeleton, a little less than adding that between the montmorillonite crystal layer, bonding force, can adsorb polar water molecules, according to cation type and relative humidity, interlayer can adsorb the water molecules of one deck or two layers.In addition, also can adsorb certain water molecules at the montmorillonite grain surface.Water of constitution is present in lattice with OH base form.
Wilkinite is as a kind of important nonmetallic minerals, and reserves are large, have a very wide distribution.There are the U.S., China, Russia, Italy, Greece, India and Germany in bentonitic major country of production.At present, no matter be petroleum drilling or geological prospecting drilling well, all adopt in a large number the drilling mud of wilkinite preparation.Wilkinite can improve mud yield and drilling benefit greatly as the synergistic agent that adds, and is conducive to creep into various complicated geologicals, and in the prevention well, accident occurs.Because the development of China Petroleum increases with the wilkinite demand year by year to drilling fluid, wilkinite has a extensive future aspect petroleum drilling.
Drilling mud plays an important role in drilling well, and bore slurry and be divided into two classes: a class is mud, and carrier is mainly water, and wilkinite is thickening material; Another kind of is oil-base mud, and carrier is mainly crude oil, diesel oil and white oil.Due to oil loving requirement, mainly adopt organic bentonite.
Be mainly to utilize cats product as properties-correcting agent to bentonitic research and production method both at home and abroad at present, by wet method, dry method or pre-gel, sodium bentonite carried out intercalation ion-exchange.Also there is research to coordinate nonionogenic tenside or anion surfactant as properties-correcting agent cats product.Nonionogenic tenside, alkylamine, amino acid, coupling agent or alcohols etc. also are used to bentonitic intercalation or finishing organises wilkinite in addition.
Bentonite use be all generally with the basis that is mixed into of organic substance, therefore prepared organobentonite lamella organic decoration more abundant, sheet interlayer spacing is larger, illustrate that between lamella, reactive force is less, arrangement is more random, just better with the consistency of organic substance, the bentonite application performance is just better.
Therefore, provide a kind of technique simple, the organic modified bentonite composite manufacture method that production cost is low just becomes the technical barrier that this technical field is badly in need of solution.
Summary of the invention
The purpose of this invention is to provide a kind of technique simple, the preparation method of the organic modified bentonite that production cost is low.
Above-mentioned purpose of the present invention reaches by the following technical programs:
A kind of preparation method of organic modified bentonite comprises the steps:
(1) sodium bentonite is added entry and stir, get sodium bentonite suspension;
(2) at room temperature, cetyl trimethylammonium bromide is water-soluble, and then add sorbitan monooleate to stir, get milk sap;
(3) step (1) gained sodium bentonite suspension is mixed with step (2) gained milk sap, carry out the constant temperature oscillation reaction, be cooled to room temperature by after centrifugal, washing, drying, pulverizing, crossing mesh sieve, obtain product.
With in the described sodium bentonite suspension of step (1) take every kilogram of sodium bentonite as benchmark, described in step (2), the cetyl trimethylammonium bromide add-on is 0.5 ~ 2.5mol, the add-on of described sorbitan monooleate is 0.5 ~ 2.5mol.
In step (1), the weight ratio of described sodium bentonite and water is (1 ~ 5): (99 ~ 95), namely 1: 99 ~ 5: 95; The preparation method of described sodium bentonite suspension is: adopting natural sodium bentonite or artificial sodium bentonite is raw material, with obtaining after water-dispersion; After also used water is disperseed, then after removing precipitated impurities, centrifugation obtains.Suspension concentration is about 1 ~ 5wt%.
In step (2), add sorbitan monooleate to stir 1.0 ~ 2.0 hours, get milk sap.
In step (3), the temperature of described constant temperature oscillation reaction is 50 ℃ ~ 90 ℃, and the time is 4 ~ 12 hours; Described drying temperature is 60 ℃ ~ 105 ℃; The described order number of crossing mesh sieve is 200 orders.
The present invention is directed to the problem that known technology exists, provide a kind of sodium bentonite suspension that utilizes to be raw material, prepare the bentonite method by cetyl trimethylammonium bromide and sorbitan monooleate absorption intercalation.Can obtain quality products, can realize that again technique is simple, reduce production costs.
The present invention compared to the prior art, significantly characteristics are in sodium bentonite suspension, add the milk sap of cats product and nonionogenic tenside.As everyone knows, sodium bentonite is subjected to aquation can act on can be in water stable suspended dispersed, and then delamination, and on the laminate of its delamination the time with negative electricity.Positively charged vesica in the milk sap of the formation of cats product and nonionogenic tenside will be because of electrostatic attraction and Van der Waals force and is adsorbed on electronegative wilkinite laminate.Because its bonding force is stronger, can not washed off in the process of centrifugation washing.In the process of drying, because water molecules between laminate volatilizees gradually, destroyed original balance and caused vesica to break, thereby made cats product and nonionogenic tenside arrange expansion between bentonite bed.At this moment, at wilkinite surface and interlayer, nonionogenic tenside also is attracted to wilkinite surface and interlayer because of Van der Waals force and hydrogen bond action to cats product because of chemisorption.This legal system that Here it is has the bentonitic principle of machine.
The present invention will be further described below by the drawings and the specific embodiments, but and do not mean that limiting the scope of the invention.
Description of drawings
Fig. 1 is the bentonite plastic design sketch of sodium bentonite and embodiment of the present invention 1-5 preparation.
Fig. 2 is the bentonite x-ray diffraction pattern of sodium bentonite and the embodiment of the present invention 1 preparation.
Embodiment
The preparation method of organic modified bentonite of the present invention, take sodium bentonite as the suspension raw material, the milk sap that mixes that adds cetyl trimethylammonium bromide and sorbitan monooleate, main points are when this milk sap mixes, to fully the complete mixed dissolution of cetyl trimethylammonium bromide and sorbitan monooleate be become milky milk sap, again this milk sap is joined in sodium bentonite suspension, the hydrophobic precipitated thing that produces, dry after separation washes away ion, cross mesh sieve after pulverizing and obtain the organobentonite product.
Above-mentioned cetyl trimethylammonium bromide add-on be in the sodium bentonite suspension every kilogram of na-montmorillonite as benchmark, add-on is 0.5 ~ 1.5mol, the add-on of sorbitan monooleate is also that every kilogram of na-montmorillonite is as benchmark in the sodium bentonite suspension, and add-on is 0.5 ~ 1.5mol.After being mixed, these two kinds of tensio-active agents join in the suspension of sodium bentonite.
Preparation sodium bentonite suspension: adopting the natural sodium bentonite of 20g or artificial sodium bentonite is raw material, use 1980g(ml) after water-dispersion, remove precipitated impurities through centrifugation, acquisition concentration is about the sodium bentonite suspension 2kg of 1wt%.
Take the 10mmol cetyl trimethylammonium bromide and join in 1L water, after dispersed with stirring is water-soluble, add the sorbitan monooleate of 10mmol, stir; Fully reaction was stirred after 1 hour, got milk sap.
The sodium bentonite suspension of preparation is mixed with milk sap, 50 ℃ of lower constant temperature oscillation reactions 4 hours.After being cooled to room temperature, centrifugation, take off the layer paste, the washing.200 purpose mesh sieves are crossed in 60 ℃ of dryings, pulverizing afterwards, namely obtain organobentonite sample 1.
Embodiment 2-5
Adopting the natural sodium bentonite of 20g or artificial sodium bentonite is raw material, implementation method is identical with embodiment 1, change concentration and the emulsification times of sodium bentonite suspension concentration, cetyl trimethylammonium bromide and sorbitan monooleate, change constant temperature oscillation reaction times temperature, change drying temperature, prepare organobentonite sample 2-5 with reference to the method for embodiment 1.Design parameter is as shown in table 1.
The experiment condition of table 1 embodiment 2-5
As shown in Figure 1, be the plastic design sketch of the organobentonite sample 1-5 of sodium bentonite and embodiment of the present invention 1-5 preparation.Organobentonite sample 1-5 with 1 gram sodium bentonite and embodiment 1-5 preparation joins in the 50ml white oil respectively, 11000rpm stirs 10min, observe the plastic effect, from left to right be respectively the plastic effect of the organobentonite sample 1-5 of sodium bentonite and embodiment 1-5 preparation in Fig. 1.As can be seen from Figure 1, after modification, the dispersiveness of organobentonite sample 1-5 in white oil significantly improves.
As shown in Figure 2, be the x-ray diffraction pattern of the organobentonite sample 1 of sodium bentonite and the embodiment of the present invention 1 preparation.In Fig. 2, curve 1 is the x-ray diffraction pattern of sodium bentonite, curve 2 is the x-ray diffraction pattern of the organobentonite sample 1 of embodiment 1 preparation, analyze by little angle XRD grating spectrum, show that organic modified bentonite of the present invention compares with sodium bentonite, 001 diffraction peak of spectrogram has considerable change.2 θ of the angle of the sign of sodium bentonite=6.8, interlamellar spacing are 1.30nm; 2 θ of the organic modified bentonite of the present invention's preparation are in 2.0 left and right, the XRD spectra of product shows that the interlamellar spacing expansion value of organic modified bentonite reaches 2.0nm ~ 3.5nm, existing more cats product and the nonionogenic tenside of proof entered bentonite bed, and organic modified bentonite has and the better consistency of organic substance.
Use: the organic modified bentonite of the present invention's preparation is as the additive of white oil base drilling fluid, and the plastic rate is increased to 95% ~ 100%.
Claims (8)
1. the preparation method of an organic modified bentonite, comprise the steps:
(1) sodium bentonite is added entry and stir, get sodium bentonite suspension;
(2) at room temperature, cetyl trimethylammonium bromide is water-soluble, and then add sorbitan monooleate to stir, get milk sap;
(3) the sodium bentonite suspension with gained mixes with milk sap, carries out the constant temperature oscillation reaction, is cooled to room temperature by after centrifugal, washing, drying, pulverizing, crossing mesh sieve, obtains organic modified bentonite.
2. the preparation method of organic modified bentonite according to claim 1, it is characterized in that: take every kilogram of sodium bentonite as benchmark, the add-on of cetyl trimethylammonium bromide is 0.5 ~ 2.5mol, and the add-on of sorbitan monooleate is 0.5 ~ 2.5mol.
3. the preparation method of organic modified bentonite according to claim 1 is characterized in that: during preparation sodium bentonite suspension, the weight ratio of sodium bentonite and water is 1 ~ 5: 99 ~ 95.
4. the preparation method of organic modified bentonite according to claim 3, it is characterized in that: the preparation method of described sodium bentonite suspension is: adopting natural sodium bentonite or artificial sodium bentonite is raw material, use water-dispersion, obtain after precipitated impurities is removed in centrifugation.
5. the preparation method of organic modified bentonite according to claim 1, is characterized in that: add sorbitan monooleate to stir 1.0 ~ 2.0 hours, get milk sap.
6. the preparation method of organic modified bentonite according to claim 1 is characterized in that: the temperature of described constant temperature oscillation reaction is 50 ℃ ~ 90 ℃, and the time is 4 ~ 12 hours.
7. the preparation method of organic modified bentonite according to claim 1, it is characterized in that: described drying temperature is 60 ℃ ~ 105 ℃.
8. the preparation method of organic modified bentonite according to claim 1, it is characterized in that: the order number of described mesh sieve is 200 orders.
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CN103145140B CN103145140B (en) | 2014-12-03 |
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CN104961578A (en) * | 2015-06-26 | 2015-10-07 | 王基敬 | Production process of high-concentration suspension liquid drip irrigation fertilizer |
CN104961577A (en) * | 2015-06-26 | 2015-10-07 | 刘志勇 | Magnetic liquid drip irrigation fertilizer and production method thereof |
CN106883831A (en) * | 2017-04-12 | 2017-06-23 | 中国地质大学(北京) | A kind of new oil base drilling fluid organic sepiolite and preparation method thereof |
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CN114425032B (en) * | 2021-12-23 | 2023-05-12 | 湖南人文科技学院 | Moisturizing and anti-inflammatory composition and preparation method and application thereof |
CN114516769A (en) * | 2022-02-21 | 2022-05-20 | 烟台浩景农业科技有限公司 | Organic and inorganic fertilizer and preparation method thereof |
CN115043411A (en) * | 2022-06-29 | 2022-09-13 | 北京化工大学 | Organic modification method of sodium-based montmorillonite and organic sodium-based montmorillonite |
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