CN101948116A - Method for improving dispersibility of organic soil - Google Patents
Method for improving dispersibility of organic soil Download PDFInfo
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- CN101948116A CN101948116A CN 201010254510 CN201010254510A CN101948116A CN 101948116 A CN101948116 A CN 101948116A CN 201010254510 CN201010254510 CN 201010254510 CN 201010254510 A CN201010254510 A CN 201010254510A CN 101948116 A CN101948116 A CN 101948116A
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- organophilic clay
- oil
- soluble nonionic
- active agent
- surface active
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Abstract
The invention provides a method for improving dispersibility of organic soil. The method comprises the following steps of: (1) taking the organic soil, organic solvent and oil-soluble nonionic surfactant; and (2) mixing the organic soil, the organic solvent and the oil-soluble nonionic surfactant in random order to form mixed solution; stirring the mixed solution at room temperature for uniform dispersion, wherein for the oil-soluble nonionic surfactant which is solid at the room temperature, the oil-soluble nonionic surfactant is stirred on the premise of ensuring the dissolution temperature of the solid oil-soluble nonionic surfactant after being mixed with the organic soil and the organic solvent; and obtaining an organic soil colloidal dispersion system with good dispersibility and high stability after stirring for uniform dispersion. The method has simple and convenient operation, and can effectively improve the dispersion degree of the organic soil in the non-polar solvent and the stability of the dispersion system colloid, obviously shorten the dispersion time of the organic soil in the non-polar solvent, reduce the energy consumption and reduce the cost.
Description
Technical field
The present invention relates to a kind of dispersiveness of organophilic clay in non-polar solvent and method of colloidal dispersion stability improved, belong to the organophilic clay applied technical field.
Background technology
For satisfying requirements such as environmental protection, drilling speed, the oil base drilling fluid base oil tends to the mineral oil that adopts viscosity less now, also or gas system wet goods, simultaneously lubricating grease, low polarity coating etc. also more adopts nonpolar alkane solvents as the base oil solvent, but it is generally relatively poor to have used the dispersiveness of organophilic clay in these non-polar solvents of thickening power always.If consider from the process for manufacturing organoclays process, and improved, with preparation dispersed better organophilic clay in these a little solvents, then usually can make the process complexity, industrialization is difficult.
Chinese patent literature CN86105312 discloses a kind of " improving the method for dispersibility of organoclays ", be easy to a kind of organic clay of dispersive in the liquid organic assembling by the follow procedure preparation: a kind of montmorillonite is suspended in water, form a kind of mobile suspension: with this suspension of solution-treated of a kind of inorganic salt, its positively charged ion is preferably divalence, the concentration of this salt should be able to make montmorillonitic clay flocculation fully basically, the montmorillonitic clay suspension of flocculation is mixed with a kind of quaternary ammonium compound, have at least one to be 10-24 carbon atom in four alkyl of the latter; Then make resulting product dehydration.
Above-mentioned patent is to consider from the organophilic clay preparation process, is improved, to make dispersed better organophilic clay, that is focusing on the dispersed better preparation process of organophilic clay, this method process has a little loaded down with trivial details, and it adopts the wet method preparation, water consumption is bigger, and it is more relatively to consume energy.
Summary of the invention
The present invention is directed to dispersing property difference that existing organophilic clay exists in non-polar solvent at non-aqueous media especially some commercial organophilic clays with and the problem of colloidal dispersion system poor stability, a kind of method of improving the organophilic clay dispersiveness is provided, also can obtains stable organophilic clay colloidal dispersion system with the dispersiveness of effective raising organophilic clay in non-aqueous media especially non-polar solvent and stability.
The method of improving the organophilic clay dispersiveness of the present invention may further comprise the steps:
(1) get organophilic clay, organic solvent and oil soluble nonionic surface active agent, wherein the organophilic clay quality is the 0.2%--5% of three's total mass, and the quality of oil soluble nonionic surface active agent is the 10%--200% of organophilic clay quality.
(2) organophilic clay, organic solvent and oil soluble nonionic surface active agent three (can be scattered in organophilic clay preparation organophilic clay dispersion system in the organic solvent earlier, add the oil soluble nonionic surface active agent again in the organophilic clay dispersion system with the random order mixing; Perhaps together be scattered in organophilic clay and oil soluble nonionic surface active agent in the organic solvent; Perhaps earlier the oil soluble nonionic surface active agent is added organic solvent and makes solution, again organophilic clay is added in this solution), make mixed solution; This mixed solution stirred under room temperature it is uniformly dispersed; And under the room temperature being solid-state oil soluble nonionic surface active agent (as Span-60), when stirring after organophilic clay and organic solvent are mixed, need guarantee to carry out under this solid oil dissolubility nonionic surface active agent solvent temperature (this temperature usually greater than 50 ℃, and be generally less than 200 ℃); After being uniformly dispersed it, stirring promptly obtains organophilic clay colloidal dispersion system better dispersed and that stability is higher.
For normal temperature down for solid oil soluble nonionic surface active agent also can with its with the organophilic clay room temperature under make mixture after the mixed grinding pulverizing, again this mixture is scattered in the organic solvent.
Described organophilic clay is with single long carbochain quaternary ammonium compound (as octadecyl trimethyl ammonium chloride, cetyl trimethylammonium bromide etc.) or carbochain quaternary ammonium compound made various commercial organophilic clays of various quaternary ammonium compound modified alta-muds, polynite or like derivatives such as (as distearyl dimethyl ammonium chloride, two h-tallow base alkyl dimethyl ammonium chloride, two h-tallow ylmethyl benzyl ammonium chlorides etc.) how long, or tests the organophilic clay of indoor these properties-correcting agent wet technique refinements.The long carbochain of quaternary ammonium compound positively charged ion is the saturated and unsaturated alkyl of 10-24 carbon atom, and all the other can be the saturated and unsaturated alkyl of 1-24 carbon atom or the aromatic alkyl of 7-10 carbon atom, and negatively charged ion can be Cl
-, Br
-, I
-, OH
-, CH
3SO
4 -Deng.
Organic solvent is as dispersion medium, be mainly each organic solvent commonly used of organophilic clay Application Areas, nonpolar alkanes organic solvent more commonly used is as mixed alkanes class organic solvent (as gas system oil, paraffin wet goods) and N-alkanes hydro carbons organic solvent (as octane etc.).
The oil soluble nonionic surface active agent is mainly some polyhydric alcohol fatty acid esters, comprises Span series (as Span-80, Span-60 etc.) and glyceryl ester series (as glyceryl monooleate etc.).
The present invention is by adding dispersiveness and the system colloidal stability that treatment agent improves organophilic clay, operation is easy to implement, can effectively improve degree of scatter and the dispersion system colloidal stability of organophilic clay in non-polar solvent, be applicable to and improve the dispersiveness of commercial organophilic clay in nonpolar alkane solvents commonly used, can obviously shorten organophilic clay and in non-polar solvent, disperse required time, cut down the consumption of energy, reduce cost, while additive safety and environmental protection, effect is obvious, better with other treatment agent compatiblenesies in systems such as oil base drilling fluid, and applicable object is comparatively extensive.
Description of drawings
Fig. 1 adds Span-80 and does not add relatively picture of each organophilic clay dispersion stability of Span-80.
Fig. 2 is that the effect after the dispersed and employing additive Span-80 of laboratory self-control organophilic clay in three kinds of oil phases improves compares picture.
Fig. 3 is the comparison picture that improves organophilic clay dispersiveness and system colloidal stability with glyceryl monooleate as additive.
Fig. 4 is that it improves the comparison picture of organophilic clay dispersiveness and system colloidal stability under certain condition as additive with Span-60.
Embodiment
Embodiment 1
Present embodiment is to prepare the organophilic clay dispersion system earlier, in the organophilic clay dispersion system, add an amount of oil soluble nonionic surface active agent, by suitable shearing action (alr mode all adopts weak shearing among the embodiment), obtain organophilic clay dispersion system better dispersed and that stability is higher, detailed process is as follows:
The 0.3g organophilic clay is scattered in the gas system oil of respective amount, 0.09g Span-80 (S80 is added in the back in this dispersion system, occupy machine soil property amount 30%), make the organophilic clay massfraction and be 2% organic rustic system oil dispersion system (2.0wt%), the rotating speed induction stirring that mixture (gross weight 15g) is changeed with per minute 300 under room temperature 12 hours, after be transferred in the 25ml colorimetric cylinder, leave standstill, the free oil height is separated out on colorimetric cylinder top when writing down 90 minutes, and organophilic clay colloidal dispersion system height accounts for total dispersion system height percentage ratio bottom calculating, and promptly draws into the glue rate.Following table is that the glue rate that becomes after three kinds of organophilic clays are not added any additives and added Span-80 contrasts:
| Project | Become glue rate/% in the gas system oil | Become glue rate/% after adding Span-80 |
| Dynagel 21 (D21 commercial organophilic clay) | 81.5 | 100 |
| Dynagel 31 (D31 commercial organophilic clay) | 99.5 | 100 |
| Domestic certain producer's organophilic clay (Z) | 14.8 | 93.4 |
If by changing 6 hours last 12 hour into, and all the other conditions are all identical with magneton churning time under the room temperature, and by as above-mentioned method calculate each system and become the glue rate, after then three kinds of organophilic clays are not added any additives and are added Span-80 to become the glue rate to contrast as shown in the table:
| Project | Become glue rate/% in the gas system oil | Become glue rate/% after adding Span-80 |
| Dynagel 21 (D21 commercial organophilic clay) | 42.5 | 100 |
| Dynagel 31 (D31 commercial organophilic clay) | 90.3 | 100 |
| Domestic certain producer's organophilic clay (Z) | 11.1 | 91.7 |
Can obviously improve the one-tenth glue effect of some commercial organophilic clays in non-polar solvent after adding a small amount of Span-80 as can be seen by above data.
Embodiment 2
With the organophilic clay massfraction among the embodiment 1 by 2% becoming 5% (preparation organophilic clay massfraction is 5% organic rustic system oil dispersion system), and the Span-80 addition becomes 10% by above 30% of the machine soil property amount of occupying, the rotating speed induction stirring that change with per minute 300 under room temperature the back 30 minutes, and all the other conditions are all identical, after be transferred in the 25ml colorimetric cylinder, leave standstill, the free oil height is separated out on colorimetric cylinder top when writing down 90 minutes, and calculate each system by embodiment 1 method and become the glue rate, become the contrast of glue rate as shown in the table after then three kinds of organophilic clays are not added any additives and added Span-80:
| Project | Become glue rate/% in the gas system oil | Become glue rate/% after adding Span-80 |
| Dynagel 21 (D21 commercial organophilic clay) | 24.6 | 99.7 |
| Dynagel 31 (D31 commercial organophilic clay) | 88.6 | 100 |
| Domestic certain producer's organophilic clay (Z) | 11.4 | 34.7 |
As can be seen shearing dynamics less (the induction stirring dynamics is less), jitter time is shorter by above data, adds Span-80 and measures under the less condition, also can obviously improve the one-tenth glue effect of some commercial organophilic clays in non-polar solvent.
Embodiment 3
Present embodiment is each organophilic clay dispersion system colloidal stability experiment.
The 0.03g organophilic clay is scattered in the respective amount gas system oil, in the experimental group dispersion system, add 0.06g Span-80 (be organophilic clay quality 200%) formation mixture, and control group does not add any additives, making massfraction is 0.2% organic rustic system oil dispersion system (0.2wt%), after mixture (gross weight 15g) is placed on the magnetic stirrer, under room temperature with walk around fast induction stirring 12 hours of per minute 300, after be transferred in the 25ml colorimetric cylinder, leave standstill, transfer finishes and leaves standstill after 24 hours and takes pictures respectively, photo as shown in Figure 1, photo when top finishes for shifting, the bottom is for leaving standstill photo after 24 hours.For Fig. 1 middle and upper part photo, wherein 2 colorimetric cylinders (all do not add additive Span-80 person, being control group) obvious sedimentation has taken place in organophilic clay in the interior dispersion system, show that sedimentation has just taken place (leaving standstill approximately 5 minutes) dispersion system in this time period is taken pictures in preparation, promptly secondary indication organophilic clay dispersiveness is relatively poor.Thus picture as can be seen additive Span-80 can obviously promote the dispersed of organophilic clay and improve the dispersion system colloidal stability.Wherein D21 represents Dynagel 21, and D31 represents Dynagel 31, and Z represents domestic certain producer's organophilic clay.
Embodiment 4
Present embodiment is tested its dispersiveness in each oil phase with the self-control organophilic clay.
Respectively 0.03g laboratory wet method self-control organophilic clay is scattered in gas system oil, paraffin oil, in the octane, in the experimental group dispersion system, add 0.03g Span-80 (be organophilic clay quality 100%), make massfraction and be 0.2% organophilic clay dispersion system, (gross weight 15g) places on the magnetic stirrer with mixture, under room temperature with walk around fast induction stirring 12 hours of per minute 300, after be transferred in the 25ml colorimetric cylinder, leave standstill, when transfer finishes and leave standstill after 24 hours and take pictures respectively, photo as shown in Figure 2, photo when top finishes for shifting, the bottom is for leaving standstill photo after 24 hours.In the photo dispersion system that does not add any additives, i.e. control group.
It is comparatively extensive to find out that by Fig. 2 additive Span-80 is suitable for oil phase, can be used in the multiple nonpolar alkane solvents system, to improve the dispersed of organophilic clay and to improve the system colloidal stability.
Embodiment 5
Present embodiment is to be that to test it be the colloidal stability promoter action to the rustic system oil dispersion of certain commercial machine to additive with the glyceryl monooleate.
Domestic certain the producer's organophilic clay (Z) of 0.03g is scattered in the respective amount gas system oil, in the experimental group dispersion system, add 0.06g glyceryl monooleate (be organophilic clay quality 200%) formation mixture, and control group does not add any additives, making massfraction is 0.2% organic rustic system oil dispersion system (every group left side colorimetric cylinder is interior among photo Fig. 3), this kind of 0.3g organophilic clay is scattered in the respective amount gas system oil, in the experimental group dispersion system, add 0.09g glyceryl monooleate (be organophilic clay quality 30%) formation mixture, and control group does not add any additives, making massfraction is 2.0% organic rustic system oil dispersion system (every group right side colorimetric cylinder is interior in the photo), after mixture (gross weight 15g) is placed on the magnetic stirrer, under room temperature with walk around fast induction stirring 2 hours of per minute 300, after be transferred in the 25ml colorimetric cylinder, leave standstill, when transfer finishes and leave standstill after 6 hours and take pictures respectively, photo as shown in Figure 3, photo when top finishes for shifting, the bottom is for leaving standstill photo after 6 hours.Thus picture as can be seen the additive glyceryl monooleate also can comparatively significantly promote the dispersed of organophilic clay and improve the dispersion system colloidal stability.
Embodiment 6
Present embodiment is the mensuration to organophilic clay grain diameter in the dispersion system.
Prepare three kinds of commercial organophilic clays and laboratory wet method respectively and make organic rustic system oil dispersion system by oneself, and add the Span-80 of 200% organophilic clay quality, getting massfraction is that 0.2% organic rustic system oil dispersion is, after mixture is placed on the magnetic stirrer, under room temperature with walk around fast induction stirring 12 hours of per minute 300, after be transferred in the 25ml colorimetric cylinder, left standstill 24 hours, the back adopts dynamic light scattering to survey on it organophilic clay grain diameter in translucent dispersion system of liquid, and measurement result is as shown in the table:
| Project | Particle diameter/nm |
| Dynagel?21 | 211 |
| Dynagel?31 | 215 |
| Domestic certain producer's organophilic clay | 185 |
| The self-control organophilic clay | 215 |
Can find out that by above data additive Span-80 can fundamentally promote the dispersion of organophilic clay, and when additive-free, as shown in Figure 1, the organophilic clay grain diameter is big in its dispersion system, gathering is very fast, sedimentation is very fast.
Embodiment 7
Present embodiment is organophilic clay to be scattered in the non-polar oil solution of oil soluble nonionic surface active agent obtain stable organophilic clay colloidal dispersion system.
First formation organophilic clay dispersion system described in the embodiment 1,2,3,5, back process of adding Span-80 and glyceryl monooleate are changed into directly organophilic clay is scattered in the gas system oil that is dissolved with Span-80 or glyceryl monooleate, and organophilic clay degree of scatter and system colloidal stability effect are suitable with each embodiment income effect in the gained organophilic clay dispersion system.
Embodiment 8
Present embodiment is being that solid oil soluble nonionic surface active agent Span-60 obtains stable organophilic clay colloidal dispersion system as additive under the room temperature.
Commercial organophilic clay Dynagel 21 and Span-60 are pulverized by 2: 1 (Span-60 is an organophilic clay quality 50%) mixed grindings of mass ratio, and the gained organophilic clay is designated as organophilic clay A.Commercial organophilic clay Dynagel 21 is scattered in respectively in the gas system oil that contains corresponding amount Span-60, it is 15g that the preparation massfraction is respectively 0.2% and 2.0% organic rustic system oil dispersion, simultaneously organophilic clay A is scattered in the gas system oil, the preparation massfraction is that 3.0% organophilic clay A gas system oil dispersion is 15g.For 0.2wt%Dynagel 21 gas system oil dispersions system, experimental group is added with the Span-60 of 1 times of organophilic clay quality; And for 2.0wt%Dynagel 21 gas system oil dispersions system, experimental group is added the Span-60 of organic soil property amount 30%.With two kinds of mixtures respectively in 80 ℃ of water-baths with walk around fast induction stirring 4 hours of per minute 300, after it is transferred in the 25ml colorimetric cylinder, and under this temperature, leave standstill, transfer finishes, and when leaving standstill 6 hours under this temperature, Taking Pictures recording, after it be transferred under the room temperature leave standstill, leave standstill 12 hours Taking Pictures recordings, photo as shown in Figure 4.In the photo dispersion system that does not add any additives, i.e. control group.This moment, dispersion temperature was 80 ℃, and when dispersion temperature is 50 ℃, its effect the same quite (Span-60 dissolves under this temperature), further within the specific limits elevated temperature, its effect is all close.
By picture as can be seen, under comparatively high temps (generally greater than 50 ℃, and less than 200 ℃) Span-60 improves the organophilic clay dispersiveness and system colloidal stability effect is suitable with Span-80 under the room temperature, so can be used for deep-well mud with the prepared organophilic clay of this method, utilize shaft bottom self high temperature to improve the dispersiveness and stability of organophilic clay.
Claims (2)
1. a method of improving the organophilic clay dispersiveness is characterized in that, may further comprise the steps:
(1) get organophilic clay, organic solvent and oil soluble nonionic surface active agent, wherein the organophilic clay quality is the 0.2%--5% of three's total mass, and the quality of oil soluble nonionic surface active agent is the 10%--200% of organophilic clay quality;
(2) organophilic clay, organic solvent and oil soluble nonionic surface active agent three are mixed with random order, make mixed solution, this mixed solution is stirred under room temperature it is uniformly dispersed; And under the room temperature being solid-state oil soluble nonionic surface active agent, when stirring after organophilic clay and organic solvent are mixed, need carry out under this solid oil dissolubility nonionic surface active agent dissolved temperature guaranteeing; After being uniformly dispersed it, stirring promptly obtains organophilic clay colloidal dispersion system better dispersed and that stability is higher.
2. the method for improving the organophilic clay dispersiveness according to claim 1, it is characterized in that, be down solid oil soluble nonionic surface active agent for normal temperature, be with its with the organophilic clay room temperature under make mixture after the mixed grinding pulverizing, again this mixture is scattered in the organic solvent.
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| CN 201010254510 CN101948116B (en) | 2010-08-16 | 2010-08-16 | Method for improving dispersibility of organic soil |
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| CN 201010254510 CN101948116B (en) | 2010-08-16 | 2010-08-16 | Method for improving dispersibility of organic soil |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103540299A (en) * | 2012-07-12 | 2014-01-29 | 中国石油化工股份有限公司 | Drilling fluid for low-pressure water-sensitive stratum |
| CN105086964A (en) * | 2014-05-12 | 2015-11-25 | 中国石油化工集团公司 | Low-toxicity oil base microbubble drilling fluid for protecting hydrocarbon reservoir |
| CN106118618A (en) * | 2016-07-07 | 2016-11-16 | 中国海洋石油总公司 | Thickening organic solvent and application and preparation method and oil base drilling fluid |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1008725B (en) * | 1985-08-13 | 1990-07-11 | Ecc国际有限公司 | Improve the method for dispersibility of organoclays |
| CN101531373A (en) * | 2009-04-13 | 2009-09-16 | 四川大学 | Active organo montmorillonite and preparation method thereof |
| CN101624515A (en) * | 2009-08-05 | 2010-01-13 | 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 |
| CN101774598A (en) * | 2009-01-12 | 2010-07-14 | 中国科学院化学研究所 | Method for preparing modified clay of alkyl ammonium salt surfactant intercalation |
-
2010
- 2010-08-16 CN CN 201010254510 patent/CN101948116B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1008725B (en) * | 1985-08-13 | 1990-07-11 | Ecc国际有限公司 | Improve the method for dispersibility of organoclays |
| CN101774598A (en) * | 2009-01-12 | 2010-07-14 | 中国科学院化学研究所 | Method for preparing modified clay of alkyl ammonium salt surfactant intercalation |
| CN101531373A (en) * | 2009-04-13 | 2009-09-16 | 四川大学 | Active organo montmorillonite and preparation method thereof |
| CN101624515A (en) * | 2009-08-05 | 2010-01-13 | 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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103540299A (en) * | 2012-07-12 | 2014-01-29 | 中国石油化工股份有限公司 | Drilling fluid for low-pressure water-sensitive stratum |
| CN103540299B (en) * | 2012-07-12 | 2017-04-12 | 中国石油化工股份有限公司 | Drilling fluid for low-pressure water-sensitive stratum |
| CN105086964A (en) * | 2014-05-12 | 2015-11-25 | 中国石油化工集团公司 | Low-toxicity oil base microbubble drilling fluid for protecting hydrocarbon reservoir |
| CN106118618A (en) * | 2016-07-07 | 2016-11-16 | 中国海洋石油总公司 | Thickening organic solvent and application and preparation method and oil base drilling fluid |
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