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WO1998051422A1 - Microencapsulation de contaminants organiques dangereux dans une matrice du sol - Google Patents

Microencapsulation de contaminants organiques dangereux dans une matrice du sol Download PDF

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Publication number
WO1998051422A1
WO1998051422A1 PCT/MX1998/000017 MX9800017W WO9851422A1 WO 1998051422 A1 WO1998051422 A1 WO 1998051422A1 MX 9800017 W MX9800017 W MX 9800017W WO 9851422 A1 WO9851422 A1 WO 9851422A1
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WO
WIPO (PCT)
Prior art keywords
silicate
soil
solution
microencapsulation
hydrocarbon
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/MX1998/000017
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English (en)
Spanish (es)
Inventor
Thomas Kennedy Mcdowell
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ingenieria Ambiental Mexicana SA de CV
Original Assignee
Ingenieria Ambiental Mexicana SA de CV
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
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Application filed by Ingenieria Ambiental Mexicana SA de CV filed Critical Ingenieria Ambiental Mexicana SA de CV
Priority to AU72395/98A priority Critical patent/AU7239598A/en
Publication of WO1998051422A1 publication Critical patent/WO1998051422A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/32—Materials not provided for elsewhere for absorbing liquids to remove pollution, e.g. oil, gasoline, fat
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09C—RECLAMATION OF CONTAMINATED SOIL
    • B09C1/00—Reclamation of contaminated soil
    • B09C1/08—Reclamation of contaminated soil chemically

Definitions

  • the present invention relates to a chemical process for the microencapsulation of hazardous organic pollutants, such as hydrocarbons and very particularly to a method of producing the microencapsulating agents or compositions and a method for the use of the agents or compositions mentioned, for the soil and similar sanitation, contaminated with organic materials.
  • Surfactants and emulsifiers have been used in environmental sanitation either to increase the coefficient of biological degradation or to emulsify and remove contaminants from soil systems such as in a soil washing process. Surfactants and dispersants have also been widely used in the treatment of oil spill on water.
  • Silica and silicates have also been widely used for sanitation of pollution problems.
  • Silica in various forms generally as silica in the form of a very fine powder, has been used for the recovery or treatment of oil spilled on water by means of a simple oil absorption.
  • Silicates have been used in many solidification processes to improve the physical characteristics of solidification in the same way they are used in many procedures for the production of specialized cements. In general, most of these silicates related to solidification processes are for the solidification of contaminant residues with heavy metals and have little application in the treatment of materials with hydrocarbons.
  • Noonan and McDowell do not prevent the use of neutral or near neutral reagents, instead the procedure is entirely based on the acid-base reaction.
  • the examples shown by Noonan and McDowell essentially show that a 1: 1: 1 ratio of emulsifier: silicate: hydrocarbon is necessary for proper treatment.
  • a soil contaminated with 10% hydrocarbon would require a total of 20% chemical additives, based on the weight of the soil. In economic terms, this limits the usefulness of this procedure to materials with 1% contamination or less.
  • earth metals for example calcium
  • silicates in the cement industry
  • Piepho in US Patent No. 4,415,467, discloses a method of absorbing oily contaminants in wastewater using coagulant, bentonite clay, lime and calcium aluminosilicate. Piepho specifically states that the calcium aluminosilicate in its disclosure is intended only for pozzolanic reactions.
  • the development of the present invention is directed to a novel method of encapsulation of emulsifiable contaminants such as hydrocarbons found in industrial process floor systems.
  • the method uses a novel surfactant for the environmental industry, for the desorption and emulsification of the contaminant followed by the addition of a silicate solution.
  • the silicate solution in turn reacts with the alkaline earth portion of the surfactant to precipitate the silica in turn forming an encapsulating shell surrounding the desorbed and emulsified material.
  • silica can be precipitated from silicate solutions by acidification or neutralization of the silicate solution. It is also known that simple solutions of alkaline earth metal salts such as calcium chloride can catalyze the precipitation of silica from silicate solutions.
  • the present invention uses the previously mentioned method, the precipitation of silicate by means of the addition of a compound of an alkaline earth metal, however, in a unique method. Instead of using a simple salt of an alkaline earth metal, it has been found that several surfactants containing a functional group of an alkaline earth metal are also capable of catalysis of the silica from the silicate solution.
  • the present method first provides for the reaction of an acidic surfactant with an alkaline earth hydroxide or other salts taken from magnesium, calcium, strontium or barium or reaction of a surfactant capable of being combined with a salt of an alkaline earth metal.
  • the base surfactant for example only, can be anionic surfactants such as phosphate esters, sulfonates, sulfosuccinate, sulfosuccinamates or simple fatty acids such as lauric, oleic or palmitic acid.
  • the reaction of these two materials produces a neutral surfactant that has emulsifying properties as well as containing a functional group of an alkaline earth metal.
  • This reaction product or preferably a solution of the reacting product is added to the contaminated material containing an emulsifiable contaminant.
  • the reaction product solution and the contaminated soil are then intimately mixed to produce an emulsion of the emulsifiable contaminant.
  • a cover known as a mycelial formation.
  • the actual size of this mycelium depends on the effectiveness of the emulsifier, but is generally in the range of 10 microns to 100 microns in diameter.
  • the actual surfactant used in the reaction product and the amount of reaction product used to emulsify any particular material will depend on both the type of emulsifiable pollutant and the concentration of said contaminant in the soil or residual matrix as well as the physical characteristics. and chemicals from the host soil or residual material.
  • the amount of intimate mixing required and the type of mixing required will depend on both contamination and soil or type of residual matrix.
  • a solution of the silicate of a metal alkali is added to the mixture being mixed again.
  • Silica in turn forms one.
  • the size of this microencapsulated particles is one of the advantages and one of the differences of the present invention over the previously cited patent of Noonan and McDowell.
  • the average size of the resulting material was claimed to be 2 to 4 microns or less which counts for the large amounts of material required to effectively treat any contaminated material with more than 1% contamination.
  • a balloon weighing only a few grams can contain several hundred grams of water, the larger the size of the balloon, the more water it can hold.
  • the present invention can encapsulate almost one hundred times more hydrocarbon for an essentially equivalent product weight than the examples previously cited by Noonan and McDowell.
  • an object of the present invention is to provide a process and the materials required to produce a microencapsulation of certain environmental pollutants. Said process can be applied to a variety of contaminants in a variety of soil or mud matrices or residues to produce a microencapsulated material resistant to environmental degradation.
  • Another objective of this invention is to provide this microencapsulation through the use of the product of reaction of surfactants and earth metals such as calcium or magnesium, hereinafter referred to as “the catalyst solution” and then reacting said material with a silicate solution of a metal alkali, hereinafter referred to as the “encapsulating solution "to form a silica cover surrounding pollutants.
  • Figure 1 shows a graph of the life period of the microencapsulated material.
  • the method of the present invention involves the use of a catalyst solution; surfactant system with an alkaline earth metal, in a reaction with an encapsulating solution: silicate solution of a metal alkali to produce a system for microencapsulation of emulsifiable organic pollutants.
  • the method can be used for sanitation or treatment of soils contaminated with organic compounds such as hydrocarbons and more particularly soils contaminated with gasoline, diesel fuel, residual oils, crude oil and the like.
  • the method can also be used for the treatment of process residues such as tank sediments or sludges related to hydrocarbons from the oil refining industry or drilling sludges from oil production.
  • the surfactant used in the first part of the reaction with the alkaline earth metal is selected from the group of acidic surfactants, esters surfactants, di-ester surfactants or fatty acids This may be,. for example, an ester such as sodium sulfosuccinate coconut diethanolamide ester, an acidic surfactant such as dodecibencenesulfonic acid, a simple fatty acid such as lauric acid, a common intermediate surfactant such as lauryl sulfate or one of the many esters of acid phosphate.
  • an ester such as sodium sulfosuccinate coconut diethanolamide ester
  • an acidic surfactant such as dodecibencenesulfonic acid
  • a simple fatty acid such as lauric acid
  • a common intermediate surfactant such as lauryl sulfate or one of the many esters of acid phosphate.
  • the alkaline earth metal reactant is selected from group II of metals consisting of beryllium, magnesium, calcium, strontium and barium.
  • the cationic portion of the alkaline earth metal is alkaline, such as, for example, carbonate or hydroxide.
  • a non-ionic, acid-free phosphate surfactant such as Alkaphos QS, marketed by the Rhone Poulenc Division of Surfactants and Specialties, 150 grams of water were added by mixing this to form a clear solution.
  • a non-ionic, acid-free phosphate surfactant such as Alkaphos QS, marketed by the Rhone Poulenc Division of Surfactants and Specialties.
  • 19.5 grams of calcium hydroxide, Ca (OH) 2 was added with vigorous mixing for a period of two hours. The temperature was maintained at 60 ° C during mixing. At the end of mixing, the sample was allowed to cool vigorously for 30 minutes to solubilize any material that did not react. This was filtered for a second time to provide a final dry weight of approximately 92.6 grams of product.
  • the filter residue, the calcium salt of the non-ionic phosphate surfactant was an essentially white water-insoluble material with an alkaline pH of 9.64.
  • This reaction product could be dispersed within a water system through the use of additional surfactants as described below in the best intended composition.
  • composition A better composition intended for dispersion of this material has the following composition:
  • the pH of the best predicted composition above varies between 9.3 and 9.8, a slightly alkaline solution.
  • Another better intended method of the present invention uses Magnesium as the anion of the alkaline earth metal.
  • the preparation of the surfactant-magnesium agent reaction product can be carried out as follows: To 100 grams of dialkiphenoxy poly (oxyethylene) acid phosphate, 200 grams of water are added. This is mixed to form a clear solution and the temperature is raised to 70 ° C. To this solution, 16.7 grams of magnesium hydroxide, Mg (OH) 2, are added slowly over a period of 4 hours, with vigorous stirring, while maintaining the necessary temperature. The solution is allowed to cool, and the precipitate is filtered. The filtered precipitate is placed back in 300 grams of water, and vigorously stirred for 30 minutes to solubilize any unreacted material.
  • the magnesium salt of the cyalkylphenoxy poly (oxyethylene) acid phosphate was a waxy white solid material with an alkaline pH of 8.43. Similar to the calcium reaction product described above, the magnesium reaction product can be dispersed in water through the use of additional surfactants.
  • a better intended composition for the dispersion of the magnesium salt product of the reaction is as follows: Magnesium salt as reaction product 14.8 n- (1,2-dicarboxyethyl) -n-octadecylsulfosuccinamate Tetrasodium 9.2
  • the pH of the best predicted composition above varies between 8.1 and 8.8, less alkaline than the best predicted composition previously described, however it is still an alkaline solution.
  • compositions previously envisaged should be manufactured in heated containers, equipped with high mixing intensity, such as a Cowles Dissolver.
  • high mixing intensity such as a Cowles Dissolver.
  • the silicate solution that is used as the reagent with the now dispersed or solubilized surfactant catalyst solution with an alkaline earth metal is taken from the group of alkali metal silicates. They can be sodium or potassium silicates, metasilicates and orthosilicates. Commercially available silicates can be found in a wide range of silica-alkali ratios. For example, sodium silicate is commercially available in weight ratios of SIO2: Na2 ⁇ from 1: 1.60 or higher as l: 3.85. While silicates of all silica-alkali ratios may find applicability in the present invention, those silicates of lower alkalinity and higher ratios will result in a more acceptable final pH product for environmental uses.
  • the silicate solution can be modified to improve its effectiveness in the actual microencapsulation of hydrocarbon contaminants.
  • One such modification is the addition of a surfactant to reduce surface tension and improve the wetting of the silicate solution when added to a soil contaminated matrix.
  • Simple modifications to the silicate solution such as dilution with water for a real concentration of use, pH adjustment, addition of viscosity promoters or the use of different concentrations of surfactant or different surfactants are anticipated by the present relationship and They are determined by the actual physical and chemical characteristics of the residual material being treated.
  • a better composition intended for the manufacture of the silicate solution is as follows:
  • E1 sodium silicate used in the best expected composition above has the following specifications: Average weight ratio of SIO2.: Na2Ü 1.33, pH of a solution is 1% water weight / weight 10.55, total solids 33.4-
  • the manufacture of the above composition is a simple mixing operation, with the materials added and mixed in the order listed.
  • the best previously envisaged encapsulation solution composition provides a final product with a pH of about 10.2 by rapidly reacting with the alkaline catalyst solution previously described to precipitate the silica surrounding the emulsified hydrocarbon and providing an impermeable microencapsulation of the hydrocarbon.
  • results of this analysis on sand contaminated with diesel fuel show an average concentration of hydrocarbons before treatment of 18,640 mg / kg as diesel fuel.
  • Actual treatment of the sample contaminated with diesel fuel required a horizontal mixer such as a propeller belt mixer or the like.
  • the reaction between the catalyst solution and the solution Encapsulant is very fast, so to ensure a distribution of the reaction, all the material that is being treated or substantially all the material that is being treated has to be exposed to the microencapsulation solution.
  • the most effective method to ensure that substantially all of the material is in contact with the encapsulating solution is the spray application through the surface, while mixing, at a high speed in a horizontal mixer to produce material movement. from the bottom to the top.
  • the actual mixing speed will depend on the type of horizontal mixer used and the size of the mixing blades or blades, however sufficient mixing speed is needed to effectively break or reduce the size of large lumps of soil or residue to a mass of relatively homogeneous particles that are on average less than 0.5 inches in diameter.
  • the mixing speed must be sufficient to stir the entire mass of solids contained within the mixer in less than one minute.
  • a 500 gram aliquot of sand contaminated with diesel fuel was placed in the mixer and this material was mixed for two minutes for homogenization.
  • 2.0 ml of a sample of the first best expected composition of the catalyst solution was diluted to 10 ml with water.
  • the mixer was started and the diluted catalyst solution was atomized on the surface of the material for a period of one minute. After an additional two minutes of mixing to ensure the contact of the catalyst solution with all the material contaminated with diesel fuel.
  • 3.0 ml of a sample of the best expected composition of the encapsulating solution was diluted to 10 ml with water.
  • the mixer was started again and the encapsulating solution was slowly atomized on the surface of the material for a period of 4 minutes Mixing for two. additional minutes to ensure complete contact of all the encapsulating solution with the entire solution 'catalyst.
  • Two composite samples were taken for analysis for the determination of residual diesel fuel, the remaining treated material being cooled.
  • the results of the analysis for the determination of diesel fuel showed an average content of 832 mg / kg after treatment, a reduction of 95.5% based on the initial content of 18,640 mg / kg of diesel fuel in the contaminated material.
  • the material after the treatment had an appearance essentially identical to the material before the treatment, that is, it was essentially a sandy material without a detectable odor of hydrocarbon.
  • silt soil was contaminated with SAE 30 commercial engine oil.
  • a 1 kg sample of silt-free hydrocarbon soil was placed in a Hobart mixer and mixed for 10 minutes to remove lumps Next, 40 grams of motor oil were slowly added while the mixer was still running, mixing this material for 30 minutes. Two composite samples were taken to determine the level of contamination, cooling the remaining material. Analysis of the samples for the determination of hydrocarbons in the engine oil range showed an average concentration before treatment of 34,120 mg / kg.
  • a 500 gram sample of the above contaminated material was placed in the laboratory mixer, helix tape type and the mixer was run for two minutes for homogenization. 3 ml were diluted. of the second best expected composition of the catalyst solution at 10 ml with water. This solution was slowly atomized for a period of 4 minutes on the surface of the contaminated material while the. Mixer continued mixing. This material was mixed for an additional three minutes to ensure complete contact. They were diluted 6 ml. of the best encapsulant solution planned at 15 mi. with water. This solution was slowly atomized over a period of five minutes on the surface of the material. The final treated material was mixed for another 4 minutes to ensure complete contact of the encapsulant solution with the entire catalyst solution. Two complete samples of the treated material were taken for analysis, the remaining material was refrigerated.
  • the analysis of the treated material showed an average concentration of 1,684 mg / kg of hydrocarbon in the engine oil range. Meaning a reduction of 95.06% in the level of hydrocarbon from the initial untreated sample.
  • the treated material did not change in appearance and after treatment it was still a friable silt soil, with no odor or perceptible hydrocarbon color. This is one of the obvious advantages of the present microencapsulation over the other normal encapsulation processes such as solidification or stabilization, since the physical characteristics are not changed thus allowing the treated material to be used for multiple purposes.
  • a 500 gram sample of the clay soil contaminated with the crude oil was placed in a horizontal laboratory mixer and this material was mixed for 5 minutes to ensure homogenization of the sample.
  • 7 ml were diluted.
  • of the first catalyst solution composition provided at 20 ml with water. With the mixer in operation, this catalyst solution was atomized for a period of 6 minutes on the surface of the contaminated material, followed by an additional 4 minutes of mixing to ensure complete contact.
  • 14 ml were diluted. of the best silicate solution provided with 14 ml of water and 0.10 grams of dioctyl sulphosuccinate sodium were added, mixing this until a clear solution was obtained.
  • This diluted encapsulant solution was slowly sprayed onto the surface of the contaminated material for a period of 6 minutes, while the mixer was in operation. The treated material was mixed for another 6 minutes to ensure complete contact. Two samples of treated material were taken for analysis while the remaining material was refrigerated. - The results of these analyzes showed an average hydrocarbon content calculated as 1,334 mg / kg oil in the treated material. Even in these most difficult conditions, the process revealed evidenced a 97.9% reduction in pollution levels. The material treated by the revealed process was brown in color with a consistency similar to the soil soil without a detectable odor of hydrocarbon, compared to the sample of untreated contaminated material that was dark black, with a sticky consistency with a tendency to form lumps and with a distinctive odor of hydrocarbon.
  • the revealed process is a microencapsulation process and not only an absorption process
  • the following longevity evaluation of the materials treated by the revealed process was performed. Absorption as well as most solidification and stabilization processes are considered as temporary solutions in which contaminants will eventually leach into the environment over a period of months to several hundred years. Rather than demonstrating an improvement in the order of magnitude, it is clearly demonstrated that this is a real microencapsulation with the contaminant completely encapsulated within the silica and that the revealed microencapsulation method results in a permanent treatment process.
  • Example 1 For the following experiments, the sample of the contaminated sand with diesel fuel prepared and treated in Example 1 was used. These analyzes were based on the US EPA Method 1320, Multiple Extraction Procedure (PEM). This test method is designed to simulate the leaching that a material would carry if it were exposed to repeated acid precipitation events. This test method consists of 10 sequential leaching events of 24 hours each, using the same sample throughout the process. In other words, the sample is subject to leaching by agitation in an acidified environment for a total of 240 hours. The results of each extraction are shown in table No. one.
  • PEM Multiple Extraction Procedure
  • the present invention provides an economical, effective and safe method of permanent microencapsulation of emulsifiable contaminants. It is also evident from the best described compositions described that these materials are safe to handle and use and are more acceptable environmental than the highly acidic or alkaline materials of the aforementioned Noonan and McDowell patent or the highly alkaline pozzolanic materials of the stabilization processes or solidification.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Public Health (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Soil Sciences (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

L'invention concerne un nouveau procédé d'encapsulation de contaminants emulsifiables tels que les hydrocarbures rencontrés dans des systèmes édaphiques ou des résidus industriels. Le procédé utilise un agent tensioactif nouveau permettant la désabsorption et l'émulsification du contaminant auquel on ajoute une solution de silicate. La fraction alcalinoterreuse de l'agent tensioactif catalyse ou provoque la précipitation du silicate sous forme de silice et la formation immédiate d'un revêtement d'encapsulation autour du matériau désabsorbé et émulsionné. Ce procédé d'encapsulation ne réagit qu'avec le contaminant dans une matrice de sol contaminé et non pas avec le sol hôte ou une matrice du résidu. Le revêtement d'encapsulation présentera un diamètre ou une dimension directement lié(e) à l'efficacité du procédé d'émulsification et à la dimension du mycélium obtenu à partir de l'émulsifiant et du contaminant. En général, le diamètre du revêtement d'encapsulation sera d'environ 200 microns. Cette microencapsulation, uniquement pour le contaminant, produit un sol traité présentant essentiellement les mêmes caractéristiques physiques que celles du sol non traité.
PCT/MX1998/000017 1997-05-14 1998-05-14 Microencapsulation de contaminants organiques dangereux dans une matrice du sol Ceased WO1998051422A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU72395/98A AU7239598A (en) 1997-05-14 1998-05-14 Microencapsulation of dangerous organic contaminants into a soil matrix

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
MX973607 1997-05-14
MX9703607A MX9703607A (es) 1997-05-14 1997-05-14 Microencapsulacion de contaminantes organicos peligrosos dentro de una matriz de suelo.

Publications (1)

Publication Number Publication Date
WO1998051422A1 true WO1998051422A1 (fr) 1998-11-19

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WO (1) WO1998051422A1 (fr)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1991005026A1 (fr) * 1989-09-26 1991-04-18 Noonan William R Procede de traitement du petrole
WO1991005586A1 (fr) * 1989-10-10 1991-05-02 Wastech, Inc. Traitement de dechets dangereux
JPH04202365A (ja) * 1990-11-29 1992-07-23 Kanegafuchi Chem Ind Co Ltd 吸油性樹脂組成物及び該組成物を用いた油の回収方法
WO1994020421A1 (fr) * 1993-03-02 1994-09-15 Institut National De La Recherche Scientifique Polymeres a base de silicone comme agents de traitement de fuites accidentelles de liquides

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1991005026A1 (fr) * 1989-09-26 1991-04-18 Noonan William R Procede de traitement du petrole
WO1991005586A1 (fr) * 1989-10-10 1991-05-02 Wastech, Inc. Traitement de dechets dangereux
JPH04202365A (ja) * 1990-11-29 1992-07-23 Kanegafuchi Chem Ind Co Ltd 吸油性樹脂組成物及び該組成物を用いた油の回収方法
WO1994020421A1 (fr) * 1993-03-02 1994-09-15 Institut National De La Recherche Scientifique Polymeres a base de silicone comme agents de traitement de fuites accidentelles de liquides

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
DATABASE WPI Week 9236, Derwent World Patents Index; AN 1992-295529/36 *

Also Published As

Publication number Publication date
AU7239598A (en) 1998-12-08
MX9703607A (es) 1998-11-30

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