US20110159289A1 - Method of encapsulating particulate materials - Google Patents
Method of encapsulating particulate materials Download PDFInfo
- Publication number
- US20110159289A1 US20110159289A1 US12/930,070 US93007010A US2011159289A1 US 20110159289 A1 US20110159289 A1 US 20110159289A1 US 93007010 A US93007010 A US 93007010A US 2011159289 A1 US2011159289 A1 US 2011159289A1
- Authority
- US
- United States
- Prior art keywords
- water
- alkoxysilane
- encapsulated
- addition
- alkyl groups
- 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.)
- Abandoned
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/20—After-treatment of capsule walls, e.g. hardening
- B01J13/22—Coating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
- B01J13/18—In situ polymerisation with all reactants being present in the same phase
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
- Y10T428/2989—Microcapsule with solid core [includes liposome]
Definitions
- the invention disclosed and claimed herein deals with a method of encapsulating particulate materials that enables the particulate materials to be used in end use applications where they currently are not useful.
- Encapsulation of particulate and liquid materials has been known for a number of years. Such materials most usually encapsulated are fragrances, shampoos, cosmetics, colorants, catalysts, laundry detergents and soaps, personal care products, textiles, active ingredients, auto care products, and the like.
- the invention disclosed and claimed herein is a method of encapsulating particulate materials.
- the method comprises providing acidified water at least sufficient for hydrolyzing a predetermined amount of alkoxysilane.
- At least one type of particulate material is dispersed in the acidified water and there is slowly added a predetermined amount of alkoxysilane having the general formula:
- R is selected from the group consisting essentially of alkyl groups, substituted alkyl groups, aryl groups, substituted aryl groups, vinyl, allyl, and hydrogen, wherein the substituents are selected from the group consisting of fluorine, amino, hydroxy, and combinations thereof.
- the alkoxysilane hydrolyze and build a predetermined particle size and then the dispersion is optionally neutralized with a base.
- Subsequent steps include the work up of the product. It is best if larger amounts of water are used during the sol gel formation to prevent gelation of the sol gel, care being taken to minimize the amount of water as the excess water must be removed from the reaction mass at the end of the reaction. Any solids in the dispersion are dried. The dry solids can be ground to a fine powder for use.
- the encapsulation method of this invention does not rely on or use cross linkers, catalysts, surfactants and any other adjuvants that are expressly stated in the prior art to facilitate other means and methods of encapsulation of particulate material.
- the encapsulation reaction is run at or near room temperature and therefore, there is no need for any heating or cooling equipment.
- the reaction of this invention can be run in less than twenty-four hours and preferred is a reaction time of less than 10 hours, and a most preferred time is a reaction time of less than 3 hours.
- Adding the alkoxysilane in smaller portions will allow the sol gel to build to the appropriate particle size. This is a critical step in the method as a particle size too small will not encapsulate the particle and a particle size too large will cause premature precipitation and gelling. Defining the size of the particle can be determined by watching the reaction medium. Building of the particle can be observed and thus if the alkoxysilane is added too slowly, no particles other than the particle to be encapsulated will be visible while elements of gelling can be observed if the addition is too rapid. As long as one observes the reaction carefully, slight amounts of these two conditions can be remedied by adjustment of the addition rate either more or less.
- the condensation reaction can be represented by the following chemical equation:
- R is an alkyl group, a substituted alkyl group, an aryl group, a substituted aryl group, vinyl, allyl or hydrogen.
- Alkyl groups are those such as methyl, ethyl, propyl, amyl, etc.
- Aryl groups are selected from phenyl and tolyl. Substituted groups are selected from the group consisting of fluorine, amino groups, hydroxy groups, and combinations thereof.
- R′ is selected from hydrogen and alkyl groups of 1 to 4 carbon atoms.
- reaction mass is subjected to mild temperatures to remove the water and dry the sample, such as 50° C. or lower, although this temperature is not overly critical. One should take caution not to melt the encapsulated particle.
- the dried sample can be subjected to grinding to reduce the size of the particles.
- the size of the ground particle is dependent on the users end use, however, it has been found that grinding the encapsulated particles to the size of table salt is the most useful, producing a flowable product.
- Ksp solubility of the particulate solid in water
- Ksp solubility constant
- Potassium chloride was dissolve in acidified water. Thereafter, methyltrimethoxysilane was slowly added to allow for the hydrolysis of the alkoxy silane. The methyltrimethoxysilane was added in two equal portions to allow the sol gel to build to the appropriate particle size. After the reaction, the sol gel was neutralized to cause the precipitation of the matrix. The sample was oven dried at 45° C. overnight to remove the water followed by grinding the resulting metallic salt sol gel to a powder about the size of table salt.
- Table IV has additional reaction data demonstrating a reduction in the amount of water required for the sol-gel formation.
- Table V has additional data showing the double coating technique.
- the encapsulated material from experiment 1 of table V was used herein.
- the water and lithium chloride was allowed to equilibrate and a sample of the final product was added to this mixture.
- the product from experiment 1 of table IV was not soluble in the water solution.
- the material upon the addition of the first quantity of methyltrimethoxysilane, the material was able to go into solution.
- the second addition of methyl trimethoxysilane completed the final encapsulation product.
Abstract
A method of encapsulating particulate materials that enables the particulate materials to be used in end use applications where they currently are not useful. The method uses specific sol gel technology to encapsulate solid particles. In addition, the method can be used to multiple coat a coated particle.
Description
- This application claims priority from U.S. Provisional Patent Application U.S. Ser. No. 61/284,818 filed Dec. 24, 2009.
- The invention disclosed and claimed herein deals with a method of encapsulating particulate materials that enables the particulate materials to be used in end use applications where they currently are not useful.
- Encapsulation of particulate and liquid materials has been known for a number of years. Such materials most usually encapsulated are fragrances, shampoos, cosmetics, colorants, catalysts, laundry detergents and soaps, personal care products, textiles, active ingredients, auto care products, and the like.
- The invention disclosed and claimed herein is a method of encapsulating particulate materials. The method comprises providing acidified water at least sufficient for hydrolyzing a predetermined amount of alkoxysilane.
- Then, at least one type of particulate material is dispersed in the acidified water and there is slowly added a predetermined amount of alkoxysilane having the general formula:
-
RxSi(OR)4-x. - In this formula, R is selected from the group consisting essentially of alkyl groups, substituted alkyl groups, aryl groups, substituted aryl groups, vinyl, allyl, and hydrogen, wherein the substituents are selected from the group consisting of fluorine, amino, hydroxy, and combinations thereof.
- Thereafter, sufficient time is allowed for the alkoxysilane to hydrolyze and build a predetermined particle size and then the dispersion is optionally neutralized with a base.
- Subsequent steps include the work up of the product. It is best if larger amounts of water are used during the sol gel formation to prevent gelation of the sol gel, care being taken to minimize the amount of water as the excess water must be removed from the reaction mass at the end of the reaction. Any solids in the dispersion are dried. The dry solids can be ground to a fine powder for use.
- It should be noted at the outset, that the encapsulation method of this invention does not rely on or use cross linkers, catalysts, surfactants and any other adjuvants that are expressly stated in the prior art to facilitate other means and methods of encapsulation of particulate material.
- It should be further noted that the encapsulation reaction is run at or near room temperature and therefore, there is no need for any heating or cooling equipment.
- The reaction of this invention can be run in less than twenty-four hours and preferred is a reaction time of less than 10 hours, and a most preferred time is a reaction time of less than 3 hours.
- There is a requirement that the stoichiometry be observed between the amount of water in the reaction system and the amount of alkoxysilane in the system in order to carefully control the condensation reaction of the sol get that is being formed, to achieve the desired results.
- It is best if the alkoxysilane is added in small portions. Introducing the alkoxysilane too quickly will result in adverse results, i.e. gelation of the reaction mass.
- Adding the alkoxysilane in smaller portions will allow the sol gel to build to the appropriate particle size. This is a critical step in the method as a particle size too small will not encapsulate the particle and a particle size too large will cause premature precipitation and gelling. Defining the size of the particle can be determined by watching the reaction medium. Building of the particle can be observed and thus if the alkoxysilane is added too slowly, no particles other than the particle to be encapsulated will be visible while elements of gelling can be observed if the addition is too rapid. As long as one observes the reaction carefully, slight amounts of these two conditions can be remedied by adjustment of the addition rate either more or less.
- The condensation reaction can be represented by the following chemical equation:
-
RxSi(OR′)4-x+H2O+H+RxSi(OH)y+R′OH - wherein R is an alkyl group, a substituted alkyl group, an aryl group, a substituted aryl group, vinyl, allyl or hydrogen. Alkyl groups are those such as methyl, ethyl, propyl, amyl, etc. Aryl groups are selected from phenyl and tolyl. Substituted groups are selected from the group consisting of fluorine, amino groups, hydroxy groups, and combinations thereof. R′ is selected from hydrogen and alkyl groups of 1 to 4 carbon atoms.
- The reaction mass is subjected to mild temperatures to remove the water and dry the sample, such as 50° C. or lower, although this temperature is not overly critical. One should take caution not to melt the encapsulated particle.
- If one wishes to use the encapsulated particles in a end use formulation that uses water as part of the formulation, it may not be necessary to remove the water, or it may be necessary to remove some of the water but not dry out the sample completely.
- Thereafter, the dried sample can be subjected to grinding to reduce the size of the particles. The size of the ground particle is dependent on the users end use, however, it has been found that grinding the encapsulated particles to the size of table salt is the most useful, producing a flowable product.
- In an effort to minimize the amount of water used in the method, one must determine the solubility of the particulate solid in water (Ksp).
- It is also contemplated within the scope of this invention to perform an encapsulation on an encapsulated material of this invention to produce an added-to coating, much like producing an onion.
- Various metal salt solid particles were encapsulated by the method of this invention in the following manner by first determining their Ksp. (TABLE I)
-
TABLE I Metal Salt Ksp Potassium chloride (KCl) total solubility Copper Chloride (CuCl2) 70.6 gm/100 ml Lithium Chloride (LiCl) 76.9 gm/100 ml Barium Chloride (BaCl2) 31 gm/100 ml Zinc Chloride (ZnCl2) 81 gm/100 ml - It is necessary to determine the solubility constant (Ksp) of each of the metallic particles, as a stoichiometric amount of water is required to properly form the sol gel and the water is also necessary to dissociate the metallic salt in the mixture. Further, it is unknown what effect the free chloride from the dissociation of the metallic salt will have on the sol gel formation.
- Potassium chloride was dissolve in acidified water. Thereafter, methyltrimethoxysilane was slowly added to allow for the hydrolysis of the alkoxy silane. The methyltrimethoxysilane was added in two equal portions to allow the sol gel to build to the appropriate particle size. After the reaction, the sol gel was neutralized to cause the precipitation of the matrix. The sample was oven dried at 45° C. overnight to remove the water followed by grinding the resulting metallic salt sol gel to a powder about the size of table salt.
- To a 200 ml beaker, 35 grams of distilled water was added. To this water, 8 grams of lithium chloride was added with agitation. The temperature of the distilled water was measured at 23° C. During dissociation of the lithium chloride the temperature rose to 60 degrees, an exotherm of 37 degrees centigrade. After cooling back to 23 degrees, 2.3 grams of Dow Corning 6070 silane (methyltrimethoxysilane—Dow Corning Corporation, Midland, Mich.) was added drop wise and allowed to mix and hydrolyze. After continuous mixing for 60 minutes, 2.3 grams of Dow Corning 6070 silane was added drop wise and allowed to mix for 120 minutes. The resulting reaction product was filtered through filter paper to collect the encapsulated metal salt. This was dried for 16 hours at 45° C. resulting in a white crystalline powder. This powder was placed in a porcelain crucible and ground to a fine white powder about the size of table salt.
- Thereafter, each of the sol gel versions of the salts set forth in TABLE I were produced by virtually the same procedure. The results can be found in TABLE II.
-
TABLE II SAMPLE # 1 2 3 4 5 Solubility WATER 35 35 35 35 35 POTASSIUM 8 INFINITE COPPER 8 70.6/100 ML Lithium 8 76.9/100 ml Barium 8 31/100 ml Zinc 8 81/100 ml MTM1 2.3 2.3 2.3 2.3 2.3 MTM2 2.3 2.3 2.3 2.3 2.3 NaOH 1.2 1.2 0 1.2 0 Product 3 gms 3 gms 3 gms Water 15 gms 15 gms 15 gms Dry weight 0.46 g 0.61 g 0.26 g 1first addition of methyltrimethoxysilane 2second addition of methyltrimethoxysilane - Table III shows additional reactions.
-
TABLE III 1 2 3 4 5 WATER 175 175 175 175 175 K 40 CU 40 LI 40 BA 40 ZN 40 RXN1 ENDO EXO EXO ENDO EXO MTM 11.5 11.5 11.5 11.5 11.5 MTM 11.5 11.5 11.5 11.5 11.5 NaOH 6 6 6 6 6 Solution Color OPAQUE BLUE/ OPAQUE OPAQUE OPAQUE GREEN Exotherm 40 60 17 Temperature ° C. - Table IV has additional reaction data demonstrating a reduction in the amount of water required for the sol-gel formation.
-
TABLE IV 1 2 3 WATER 35 35 35 CU 28 Li 30.4 Ba 11.7 MTM 8.7 8.7 8.7 MTM 8.7 8.7 8.7 EXO TEMP. ° C. 60 40 17 SOLN pH 2 6 - Table V has additional data showing the double coating technique. The encapsulated material from experiment 1 of table V was used herein. The water and lithium chloride was allowed to equilibrate and a sample of the final product was added to this mixture. The product from experiment 1 of table IV was not soluble in the water solution. However, upon the addition of the first quantity of methyltrimethoxysilane, the material was able to go into solution. The second addition of methyl trimethoxysilane completed the final encapsulation product.
-
TABLE V 1 WATER 17.5 Li 15.7 MTM 4.35 MTM 4.35 SAMPLE 1 5.0 FROM TABLE V EXO TEMP ° C. 67 SOLUTION pH 4
Claims (7)
1. A method of encapsulating particulate materials, the method comprising:
a. providing acidified water at least sufficient for hydrolyzing a predetermined amount of alkoxysilane;
b. dispersing at least one type of particulate material in the acidified water;
c. slowly adding a predetermined amount of alkoxysilane having the general formula:
RxSi(OR′)4-x
RxSi(OR′)4-x
wherein R is selected from the group consisting essentially of alkyl groups, substituted alkyl groups, aryl groups, substituted aryl groups, vinyl, allyl, and hydrogen, wherein the substituents are selected from the group consisting of fluorine, amino, hydroxy, and combinations thereof, and wherein R′ is selected from hydrogen and alkyl groups of 1 to 4 carbon atoms;
d. allowing sufficient time for the alkoxysilane to hydrolyze and build a predetermined particle size.
2. The method as claimed in claim 1 wherein, in addition, there is a step e. in which the product of d. is neutralized with base.
3. The method as claimed in claim 1 wherein, in addition, the water is removed from the dispersion and any solids in the dispersion are dried.
4. The method as claimed in claim 2 wherein, in addition, the dry solids are ground to a fine powder.
5. An encapsulated particulate material prepared by the method of claim 1 .
6. A method as claimed in claim 1 in which an encapsulated material from the method of claim 1 is further subjected to the method of claim 1 to provide an additional coating of encapsulation material.
7. A method as claimed in claim 5 in which more than two coats are provided for an encapsulated material.
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US12/930,070 US20110159289A1 (en) | 2009-12-24 | 2010-12-24 | Method of encapsulating particulate materials |
US13/537,416 US8894409B1 (en) | 2007-11-10 | 2012-06-29 | Colored flame candle |
US15/080,698 US10543472B2 (en) | 2009-12-24 | 2016-03-25 | Method of encapsulating particulate material |
US16/713,613 US11045780B2 (en) | 2009-12-24 | 2019-12-13 | Method of encapsulating particulate material |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US28481809P | 2009-12-24 | 2009-12-24 | |
US12/930,070 US20110159289A1 (en) | 2009-12-24 | 2010-12-24 | Method of encapsulating particulate materials |
Related Child Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US13/537,416 Continuation-In-Part US8894409B1 (en) | 2007-11-10 | 2012-06-29 | Colored flame candle |
US15/080,698 Division US10543472B2 (en) | 2009-12-24 | 2016-03-25 | Method of encapsulating particulate material |
Publications (1)
Publication Number | Publication Date |
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US20110159289A1 true US20110159289A1 (en) | 2011-06-30 |
Family
ID=44187926
Family Applications (3)
Application Number | Title | Priority Date | Filing Date |
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US12/930,070 Abandoned US20110159289A1 (en) | 2007-11-10 | 2010-12-24 | Method of encapsulating particulate materials |
US15/080,698 Expired - Fee Related US10543472B2 (en) | 2009-12-24 | 2016-03-25 | Method of encapsulating particulate material |
US16/713,613 Active US11045780B2 (en) | 2009-12-24 | 2019-12-13 | Method of encapsulating particulate material |
Family Applications After (2)
Application Number | Title | Priority Date | Filing Date |
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US15/080,698 Expired - Fee Related US10543472B2 (en) | 2009-12-24 | 2016-03-25 | Method of encapsulating particulate material |
US16/713,613 Active US11045780B2 (en) | 2009-12-24 | 2019-12-13 | Method of encapsulating particulate material |
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US (3) | US20110159289A1 (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2014186454A1 (en) * | 2013-05-14 | 2014-11-20 | University Of Houston | Waterproof coating with nanoscopic/microscopic features |
US20160207021A1 (en) * | 2009-12-24 | 2016-07-21 | John D. Blizzard | Method of encapsulating particulate material |
US10266702B2 (en) | 2012-06-08 | 2019-04-23 | University Of Houston System | Self-cleaning coatings and methods for making same |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5989767A (en) * | 1998-12-15 | 1999-11-23 | Eastman Kodak Company | Carrier particles for electrostatographic developers |
US6337089B1 (en) * | 1998-02-06 | 2002-01-08 | Seiwa Kasei Company, Limited | Microcapsule containing core material and method for producing the same |
US6447907B1 (en) * | 1998-07-22 | 2002-09-10 | Fraunhofer-Gesellschaft Zur Forderung Der Angewandten Forschung E.V. | Spherical ionomer particles and production thereof |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20110159289A1 (en) * | 2009-12-24 | 2011-06-30 | Blizzard John D | Method of encapsulating particulate materials |
-
2010
- 2010-12-24 US US12/930,070 patent/US20110159289A1/en not_active Abandoned
-
2016
- 2016-03-25 US US15/080,698 patent/US10543472B2/en not_active Expired - Fee Related
-
2019
- 2019-12-13 US US16/713,613 patent/US11045780B2/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6337089B1 (en) * | 1998-02-06 | 2002-01-08 | Seiwa Kasei Company, Limited | Microcapsule containing core material and method for producing the same |
US6447907B1 (en) * | 1998-07-22 | 2002-09-10 | Fraunhofer-Gesellschaft Zur Forderung Der Angewandten Forschung E.V. | Spherical ionomer particles and production thereof |
US5989767A (en) * | 1998-12-15 | 1999-11-23 | Eastman Kodak Company | Carrier particles for electrostatographic developers |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20160207021A1 (en) * | 2009-12-24 | 2016-07-21 | John D. Blizzard | Method of encapsulating particulate material |
US10543472B2 (en) * | 2009-12-24 | 2020-01-28 | John D. Blizzard | Method of encapsulating particulate material |
US11045780B2 (en) * | 2009-12-24 | 2021-06-29 | Quadsil, Inc. | Method of encapsulating particulate material |
US10266702B2 (en) | 2012-06-08 | 2019-04-23 | University Of Houston System | Self-cleaning coatings and methods for making same |
WO2014186454A1 (en) * | 2013-05-14 | 2014-11-20 | University Of Houston | Waterproof coating with nanoscopic/microscopic features |
US9694388B2 (en) | 2013-05-14 | 2017-07-04 | University Of Houston System | Waterproof coating with nanoscopic/microscopic features and methods of making same |
Also Published As
Publication number | Publication date |
---|---|
US20200114331A1 (en) | 2020-04-16 |
US20160207021A1 (en) | 2016-07-21 |
US10543472B2 (en) | 2020-01-28 |
US11045780B2 (en) | 2021-06-29 |
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