US2684947A - Noncaking silicofujoride- - Google Patents
Noncaking silicofujoride- Download PDFInfo
- Publication number
- US2684947A US2684947A US2684947DA US2684947A US 2684947 A US2684947 A US 2684947A US 2684947D A US2684947D A US 2684947DA US 2684947 A US2684947 A US 2684947A
- Authority
- US
- United States
- Prior art keywords
- magnesium oxide
- magnesium
- ammonium
- silicofluoride
- caking
- 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.)
- Expired - Lifetime
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 23
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 22
- 239000000395 magnesium oxide Substances 0.000 claims description 21
- 239000000203 mixture Substances 0.000 claims description 18
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 8
- 239000011777 magnesium Substances 0.000 claims description 8
- 229910052749 magnesium Inorganic materials 0.000 claims description 8
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 5
- 239000011701 zinc Substances 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 description 12
- 235000001055 magnesium Nutrition 0.000 description 7
- 229940091250 magnesium supplement Drugs 0.000 description 7
- 229940070337 ammonium silicofluoride Drugs 0.000 description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- MOMKYJPSVWEWPM-UHFFFAOYSA-N 4-(chloromethyl)-2-(4-methylphenyl)-1,3-thiazole Chemical compound C1=CC(C)=CC=C1C1=NC(CCl)=CS1 MOMKYJPSVWEWPM-UHFFFAOYSA-N 0.000 description 1
- IBZGBXXTIGCACK-UHFFFAOYSA-N 6,7,9,11-tetrahydroxy-9-(2-hydroxyacetyl)-4-methoxy-8,10-dihydro-7h-tetracene-5,12-dione Chemical class C1C(O)(C(=O)CO)CC(O)C2=C1C(O)=C1C(=O)C(C=CC=C3OC)=C3C(=O)C1=C2O IBZGBXXTIGCACK-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 235000010216 calcium carbonate Nutrition 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 235000012255 calcium oxide Nutrition 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 235000014380 magnesium carbonate Nutrition 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 235000011147 magnesium chloride Nutrition 0.000 description 1
- 229960005336 magnesium citrate Drugs 0.000 description 1
- 235000002538 magnesium citrate Nutrition 0.000 description 1
- 239000004337 magnesium citrate Substances 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 239000000391 magnesium silicate Substances 0.000 description 1
- 229910052919 magnesium silicate Inorganic materials 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 235000019983 sodium metaphosphate Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 235000012222 talc Nutrition 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- PLSARIKBYIPYPF-UHFFFAOYSA-H trimagnesium dicitrate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O PLSARIKBYIPYPF-UHFFFAOYSA-H 0.000 description 1
- MLIKYFGFHUYZAL-UHFFFAOYSA-K trisodium;hydron;phosphonato phosphate Chemical compound [Na+].[Na+].[Na+].OP([O-])(=O)OP([O-])([O-])=O MLIKYFGFHUYZAL-UHFFFAOYSA-K 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 235000014692 zinc oxide Nutrition 0.000 description 1
Definitions
- The'present invention relates to powdered silicofluori-de compositions which do not form hard cakeswhen' stored under adverse conditions of temperature and humidity.
- magnesium oxide The quantity of magnesium oxide required to prevent caking will be dependent upon the particular siliconuoride salt in which it is incorporated as well as the physi-- cal characteristics of the magnesium oxide itself, but in general an amount in the range of 0.3-1.0%, by weight, is satisfactory. It will be recognized that concentrations less than 0.3% can be used where storage conditions are not particularly adverse and concentrations greater than 1.0% may also be employed. in particular, it is sometimes necessary to use magnesium oxide in amounts up to 2.0% or even more to er iectively prevent the caking of zinc silicofluoride salts.
- the magnesium oxide employed should preferably be of a light grade, such as extra light calcined magnesia, having a bulk density or 10 lbs. per cubic foot or less.
- Example 1 The caking tendency of ammonium silicofluoride was determined by placing 75 grams of the salt in a 3.5" I. D. Petri dish and storing it in a humidor that was maintained at 104 F. and 75% relative humidity. By the end of 4.8 hours, the ammonium silicofluoride had formed a hard cake. Experience has shown that this so-called accel- 2 erated Petri dish storage test correlates well with actual caking tendencies undernormal storage conditions.
- a second ammonium silicofluoride"composition was prepared by incorporating 0.3 by weight, magnesium oxide'inthe ammonium since-fluoride described immediately above.
- the magnesium oxide was a light grade 'having'abulk density of 7.4 lbs. per 'cubic it; This composition was also stored in' an open Petri dish at 195 and 75% relative humidity, but unlike the pure am inonium silicofluoride it did not form a calreeven after 18 days'storage.
- a mixture of silicofluoride salts comprising 40% of the ammonium salt and of the magnesium salt was subjected to the Petri dish storage test and formed a very hard cake after 2 days.
- 0.4%, by weight, of the magnesium oxide described in Example 1 was incorporated in the above described mixture, the resulting composition did not form a cake even after 18 days.
- Example 4 To illustrate the effect that the magnesium oxide concentration has upon caking tendency, the magnesium oxide described in Example 1 was incorporated into the mixed ammonium and magnesium silicofluoride described in Example 3 over a concentration range of 0.05-l.0-%, by weight.
- the results of the Petri dish storage test are set forth in the table below:
- magnesium oxide functions to prevent the caking of water-soluble silicofiuoride salts.
- magnesium citrate, trisodium pyrophosphate, magnesium chloride, magnesium sulfate, sodium metaphosphate, calcium carbonate, calcium oxide, magnesium carbonate, starch, talcum, magnesium silicate and zinc oxide were tested, but found to be ineffective in preventing the caking of water-soluble silicofluoride salts.
- a mixture consisting essentially of a compound selected from the group consisting of ammonium, magnesium and zinc silicofluorides and mixtures thereof and containing in intimate admixture therewith a minor proportion of magnesium oxide not in excess of 5%, but in an amount sumcient to prevent caking.
- a mixture consisting essentially of a cmpound selected from the group consisting of ammonium, magnesium and zinc silicofiuorides and mixtures thereof and containing in intimate admixture therewith a minor proportion of a light magnesium oxide not in excess of but in an amount sufficient to prevent caking, said magnesium oxide having a density of less than about pounds per cubic foot.
- a mixture consisting essentially of a compound selected from the group consisting of ammonium, magnesium and zinc silieofluorides and mixtures thereof and containing in intimate admixture therevvith approximately 0.31.0%, by Weight, of a light grade magnesium oxide having a density of less than about 10 pounds per cubic foot.
- a mixture consisting essentially of ammonium silicofluoride and containing in intimate admixture therewith approximately LLB-1.0%, by Weight, of a light grade magnesium oxide having a density of less than about 10 pounds per cubic foot.
- a mixture consisting essentially of magnesium silicofluoride and containing in intimate admixture therewith approximately 0.3-1.0%, by Weight, of a light grade magnesium oxide having a density of less than about 10 pounds per cubic foot.
- a mixture consisting essentially of a mixed water-soluble silicofluoride salt (approximately 40% ammonium silicofiuoride and 50% magnesium silicofiuoride) and containing in intimate admixture therewith approximately O.3-l.0%, by
Landscapes
- Silicates, Zeolites, And Molecular Sieves (AREA)
Description
Patented July 27, 1954 NONCAKING SILICOFLU OREDE.
COMPOSITIONS No Drawing. Aopplicatien ()ctober 21, 1952, Serial No. 316,071
l 6 Claims.
The'present invention relates to powdered silicofluori-de compositions which do not form hard cakeswhen' stored under adverse conditions of temperature and humidity.
Water-soluble silicofluoride salts, such as sodium, ammonium, magnesium, etc. salts, are widely used as laundry sours. Unfortunately, however, when the powdered silicofiuoride salts are stored under conditions of high temperature and/or high relative:humidity, they iorm..hard caires which area very diflicult.to breakiup. The difficulties 3.580012338C1 ..Wlth .thispronounced caking tendency are: obvious and,..in spiteoftthe diligent eiforts of ithose skilledxin. the .art, no' practical method has. heretofore. been discovered to. overcome condition.
Accordingly, it is an object of this invention to provide powdered water-soluble silieofluoride compositionswhich do not cake when stored under conditions'of-high' temperature and/or high relative humidity.
It has now been discovered that the caking tendency of the water-soluble silicofiuoride salts can be eliminated or very substantially reduced by incorporating therein a minor amount of magnesium oxide. The quantity of magnesium oxide required to prevent caking will be dependent upon the particular siliconuoride salt in which it is incorporated as well as the physi-- cal characteristics of the magnesium oxide itself, but in general an amount in the range of 0.3-1.0%, by weight, is satisfactory. It will be recognized that concentrations less than 0.3% can be used where storage conditions are not particularly adverse and concentrations greater than 1.0% may also be employed. in particular, it is sometimes necessary to use magnesium oxide in amounts up to 2.0% or even more to er iectively prevent the caking of zinc silicofluoride salts. The magnesium oxide employed should preferably be of a light grade, such as extra light calcined magnesia, having a bulk density or 10 lbs. per cubic foot or less.
The following examples are set forth to more clearly illustrate the principle and practice of this invention to those skilled in the art.
Example 1 The caking tendency of ammonium silicofluoride was determined by placing 75 grams of the salt in a 3.5" I. D. Petri dish and storing it in a humidor that was maintained at 104 F. and 75% relative humidity. By the end of 4.8 hours, the ammonium silicofluoride had formed a hard cake. Experience has shown that this so-called accel- 2 erated Petri dish storage test correlates well with actual caking tendencies undernormal storage conditions.
A second ammonium silicofluoride"composition was prepared by incorporating 0.3 by weight, magnesium oxide'inthe ammonium since-fluoride described immediately above. The magnesium oxide was a light grade 'having'abulk density of 7.4 lbs. per 'cubic it; This composition was also stored in' an open Petri dish at 195 and 75% relative humidity, but unlike the pure am inonium silicofluoride it did not form a calreeven after 18 days'storage.
Example .2
A mixture of silicofluoride salts comprising 40% of the ammonium salt and of the magnesium salt was subjected to the Petri dish storage test and formed a very hard cake after 2 days. When 0.4%, by weight, of the magnesium oxide described in Example 1 was incorporated in the above described mixture, the resulting composition did not form a cake even after 18 days.
Example 4 To illustrate the effect that the magnesium oxide concentration has upon caking tendency, the magnesium oxide described in Example 1 was incorporated into the mixed ammonium and magnesium silicofluoride described in Example 3 over a concentration range of 0.05-l.0-%, by weight. The results of the Petri dish storage test are set forth in the table below:
MgO Concentration,
Weight Percent Comment CakJeDd hard in less than 4 days.
. 0. Oaked hard in 5 days. Formed slight cake in about 18 days.
No caking in 18 days. No rigklng in 28 days.
It is tendency decreases with increasing magnesium oxide concentration and that excellent anticaking properties are obtained at less than 1% magnesium oxide content with the particular silicofluoride salt combination tested. Other data indicate that with the zinc silicofiuoride salt, the concentration of magnesium oxide should be in creased to approximately 12%.
The manner in which magnesium oxide functions to prevent the caking of water-soluble silicofiuoride salts is not presently known. However, it appears to be unique and specific in its action in that many chemically related compounds are not efiective in preventing such caking. For example, magnesium citrate, trisodium pyrophosphate, magnesium chloride, magnesium sulfate, sodium metaphosphate, calcium carbonate, calcium oxide, magnesium carbonate, starch, talcum, magnesium silicate and zinc oxide were tested, but found to be ineffective in preventing the caking of water-soluble silicofluoride salts.
What is claimed is:
1. A mixture consisting essentially of a compound selected from the group consisting of ammonium, magnesium and zinc silicofluorides and mixtures thereof and containing in intimate admixture therewith a minor proportion of magnesium oxide not in excess of 5%, but in an amount sumcient to prevent caking.
2. A mixture consisting essentially of a cmpound selected from the group consisting of ammonium, magnesium and zinc silicofiuorides and mixtures thereof and containing in intimate admixture therewith a minor proportion of a light magnesium oxide not in excess of but in an amount sufficient to prevent caking, said magnesium oxide having a density of less than about pounds per cubic foot.
3. A mixture consisting essentially of a compound selected from the group consisting of ammonium, magnesium and zinc silieofluorides and mixtures thereof and containing in intimate admixture therevvith approximately 0.31.0%, by Weight, of a light grade magnesium oxide having a density of less than about 10 pounds per cubic foot.
4. A mixture consisting essentially of ammonium silicofluoride and containing in intimate admixture therewith approximately LLB-1.0%, by Weight, of a light grade magnesium oxide having a density of less than about 10 pounds per cubic foot.
5. A mixture consisting essentially of magnesium silicofluoride and containing in intimate admixture therewith approximately 0.3-1.0%, by Weight, of a light grade magnesium oxide having a density of less than about 10 pounds per cubic foot.
6. A mixture consisting essentially of a mixed water-soluble silicofluoride salt (approximately 40% ammonium silicofiuoride and 50% magnesium silicofiuoride) and containing in intimate admixture therewith approximately O.3-l.0%, by
' Weight, of a light grade magnesium oxide having a density of less than about 10 pounds per cubic foot.
References Cited in the file of this patent UNITED STATES PATENTS OTHER REFERENCES J. W. Mellors A Comprehensive Treatise on Inorganic and Theoretical Chemistry, vol. 6, 1925 ed., page 948. Longmans, Green and 00., N. Y.
Claims (1)
- 3. A MIXTURE CONSISTING ESSENTIALLY OF A COMPOUND SELECTED FROM THE GROUP CONSISTING OF AMMONIUM, MAGNESIUM AND ZINC SILICOFLUORIDES AND MIXTURES THEREOF AND CONTAINING IN INTIMATE ADMIXTURE THEREWITH APPROXIMATELY 0.3-1.0%, BY WEIGHT, OF A LIGHT GRADE MAGNESIUM OXIDE HAVING A DENSITY OF LESS THAN ABOUT 10 POUNDS PER CUBIC FOOT.
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2684947A true US2684947A (en) | 1954-07-27 |
Family
ID=3440463
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US2684947D Expired - Lifetime US2684947A (en) | Noncaking silicofujoride- |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US2684947A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2861024A (en) * | 1957-11-12 | 1958-11-18 | Merck & Co Inc | Antibiotic dusts |
| US2946751A (en) * | 1956-03-26 | 1960-07-26 | Exxon Research Engineering Co | Continuous grease manufacture using coated free-flowing alkali metal saponifying agent |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US676548A (en) * | 1897-12-20 | 1901-06-18 | Julius A Reich | Fluorin compound and method of making same. |
| US1617708A (en) * | 1926-05-14 | 1927-02-15 | Gehauf Bernard | Method of making silicofluorides and products thereof |
| US2218031A (en) * | 1937-09-29 | 1940-10-15 | Du Pont | Preventing the caking of sodium perborate |
| US2426836A (en) * | 1947-09-02 | Noncaking laundry sour | ||
| US2460680A (en) * | 1949-02-01 | Laundry souring composition | ||
| US2589330A (en) * | 1952-03-18 | Anticaking agent for cleansing |
-
0
- US US2684947D patent/US2684947A/en not_active Expired - Lifetime
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2426836A (en) * | 1947-09-02 | Noncaking laundry sour | ||
| US2460680A (en) * | 1949-02-01 | Laundry souring composition | ||
| US2589330A (en) * | 1952-03-18 | Anticaking agent for cleansing | ||
| US676548A (en) * | 1897-12-20 | 1901-06-18 | Julius A Reich | Fluorin compound and method of making same. |
| US1617708A (en) * | 1926-05-14 | 1927-02-15 | Gehauf Bernard | Method of making silicofluorides and products thereof |
| US2218031A (en) * | 1937-09-29 | 1940-10-15 | Du Pont | Preventing the caking of sodium perborate |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2946751A (en) * | 1956-03-26 | 1960-07-26 | Exxon Research Engineering Co | Continuous grease manufacture using coated free-flowing alkali metal saponifying agent |
| US2861024A (en) * | 1957-11-12 | 1958-11-18 | Merck & Co Inc | Antibiotic dusts |
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