US3630928A - Particles containing mixtures of polyphosphates and silicates - Google Patents
Particles containing mixtures of polyphosphates and silicates Download PDFInfo
- Publication number
- US3630928A US3630928A US696114A US3630928DA US3630928A US 3630928 A US3630928 A US 3630928A US 696114 A US696114 A US 696114A US 3630928D A US3630928D A US 3630928DA US 3630928 A US3630928 A US 3630928A
- Authority
- US
- United States
- Prior art keywords
- silicate
- sodium tripolyphosphate
- mixture
- product
- solution
- 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
Links
- 239000000203 mixture Substances 0.000 title abstract description 28
- 239000002245 particle Substances 0.000 title abstract description 15
- 229920000388 Polyphosphate Polymers 0.000 title description 8
- 239000001205 polyphosphate Substances 0.000 title description 8
- 235000011176 polyphosphates Nutrition 0.000 title description 8
- 150000004760 silicates Chemical class 0.000 title description 3
- 235000019832 sodium triphosphate Nutrition 0.000 abstract description 37
- 239000008187 granular material Substances 0.000 abstract description 12
- 239000007864 aqueous solution Substances 0.000 abstract description 4
- 229910052910 alkali metal silicate Inorganic materials 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 3
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 31
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 30
- 239000000047 product Substances 0.000 description 29
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 13
- 239000004115 Sodium Silicate Substances 0.000 description 12
- 229910052911 sodium silicate Inorganic materials 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 239000003599 detergent Substances 0.000 description 9
- 239000004615 ingredient Substances 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 229920003023 plastic Polymers 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- 239000000080 wetting agent Substances 0.000 description 5
- 238000009472 formulation Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- DUIOKRXOKLLURE-UHFFFAOYSA-N 2-octylphenol Polymers CCCCCCCCC1=CC=CC=C1O DUIOKRXOKLLURE-UHFFFAOYSA-N 0.000 description 2
- 229920000426 Microplastic Polymers 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000013504 Triton X-100 Substances 0.000 description 2
- 229920004890 Triton X-100 Polymers 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- -1 isooctyl phenyl Chemical group 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- GPRLSGONYQIRFK-MNYXATJNSA-N triton Chemical compound [3H+] GPRLSGONYQIRFK-MNYXATJNSA-N 0.000 description 2
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 1
- 239000004606 Fillers/Extenders Substances 0.000 description 1
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 150000005215 alkyl ethers Chemical class 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000007973 cyanuric acids Chemical class 0.000 description 1
- 230000010006 flight Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 239000012254 powdered material Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D11/00—Special methods for preparing compositions containing mixtures of detergents
- C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
-
- 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
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/12—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic in rotating drums
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/02—Inorganic compounds
- C11D7/04—Water-soluble compounds
- C11D7/10—Salts
- C11D7/14—Silicates
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/02—Inorganic compounds
- C11D7/04—Water-soluble compounds
- C11D7/10—Salts
- C11D7/16—Phosphates including polyphosphates
Definitions
- the invention relates to producing strong, stable particles that contain a mixture of a polyphosphate and a silicate.
- an alkali metal silicate normallyuodiumnsih- Eate is iriEbTfi'dr'at'edTiitb
- Thedetergentjprmulatign... ""Regrettablyflhe "niixturebf sodium tripolyphosphate and a silicate in a dry-mixed, detergent formulation results in serious problems. These ingredients cake together into hard agglomerates that are difficult to pour and handle and which :cause undesired segregation of some components of the formulation.
- One solution to the caking problem is set ⁇ orth in U.S. Patent 2,909,490 issued to Max Metziger on Oct.
- This patented duplex mixture has certain drawbacks. Initially, it can only be formed with the less alkaline silicates, i.e., SiO /Na; weight ratios of 3.22:1 to 2.40: 1. Further, when high silica to polyphdsphate mole ratios, e.g., at least 1:1, are desired in the mixture for optimum corrosion inhibition, only the less alkaline (Slog/N830 of 3.22:1) silicate can be employed to obtain the patentees duplex product.
- It is a further object of the present invention to produce strong, stable particles that contain a mixture of a silicate and sodium tripolyphosphate in which the silicate has an SiO /-Na O weight ratio of below about 2.40:1.
- powdered sodium tripolyphosphate is used as one of the feed reactant. If the sodium tripolyphosphate is not in powdered form, it should be ground by conventional means so that substantially all of the polyphosphate passes through a 40 mesh screen with at least about being --80 mesh.
- the sodium tripolyphosphate is then placed in an agitated reaction chamber such as a ribbon blender or rotating drum and maintained in a state of constant agitation.
- the silicate solution should have an SiO;/Na,O weight ratio of below 2.40:1 and preferably 2.0:1.
- An especially useful sodium silicate solution is the Philadelphia. Quartz Company product D -brand silicate which contains 14.7% N330; 29.4% SiO,; and 55.9% H 0.-
- the silicate solution is dispersed into the bed of sodium tripolyphosphate, preferably through spray nozzles or other distributing means. In many cases it is preferred to added up to about 10% by weight of water to the D -brand silicate solution as received in order to decrease its viscosity and permit more easy distribution of the sodium silicate solution on the bed of polyphosphate.
- ambient temperatures are preferred during this mixing process although higher temperatures can be employed, provided material amounts of water in the silicate solution are not evaporated off.
- the silica 'ol hosphate the mole ratio of SiO, to tripolyphosp assure 1:1.
- the mixture becomes sticky and agglomerates of the granules is then increased in a heated chamber so that the granules reach a temperature of from to C. during which they lose moisture.
- the granules are maintained at this temperature until they are dry appearing. Thereafter, they are ground, if necessary, so that they are chiefly in the 8 to +50 mesh size and recovered as product. Any powdered product less than $0 mesh can be recycled to the reaction chamber by mixing it with additional, powdered polyphosphate before the addition of more silicate solution.
- a wetting agent i.e., a surfactant
- Suitable wetting agents include lower alkyl ethers of polyoxyethylated octyl phenols, such as those sold under the Triton CF trade name, for example Triton CF-54 which is the butylether of polyoxyethylated octyl phenol; and Triton X-100 which is the isooctyl phenyl polyethoxyethanol.
- a sodium silicate solution such as D -brand silicate which contains about 55% water can be used as received from the manufacturer and added directly to the sodium tripolyphosphate. However, in many cases it is desired to add water to the silicate solution until the H content of the solution reaches about 60% by weight. The added water lowers the viscosity of the silicate solution and permits it to be more readily dispersed throughout the polyphosphate. It should be added, however, that the addition of larger amounts of water is undesirable because the resulting mixture of sodium tripolyphosphate and aqueous silicate does not yield the proper degree of tackiness necessary to obtain the desired soft, plastic, deformable granules.
- plastic, deformhable granules are necessary in the practice of the present invention to obtain, after drying, strong granules which have a desirably low density, e.g., about 0.7 to about 0.8 g./cc. which do not crumble on being dry mixed with other'ingredients in a blender.
- the base of the pipew hich extended into the mixer contained eight small holes about 2 inches apart through which the silicate solution could be finely distributed onto the tumbling bed of sodium tripolyphosphate.
- the entire silicate solution was added over a period of twenty minute's.
- the batch became sticky, and all of the powdered material agglomerated into irregular lumps whichwere tacky and plastic.
- These plastic lumps were dried at 65 C. until they were hard and were then crushed and screened. About 80% of the crushed particles were recovered as a 8 +50 mesh granular product having a bulk density of 0.85 g./cc., with about 20% being separated as 50 mesh fines.
- a sample of the granular product was used to make up an aqueous 1% solution and found to be completely free of insolubles, and further was found to have a pH of 10.7.
- the granular product contained 19.5% total moisture (on ignition) and had a mole ratio of SiO, to sodium tripolyphosphate of 1.23:1.
- a' sample was thoroguhly blended with other conventional detergent ingredients in a mechanical mixer and the granular product did not break down, nor did the bulk density increase.
- Example 2 The procedure of Example 1 was repeated except that only 20 pounds of powdered sodium tripolyphosphate was added to the mixer along with 5 pounds of the -50 mesh granular product of Example 1. Further, the amount of silicate solution added was reduced by 20%. The silicate solution was added at a slower rate and required 36 minutes to add the entire silicate solution. The resulting tacky lumps were again dried at 65 C. until hard, crushed and screened. About of the total batch was recovered as 8 +50 mesh granular product having a bulk density of 0.76 g./cc. A sample of the resulting product was used to make up an aqueous 1% solution and was found to contain no insolubles and to give a pH of 10.7. The product was found to contain 20.5% total moisture (on ignition) and to have a mole ratio of SiO, to sodium tripolyphosphate of 1.23:1. The resulting product was formed of hard particles that did not break down upon being mechanically blended with other detergent ingredients.
- Example 3 The procedure of Example 1 was repeated except that 30 pounds of powdered sodium tripolyphosphate was used having a screen size distribution as follows:
- EXAMPLE 4 Twenty pounds of powdered sodium tripolyphosphate having a particle size as set forth in Example 3 at a temperature of 75 C. was added to the rotary mixture described in Example 1, and 5 pounds of --50 mesh fines from the product of Example 3 were added. A mixture of 12.6 pounds of D -brand silicate solution, 0.39 pounds of water, and 0.52 pounds of Tergitol Min-Foam (Union Carbide Co. wetting agent, modified linear alcohol ethoxylate) were added to the tumbling bed of sodium tripolyphosphate over a period of 27 minutes. The resulting mixture was almost entirely in the form of a 4 +8 mesh plastic, sticky agglomerate. The product was dried at 65 C. until hard and then was crushed and screened. The greater portion of the product was separated as a 8 +50 mesh granular product which had a bulk density of 0.79
- Process for producing strong, stable particles containing a mixture of a silicate and sodium tripolyphosphate in the mole proportion of at least 1:1 which comprises adding an aqueous solution of a sodium silicate having an SiO /Na O weight ratio of about 2.0:1 or less to a bed of powdered, sodium tripolyphosphate until the Si to sodium tripolyphosphate mole ratio is at least 1:1 and a sticky mixture results from said addition, agitating References Cited UNITED STATES PATENTS 2,895,916 7/1959 Milenkevich et al 252-99 2,909,490 10/1959 Metziger 252- 3,154,496 10/1964 Roald 252-99 3,231,505 1/1966 Farrar et al 252-138 3,255,117 6/1966 Knapp et al 252-99 3,248,330 4/1966 Personalstein et a1 252-99 LEON D. ROSDOL, Primary Examiner D. L. ALBRECHT, Assistant Examiner US. Cl. '
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Inorganic Chemistry (AREA)
- Detergent Compositions (AREA)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US69611468A | 1968-01-08 | 1968-01-08 |
Publications (1)
Publication Number | Publication Date |
---|---|
US3630928A true US3630928A (en) | 1971-12-28 |
Family
ID=24795763
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US696114A Expired - Lifetime US3630928A (en) | 1968-01-08 | 1968-01-08 | Particles containing mixtures of polyphosphates and silicates |
Country Status (11)
Country | Link |
---|---|
US (1) | US3630928A (fi) |
BE (1) | BE725950A (fi) |
BR (1) | BR6905422D0 (fi) |
CH (1) | CH510110A (fi) |
DE (1) | DE1900781A1 (fi) |
ES (1) | ES362229A1 (fi) |
FR (1) | FR1603903A (fi) |
GB (1) | GB1206707A (fi) |
NL (1) | NL6900261A (fi) |
SE (1) | SE364983B (fi) |
ZA (1) | ZA687491B (fi) |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3888781A (en) * | 1972-09-05 | 1975-06-10 | Procter & Gamble | Process for preparing a granular automatic dishwashing detergent composition |
US3996399A (en) * | 1974-06-10 | 1976-12-07 | Societe Francaise des Silicates Speciauz "SIFRANCE" | Process for improving the stability and shaping of anhydrous sodium metasilicate, and the products, and compositions containing same |
US4077897A (en) * | 1976-02-13 | 1978-03-07 | The Procter & Gamble Company | Process for preparing detergent compositions |
US4169806A (en) * | 1978-08-09 | 1979-10-02 | The Procter & Gamble Company | Agglomeration process for making granular detergents |
US4182683A (en) * | 1976-05-17 | 1980-01-08 | Berk Gunter H | Process for the manufacture of a dishwashing detergent |
US4228025A (en) * | 1979-06-29 | 1980-10-14 | The Procter & Gamble Company | Agglomeration process for making granular detergents |
US4740327A (en) * | 1982-01-18 | 1988-04-26 | Colgate-Palmolive Company | Automatic dishwasher detergent compositions with chlorine bleach having thixotropic properties |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3038413C2 (de) * | 1980-10-10 | 1986-10-09 | Unilever N.V., Rotterdam | Alkalimetalltripolyphosphat/Alkalimetallsilikat-Cogranulate mit verbessertem Ausspülverhalten |
DE3624336A1 (de) * | 1986-07-18 | 1988-01-28 | Henkel Kgaa | Verfahren zur herstellung von rieselfaehigen alkalischen reinigungsmitteln durch kompaktierende granulation |
-
0
- ZA ZA687491D patent/ZA687491B/xx unknown
-
1968
- 1968-01-08 US US696114A patent/US3630928A/en not_active Expired - Lifetime
- 1968-11-21 GB GB55200/68A patent/GB1206707A/en not_active Expired
- 1968-12-20 FR FR1603903D patent/FR1603903A/fr not_active Expired
- 1968-12-23 BE BE725950D patent/BE725950A/xx unknown
-
1969
- 1969-01-07 NL NL6900261A patent/NL6900261A/xx unknown
- 1969-01-08 SE SE00202/69A patent/SE364983B/xx unknown
- 1969-01-08 DE DE19691900781 patent/DE1900781A1/de active Pending
- 1969-01-08 ES ES362229A patent/ES362229A1/es not_active Expired
- 1969-01-08 BR BR205422/69A patent/BR6905422D0/pt unknown
- 1969-01-08 CH CH17269A patent/CH510110A/de not_active IP Right Cessation
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3888781A (en) * | 1972-09-05 | 1975-06-10 | Procter & Gamble | Process for preparing a granular automatic dishwashing detergent composition |
US3996399A (en) * | 1974-06-10 | 1976-12-07 | Societe Francaise des Silicates Speciauz "SIFRANCE" | Process for improving the stability and shaping of anhydrous sodium metasilicate, and the products, and compositions containing same |
US4077897A (en) * | 1976-02-13 | 1978-03-07 | The Procter & Gamble Company | Process for preparing detergent compositions |
US4182683A (en) * | 1976-05-17 | 1980-01-08 | Berk Gunter H | Process for the manufacture of a dishwashing detergent |
US4169806A (en) * | 1978-08-09 | 1979-10-02 | The Procter & Gamble Company | Agglomeration process for making granular detergents |
US4228025A (en) * | 1979-06-29 | 1980-10-14 | The Procter & Gamble Company | Agglomeration process for making granular detergents |
US4740327A (en) * | 1982-01-18 | 1988-04-26 | Colgate-Palmolive Company | Automatic dishwasher detergent compositions with chlorine bleach having thixotropic properties |
Also Published As
Publication number | Publication date |
---|---|
DE1900781A1 (de) | 1969-09-11 |
ES362229A1 (es) | 1970-11-01 |
BE725950A (fi) | 1969-06-23 |
ZA687491B (fi) | |
FR1603903A (fi) | 1971-06-14 |
NL6900261A (fi) | 1969-07-10 |
BR6905422D0 (pt) | 1973-05-17 |
GB1206707A (en) | 1970-09-30 |
SE364983B (fi) | 1974-03-11 |
CH510110A (de) | 1971-07-15 |
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