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. '

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• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Organic Chemistry (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)

Publications (1)

Family

ID=24795763

Family Applications (1)

Country Status (11)

Cited By (7)

Families Citing this family (2)

• 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 CH CH17269A patent/CH510110A/de not_active IP Right Cessation
  • 1969-01-08 DE DE19691900781 patent/DE1900781A1/de active Pending
  • 1969-01-08 SE SE00202/69A patent/SE364983B/xx unknown
  • 1969-01-08 BR BR205422/69A patent/BR6905422D0/pt unknown
  • 1969-01-08 ES ES362229A patent/ES362229A1/es not_active Expired

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