US3423321A - Detergent processes - Google Patents

Detergent processes Download PDF

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Publication number
US3423321A
US3423321A US383479A US3423321DA US3423321A US 3423321 A US3423321 A US 3423321A US 383479 A US383479 A US 383479A US 3423321D A US3423321D A US 3423321DA US 3423321 A US3423321 A US 3423321A
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United States
Prior art keywords
slurry
sodium
detergent
sodium tripolyphosphate
processes
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Expired - Lifetime
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US383479A
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English (en)
Inventor
Kenneth J Shaver
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Monsanto Co
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Monsanto Co
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Publication date
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/16—Oxyacids of phosphorus; Salts thereof
    • C01B25/26—Phosphates
    • C01B25/38—Condensed phosphates
    • C01B25/40—Polyphosphates
    • C01B25/41—Polyphosphates of alkali metals
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/16—Oxyacids of phosphorus; Salts thereof
    • C01B25/26—Phosphates
    • C01B25/38—Condensed phosphates
    • C01B25/40—Polyphosphates
    • C01B25/41—Polyphosphates of alkali metals
    • C01B25/418—After-treatment
    • 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
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—Water-soluble compounds
    • C11D3/06—Phosphates, including polyphosphates
    • C11D3/062—Special methods concerning phosphates
    • 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
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/34—Organic compounds containing sulfur
    • C11D3/3418—Toluene -, xylene -, cumene -, benzene - or naphthalene sulfonates or sulfates

Definitions

  • This step of these processes has, for obvious reasons, been termed the foaming-hydration step.
  • enough free water has to be removed from the continuous aqueous phase of the slurry in these processes while the slurry is in the foamed condition to result in the loss by the slurry of its fluid properties.
  • the slurry is converted into a solid, porous product containing the desired sodium tripolyphosphate hexahydrate crystals and having a relatively low bulk density.
  • free water can be removed from the foamed slurry by evaporation due to the large amounts of heat evolved in the desired reaction, or by heating the foamed slurry externally; for example by infra-red lamps or hot tubes or pipes, or in a hot container; or by passing dry and/ or hot gases through the foamed slurry, as well as by many expedients which will be obvious to those skilled in the art in the light of the aforesaid disclosure.
  • the free water can be removed from the resulting lighter density solid, porous product by subjecting said product to an additional drying step in, for example, a rotary drying oven, a pan drying oven, or a fluidized bed dryer after it no longer demonstrates any fluid (slurry) properties.
  • the resulting precursor slurry is stirred for about minutes during which steam is passed through jacket 5 in order to increase the temperature of the precursor slurry to about 85 C.
  • the hot slurry is then pumped through lines 9 and 11 to a conventional vacuum type deaerator 13.
  • Deaerated slurry then passes through lines 15 and 17, through slurry pump 19, and line 21 to an efficient blender 31 (in this instance line 21 leads to the inlet port of a conventional centrifugal pump).
  • line 21 leads to the inlet port of a conventional centrifugal pump.
  • the slurry is monitored by means of a flow meter and a density meter 27.
  • a 50 weight percent aqueous solution of sodium hydroxide is pumped from the caustic storage tank 33 through line 35 and caustic metering pump 37 to heat exchanger 39 where its temperature is increased to about 70 C. From there it is pumped through line 41 into the same entry port of blender 31 as that into which the precursor slurry is being introduced.
  • the speed of caustic metering pump 37 is adjusted (depending upon the data from flow meter 25 and density meter 27) so that for every 100 parts by weight of precursor slurry there are introduced into blender 31, 24.5 parts by weight of NaOH.
  • the granulated product 51 is gently wiped by a series of rotating stainless steel wires 55 in order to break up any soft agglomerated lumps, and then transferred via ramp 57 to transfer belt 59. From there it is dropped onto a vibrating screen 61 to break up any remaining agglomerates. At this point the detergent product contains about 12 weight percent of free water and 13 weight percent of combined (hydration) water in the form of sodium tripolyphosphate hexahydrate. This product is then passed through a conventional fluidized bed dryer 63 to remove almost all of the free water, and from there into product storage bin 65.
  • the sodium tripolyphosphate hexahydrate crystals that are incorporated into the detergent slurries can be intermixed with the water, sodium trimetaphosphate, and other ingredients that may be utilized in the formulation of the desired detergent composition can apparently be incorporated into the slurry in practically any particular manner desired.
  • the hexahydrate crystals be incorporated into the slurry prior to the foaming-hydration step of the preferred detergent process described above (i.e., prior to that point in the process wherein a significant proportion of the sodium trimetaphosphate is converted to sodium tripolyphosphate hexahydrate while the slurry is in the foamed condition).
  • the hexahydrate crystals can be intermixed with any one of the slurry ingredients (or a combination of any of the slurry ingredients) that are to be blended into the slurry prior to the foaminghydration step. They can be added separately to the slurry, if desired, in a relatively pure form, or even initially in the form of anhydrous Form I or Form II sodium tripolyphosphate (in which case the tripolyphosphate is permitted to hydrate prior to the critical foaming-hydration step).
  • Still another way in which the desired sodium tripolyphosphate hexahydrate crystals can be incorporated into the detergent slurry in accordance with the improved processes of this invention is via the in situ conversion of some of the sodium trimetaphosphate in the slurry prior to the foaming-hydration step; for example, by adding less than the stoichiometric amount of strong base required to react with all of the sodium trimetaphosphate in the slurry sutficiently prior to the foaming-hydration step so that the desired amount of sodium tripolyphosphate crystals are formed in the slurry prior to the foaming-hydration step, or by permitting a certain amount of the trimetaphosphate reaction with strong base to occur before the light density foam is formed.
  • the desired results can be obtained when sodium tripolyphosphate crystals are intermixed into the slurry even when the slurry is in the foamed condition, provided that the trimetaphosphate conversion reaction in the foam has not yet been initiated.
  • sodium tripolyphosphate crystals for example, as little as 1 weight percent, or even less
  • sodium tripolyphosphate crystals can be utilized advantageously in the practice of the present invention, generally, for best results, from about 3 to about 50, and preferably from about 5 to about 15 weight percent, based upon the total amount of sodium trimetaphosphate used in the detergent slurries should be used.
  • size of these sodium tripolyphosphate crystals is not critical with respect to the successful practice of the present invention, it is preferred that they be small enough to pass through as mesh US. Standard screen.
  • Example I Into a conventional stainless steel mixing vessel which is fitted with a conventional paddle-type stirrer and jacketed so that either hot or cold water or steam can be used in the jacket, are charged 2,200 parts of water, 900 parts of sodium dodecylbenzene sulfonate, 600 parts of sodium lauryl sulfate, 1,000 parts of sodium sulfate, 2,940 parts of sodium trimetaphosphate, parts of powdered 100 mesh) sodium tripolyphosphate hexahydrate, 1,140 parts of sodium silicate (47% solids) having an SiO Na O ratio of 2.40 and 55 parts of detergent grade sodium carboxymethylcellulose. The resulting precursor slurry is stirred for about 10 minutes, during which time the temperature of the slurry is raised to 80 C. by circulating steam through the mixer jacket.
  • One hundred grams of the air-dried product of the particular detergent composition being tested are placed on a 100 mesh US. Standard screen, along with three oneinch rubber balls.
  • the sample and rubber balls are then shaken by means of a Ro-Tap sieve shaking machine for 30 minutes.
  • the amount of detergent product that has passed through the 100 mesh screen is weighed.
  • Most of the material which passes through the screen results from the breaking down of the original agglomerated detergent particles due to the pounding of the rubber balls.
  • the weight in grams of material which passes through the 100 mesh screen is given as percent dust in the tables.
  • the detergent pro ducts having relatively higher percent dust in the tables are more frangible (more easily broken down to produce irritating dust on handling, etc.) than are those that have relatively lower percent dust in the frangibility test. Note that the product in Table 1 which demonstrates the greater resistance to friation is that made according to the instant invention.
  • Table 1 illustrate both the significant improvement in particle size distribution and the frangibility of the detergent products that can result from use of the sodium tripolyphosphate hexahydrate crystals in accordance with this aspect of the present invention.
  • +10 mesh and 100 mesh material is generally considered undesirable for detergent products, with the dusty 100 mesh material being the least desirable.
  • Another unexpected advantage of such use of hexahydrate crystals is that the particle size distribution is more uniform (when the process is repeated, for example, under what are apparently identical conditions) from batch to batch or over an extended continuous run with a given detergent formulation than was heretofore believed possible.
  • Still another surprising advantage resulting from use of sodium tripolyphosphate hexahydrate crystals in accordance with the processes of this invention relates to the rate of conversion of the sodium trime-taphosphate to sodium tripolyphosphate hexahydrate.
  • the proportion of unconverted trimetaphosphate that appears in the final detergent product when hexahydrate crystals are utilized is significantly lower than when hexahydrate crystals are not used.
  • only about 2% of unreacted trimetaphosphate remains in the product from Example I, above, while more than 7% unreacted trimetaphosphate is present in the so-called control material.
  • R for example, can be methyl, ethyl, propyl, isopropyl, butyl, isobutyl, t-butyl, amyl, isoamyl, hexyl, isohexyl, 1,1-dimethyl butyl, 1,2-dimethyl butyl, and the like, which R can be hydrogen, methyl, or ethyl.
  • Typical examples of the lower molecular sulfate compounds of structure (I), above, include benzene sulfonates, toluene sulfonates, xylene sulfonates, 3-ethylbenzene sulfonates, cumene sulfonate, Z-t-butylbenzene sulfonates, 3-n-hexylbenzene sulfonates, and the like.
  • M can be ammonium, sodium, potassium, lithium, rubidium or cesium, but is preferably either ammonium, sodium, or potassium. Of these, because of its cost advantage and its general availability, as well as other considerations, sodium is still further preferred.
  • the lower molecular weight aromatic sulfonate compounds that appear to perform most advantageously in the processes of the present invention are sodium benzene sulfonate, sodium toluene sulfonate, and sodium xylene sulfonate. No logical reasons can be offered as to how or why these lower molecular weight aromatic sulfonate compounds have the surprising eifect that they do on the granulated detergent products. These effects are readily observable, however, and will apparently result no matter in what particular manipulative manner the aromatic sulfonate material is introduced into the slurry, so long as it is reasonably well dispersed or dissolved therein prior to the foaminghydration step of the process.
  • Example II Example I is repeated, except that, instead of the 125 parts of sodium tripolyphosphate hexahydrate crystals, 250 parts of a mixture containing 50 weight percent of powdered (-100 mesh) sodium toluene sulfonate and 50 weight percent of powdered (100 mesh) sodium tripolyphosphate hexahydrate crystals is used. Data comparing the properties of the resulting product with that of Example I, above, can be found in Table 2, below.
  • Example III Example I is repeated, except that only 1800 parts of water and only 100 parts of sodium lauryl sulfate are used, and 500 parts of a condensation product of 12 moles of ethylene oxide with one mole of n-dodecylphenol are utilized in place of the sodium dodecylbenzene sulfonate.
  • the resulting particulated product (after being airdried overnight) contains only about 13 weight percent of mesh particles, and only about 2 weight percent of -100 mesh particles.
  • the final, particulated (air-dried) detergent product consists mostly (more than 60' weight percent) of +l0-mesh particles.
  • a process for manufacturing a detergent composition containing sodium tripolyphosphate hexahydrate which process comprises the steps of (a) interspersing a gas in a fluid aqueous slurry to thereby form a foam; said slurry having a solid dispersed phase comprising sodium trimetaphosphate; (b) simultaneously, maintaining said foam at a temperature below about 135 C.
  • step (b) the improvement which comprises incorporating into said slurry prior to step (b) at least about 1 percent, based on the weight of said slurry, of crystals of sodium tripolyphosphate hexahydrate.
  • said slurry additionally contains from about 1 to about 30 weight percent, on a detergent solids basis, of a lower molecular weight aromatic sulfonate compound having the structure wherein R is selected from the group consisting of hydrogen and alkyl radicals containing from 1 to 6 carbon atoms, R is selected from the group consisting of hydrogen and alkyl radicals containing from 1 to 2 carbon atoms, and. M is an alkali metal cation.
  • a process for manufacturing a porous, particulated solid detergent composition containing sodium tripolyphosphate hexahydrate without the. necessity for a spray-drying step which process comprises the steps of (a) intermixing Water and sodium trimetaphosphate to thereby form a fluid aqueous slurry containing at least about 10 weight percent of sodium trimetaphosphate, (b) adjusting the temperature of at least a portion of said slurry to between about 60 C.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Detergent Compositions (AREA)
US383479A 1964-07-17 1964-07-17 Detergent processes Expired - Lifetime US3423321A (en)

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US38347964A 1964-07-17 1964-07-17

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US (1) US3423321A (ru)
BE (1) BE667032A (ru)
DE (1) DE1467637A1 (ru)
LU (1) LU49100A1 (ru)
NL (2) NL6509189A (ru)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2066255A5 (ru) * 1969-10-24 1971-08-06 Colgate Palmolive Co
US3887614A (en) * 1969-12-03 1975-06-03 Lion Fat Oil Co Ltd Detergent composed of hollow spherical pellets, and process for manufacturing the same
US4151411A (en) * 1978-02-09 1979-04-24 The United States Of America As Represented By The Secretary Of The Navy Laser safety goggles
US6376453B1 (en) * 1997-12-10 2002-04-23 Kao Corporation Detergent particles

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE622142A (ru) * 1961-09-05
BE633146A (ru) * 1962-06-06
US2365190A (en) * 1944-12-19 Washing compositions
US2622068A (en) * 1948-06-04 1952-12-16 Procter & Gamble Process of making heat dried detergent compositions containing form ii sodium triphosphate
US2920939A (en) * 1957-02-14 1960-01-12 Monsanto Chemicals Method of producing phosphates
US3232880A (en) * 1961-04-10 1966-02-01 Ultra Chemical Works Inc Liquid detergent composition

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2365190A (en) * 1944-12-19 Washing compositions
US2622068A (en) * 1948-06-04 1952-12-16 Procter & Gamble Process of making heat dried detergent compositions containing form ii sodium triphosphate
US2920939A (en) * 1957-02-14 1960-01-12 Monsanto Chemicals Method of producing phosphates
US3232880A (en) * 1961-04-10 1966-02-01 Ultra Chemical Works Inc Liquid detergent composition
BE622142A (ru) * 1961-09-05
BE633146A (ru) * 1962-06-06

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2066255A5 (ru) * 1969-10-24 1971-08-06 Colgate Palmolive Co
US3887614A (en) * 1969-12-03 1975-06-03 Lion Fat Oil Co Ltd Detergent composed of hollow spherical pellets, and process for manufacturing the same
US4151411A (en) * 1978-02-09 1979-04-24 The United States Of America As Represented By The Secretary Of The Navy Laser safety goggles
US6376453B1 (en) * 1997-12-10 2002-04-23 Kao Corporation Detergent particles

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DE1467637A1 (de) 1969-12-11
NL6509189A (ru) 1966-01-18
LU49100A1 (ru) 1966-01-17
NL131792C (ru)
BE667032A (ru) 1966-01-17

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