US3639288A - Detergent slurry process - Google Patents

Detergent slurry process Download PDF

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Publication number
US3639288A
US3639288A US714523A US3639288DA US3639288A US 3639288 A US3639288 A US 3639288A US 714523 A US714523 A US 714523A US 3639288D A US3639288D A US 3639288DA US 3639288 A US3639288 A US 3639288A
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United States
Prior art keywords
sodium tripolyphosphate
slurry
water
dispersion
crystals
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Expired - Lifetime
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US714523A
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English (en)
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Frederik Johan Kerkhoven
Seyer Troost
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Lever Brothers Co
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Lever Brothers Co
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    • 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
    • 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

Definitions

  • ABSTRACT I Detergent compositions are produced by heat-drying a slurry Mar. 21, Netherlands containing small crystals of Sodium p yp p ahydrate. The small crystals are formed by dispersing an- [52] [1.8. CI yd ip yp p in water prior to its y 252/137 252/138 tion with the water and subsequently other constituents of the [5 1] ll ll.
  • Heat-dried detergent compositions containing sodium tripolyphosphate are conventionally made by firstly preparing a fluid mixture of water, surface-active agents and usually inorganic salts, adding sodium tripolyphosphate to this mixture and subsequently heat-drying the resulting slurry, for example by spray-drying. Due to fluctuations in the quality of commercial sodium tripolyphosphates, mainly in their fast hydrating Form I and slower hydrating Form ll content, but also in their moisture, trace metal and other phosphates content, and in their specific surface area, etc., there are often undesired variations in their processing and consequently in the uniformity of the resulting products. Additionally, unpredictable changes in slurry viscosity, caused by variations in the hydration characteristics of the sodium tripolyphosphate used, give difficulties in the subsequent heat-drying.
  • the different hydration characteristics of different sodium tripolyphosphates can also give wide variations in the proper ties of the heat-dried detergent compositions prepared from them.
  • the application of conventional slurry-making techniques when using sodium tripolyphosphate with a high, fast hydrating, Form l content can allow the formation of hard lumps, commonly termed grit, in the slurries which cause blockages in pipes, filters and spraying nozzles.
  • This delayed hydration, coupled with the relatively high solubility in water of Form l sodium tripolyphosphate is believed to result in the formation of large crystals of sodium tripolyphosphate hexahydrate in the slurry.
  • the sodium tripolyphosphate hexahydrate crystals should have a maximum dimension of not greater than 100/1. as larger crystals are apt to impart crawly flow properties to the dried compositions, especially in the case of compositions of the mixed active type containing a nonionic surface-active agent. in some particularly difficult cases crawly powder properties may even be obtained with a crystal size of less than 100p.
  • the invention includes, in one aspect, a detergent composition containing sodium tripolyphosphate hexahydrate crystals substantially all of which have a maximum dimension ofnot more than 50
  • the small sodium tripolyphosphate hexahydrate crystals formed in the process of the invention can be produced from any commercial quality of anhydrous sodium tripolyphosphate, whether of high Form l or of high Form ll content, provided that the sodium tripolyphosphate is substantially homogeneously dispersed in the water prior to hydration. This dispersion is preferably performed using intensive stirring. it will be appreciated that the anhydrous sodium tripolyphosphate should be in powder form to enable the dispersion to be achieved.
  • the operating temperatures for the dispersion of the anhydrous sodium tripolyphosphate in the water and for its subsequent hydration are chosen according in particular to the type of sodium tripolyphosphate used, the type of apparatus employed for both operations, the other components, if any, in the water of dispersion and the crystal size desired in the product. For economic reasons it is desirable to use both for dispersion and hydration temperatures in the region of ambient temperature and it is an important beneficial feature of the present invention that this may be achieved while obtaining high-quality products.
  • anhydrous sodium tripolyphosphate in order to disperse substantially homogeneously the anhydrous sodium tripolyphosphate in the water prior to its hydration it is preferred to use intensive stirring at the point of their first contact.
  • An apparatus found to be highly effective for accomplishing this is a nonrecirculatory, intensively stirrable device for example a disc-rotor pump which has the advantage of having a small holdup.
  • the subsequent hydration of the dispersed sodium tripolyphosphate can be accomplished in less intensively stirred vessels, for example in a Lang disintegrator mixer.
  • anhydrous sodium tripolyphosphate Using sufficiently rapid dispersion of the anhydrous sodium tripolyphosphate in the water it is possible to form the desired small crystals of the hexahydrate from all commercially available types of anhydrous sodium tripolyphosphate at temperatures of around ambient temperature, that is within the-region of from about l5 to 45 C., preferably from about 20 to 25 C.
  • anhydrous sodium tripolyphosphate particularly those having a high Form l content
  • the rate of hydration should be lowered, usually by the use of temperatures higher or lower than ambient temperatures, so as to allow dispersion to be achieved before hydration. This is particularly important in the case of anhydrous sodium tripolyphosphate with a high content of fast-hydrating Form l material. It has been found that the process of the present invention can be accomplished in crutcher mixers using water temperatures as low as from about 0 to 15 C.
  • hydration should be allowed to occur by raising the temperature, preferably to within from about 15 to 45 C. At these temperatures it is believed that hydration proceeds at a maximum rate, which is conducive to the production of small crystals.
  • the use of water to form the dispersion of the anhydrous sodium tripolyphosphate is an essential feature of the present invention. This enables dispersion of the sodium tripolyphosphate to be accomplished before hydration, which would be prevented by the presence of major quantities of other ingredients in the water, and is so prevented in conven-' tional slurry-making processes in which the anhydrous sodium tripolyphosphate is the last component to be added to the slurry and in which relatively large sodium tripolyphosphate crystals are thereby formed. in order to obtain large numbers of small crystals as required it is desirable to have hydration occur at a high rate.
  • the ratio of the water to the anhydrous sodium tripolyphosphate used in the process effects to some extent the size of the sodium tripolyphosphate crystals produced.
  • the water used for dispersion of the anhydrous sodium tripolyphosphate may contain minor amounts of other constituents of the detergent composition to be produced, for example up toabout percent by weight of other constituentsThis is, of course, appreciably less than the proportion of nonaqueous constituents in conventional aqueous slurries before addition of the I anhydrous sodiu tripolyphosphate.
  • sodium silicates water-glass
  • an anionic surface-active agent for example soap
  • soap may advantageously be added to the water used to form the dispersion of the sodium tripolyphosphate or to the dispersion itself prior to hydration.
  • the use of both the silicates and the anionic surfactant appear to aid the formation of small crystals of the sodium tripolyphosphate hexahydrate and the presence of the latter improves the handling properties of the slurry.
  • the process according to the invention is particularly advantageous in that it enables the production of detergent compositions having good physical properties, irrespective of the type of detergent active material or mixtures thereof used.
  • the process of the invention is beneficial in preparing low-sudsing, ternary active compositions which contain synthetic anionic surface-active agents, nonionic surface-active agents and soaps, which are recognized as being particularly difficult to manufacture with good physical properties. Hitherto, it has been very difficult to produce a noncaking powder based on these mixed active systems, especially those which contain a relatively large amount of the nonionic constituent.
  • An additional advantage of the process according to the invention is that it can be applied successfully to all commercial qualities of anhydrous sodium tripolyphosphate. Further, process conditions may be chosen to suit a variety of different qualitiesof sodium tripolyphosphate so that the process may be operated without the frequent changes of conditions otherwise necessary.
  • the process of the invention is readily adaptable to the continuous preparation of detergent slurries for subsequent heatdrying but is also suitable for batchwise operation.
  • the anhydrous sodium tripolyphosphate is dispersed in the water continuously, the hydration of the sodium tripolyphosphate and the subsequent admixing of the other constituents being operable on either a continuous or a batchwise basis.
  • the invention comprises an apparatus for the preparation of a slurry for heat-drying to form a detergent composition, comprising a nonrecirculatory, intensively stirrable device, dosing systems for continuously feeding water and anhydrous sodium tripolyphosphate to the intensively stirrable device so as to disperse substantially homogeneously the sodium tripolyphosphate in the water, a stirrable vessel adapted to receive the dispersion of sodium tripolyphosphate in water from the intensively stirrable device and means for feeding other ingredients of the detergent composition to the stirrable vessel.
  • FIG. 1 shows a continuously operable slurry-making apparatus while the apparatus in FIG. 2 is adapted for batchwise operation.
  • a disc-rotor pump 1 having a motor la, a rotatable disc lb and a hopper 1c is supplied with water through a pipe 2, the flow through which is controlled by a valve 3 and a flowmeter 4.
  • a hopper 5 is positioned over an endless belt 6 for feeding anhydrous sodium tripolyphosphate to the disc-rotor pump 1.
  • a pipe 7 connects with the pipe 2 for feeding any additional liquid materials to the disc-rotor pump.
  • An output pipe 8 from the disc-rotor pump I leads into a Lang disintegrator mixer 9, comprising an open top vessel 9a, an impeller 9b and a motor 90.
  • a further pipe 10 leads into the Lang mixer for the addition thereto of any additional materials.
  • the output pipe 11 from the Lang mixer 9 is controlled by a valve 12 and leads to a pump 13 and thence to apparatus which is different in the two Figures. I v
  • the pipe 11 from the Lang mixer 9 leads'into a second Lang disintegrator mixer 14, having an open top vessel 14a, an impeller 14b and a motor 14c.
  • An additional pipe 15 also leads into the second Lang mixer 14 for supplying thereto any other liquid constituents of detergent compositions being prepared. Further means (not shown) may be provided for adding any solid slurry constituents to the Lang mixer 14.
  • the output pipe 16 from the second Lang mixer 14 is controlled by a valve 17.
  • the pipe 11 from the Lang mixer 9 leads to two crutcher mixers l8 and 19, each having an open tope vessel, 18a and 19a and an impeller 18b and 19b, respectively (the means for rotating the impellers is not shown).
  • the flow from the pipe 11 to the crutcher mixers l8 and 19 is controlled, respectively, by valves 20 and 21.
  • a further pipe 22 leads to the crutcher mixers l8 and 19, for supplying any other liquid slurry constituents to the mixers, as controlled by valves 23 and 24, respectively. Further means (not shown) may be provided for adding any other solid slurry constituents to the mixers.
  • the outputs from the crutcher mixers, 18 and 19 are controlled by valves 25 and 26, respectively, connecting with a common pipe 27.
  • anhydrous sodium tripolyphosphate is fed to the disc-rotor pump 1 from the belt 6 at a constant rate while water, containing any desired additives such as silicates from the pipe 7, is fed to the disc-rotor pump through the pipe 2.
  • the sodium tripolyphosphate is very rapidly dispersed in the water before any substantial degree of hydration can take place.
  • the dispersion of the sodium tripolyphosphate in the water is fed to the Lang mixer 9, to which any other desired additive, for example soap, is fed through the pipe 10. Hydration occurs to some extent in the Lang mixer.
  • the slurry so formed is then fed either to the second Lang mixer 14 in FIG. 1 or to one or other of the crutcher mixers 18 and 19 in FIG. 2.
  • the other ingredients of the slurries are fed through the line 15 in FIG. 1 or the line 22 in FIG. 2 to the final mixing vessels so as to produce, in the apparatus shown in FIG. 1 in a continuous stream of slurry and in the apparatus shown in FIG. 2 a series of batches of slurry from alternate crutcher mixers, which are discharged to heat-drying apparatus through the lines 16 and 27 in FIGS. 1 and 2 respectively.
  • the slurry For the final heat-drying it is usual to heat the slurry to about 70-80 C. or higher, which temperature may be used for the admixture of the other detergent constituents if desired.
  • the final slurry is of excellent and stable consistency for pumping and spraying in the heat-drying process.
  • detergent compositions can be prepared by the process of the invention, including those containing anionic and/or nonionic and/or even amphoteric substances as the detergent active agent or agents.
  • detergent active agents which are generally compatible with sodium tripolyphosphate, include for example soaps (i.e., the sodium and/or potassium salts of long chain fatty acids, water-soluble alkylaryl sulphonates, such as sodium dodecyl benzene sulphonate and sodium tetradecyl benzene sulphonates, water-soluble alkane and alkene sulphonates, alkyl sulphates obtained for example by sulphation of aliphatic alcohols with branched or unbranched alkyl chains, including sodium lauryl sulphate, sodium hexadecyl sulphate and sodium octadecyl sulphate, alkali salts of sulphated or phosphated alkylene oxide condensation products prepared by ethoxy
  • the above substances may form the active detergent components of the detergent composition of the invention.
  • the detergent compositions may additionally contain other conventional additives, including for example various fillers, alkaline substances, soilsuspending' agents, bleaching agents, optical brighteners, coloring agents, germicides, perfumes and lather boosters.
  • the resultant sodium tripolyphosphate dispersion was fed from the pump to a 30 liters capacity stirred tank which each time it became filled was emptied and its contents poured into a larger stirred tank of 1,000 liters capacity.
  • the slurry was heated and the contents of the tank made up to about 1,000 liters with the following:
  • EXAMPLE II An aqueous sodium silicate solution and powdered anhydrous sodium tripolyphosphate (of 20 percent Form l content) were continuously dosed to a disc-rotor pump arranged as in example l.
  • the aqueous solution had the composition:
  • the resultant mixture was heated to 80 C. and pumped to a spray-drying plant from which it was spray-dried to give a freeflowing, crisp, dry detergent composition having no tendency to caking.
  • the resultant solution was continuously fed at 20 C, and at a rate of about 7 kg./min, to a disc-rotor pump.
  • Anhydrous sodium tripolyphosphate (about 30 Form 1) was also fed to the disc-rotor pump at a rate of 4.13 kg./min.
  • a separate flow of alkyl benzene sulphonate paste was fed to the disc-rotor pump at a rate of 3.0 kg./min. After 45 minutes the flows of material to the disc-rotor pump were stopped and the resultant mixture which had been fed to a stirred mixing tank was made up with the following:
  • the slurry thus obtained contained sodium tripolyphosphate crystals of approximately 20-40,:t.
  • a detergent composition prepared by spray-drying the slurry was free-flowing and showed no tendency to caking.
  • the resultant detergent slurry was continuously pumped to a tower from which it was spray-dried to give a detergent composition which contained sodium tripolyphosphate hexahydrate crystals of about 20-30;; in size.
  • the composition was exceptionally free-flowing, dry and had a good appearance.
  • compositions which was prepared by a process of the invention had hexahydrate crystals of 50-70;.t. This composition had a satisfactory appearance but was less free-flowing than the composition of 20-30;. crystal size, although still acceptable.
  • a further composition having the same constitution was prepared by a conventional process.
  • the hexahydrate crystal size range in the composition was about 80-l 10p. and the composition had crawly" flow properties instead of being free flowing and it felt rather sticky.
  • detergent compositions of the low-sudsing type containing termary mixtures of I detergent active compounds should contain sodium tripolyphosphate hexahydrate crystals the size of substantially-all of which is not more than about IOO for them to be acceptable.
  • a process for preparing a detergent slurry containing sodium tripolyphosphate hexahydrate crystals of a size not exceeding 100p. for spray drying to form a built detergent composition which comprises forming a substantially homogeneous dispersion of anhydrous sodium tripolyphosphosphate in water at a temperature between about C. to about l C.
  • a process for preparing a heat-dried built detergent composition containing sodium tripolyphosphate hexahydrate crystals of a size not exceeding p. which comprises forming substantially homogeneous dispersion of anhydrous sodium tripolyphosphate in water at a temperature between 0 C. to.

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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)
US714523A 1967-03-21 1968-03-20 Detergent slurry process Expired - Lifetime US3639288A (en)

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NL6704145A NL6704145A (xx) 1967-03-21 1967-03-21

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US (1) US3639288A (xx)
AT (1) AT288570B (xx)
BE (1) BE712428A (xx)
CH (1) CH498194A (xx)
DE (1) DE1767002A1 (xx)
ES (2) ES351808A1 (xx)
FR (1) FR1556820A (xx)
GB (1) GB1223613A (xx)
LU (1) LU55733A1 (xx)
NL (1) NL6704145A (xx)

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4115308A (en) * 1976-12-27 1978-09-19 The Procter & Gamble Company High-shear process for preparing silicate-containing paste-form detergent compositions
US4264464A (en) * 1977-10-06 1981-04-28 Colgate-Palmolive Company High bulk density particulate heavy duty laundry detergent
US4276326A (en) * 1976-02-26 1981-06-30 Colgate-Palmolive Company Free flowing builder beads and detergents
US4330424A (en) * 1978-12-28 1982-05-18 Colgate Palmolive Company Free flowing builder beads and detergents
US4399048A (en) * 1977-10-06 1983-08-16 Colgate-Palmolive Company High bulk density particulate heavy duty laundry detergent
US4406808A (en) * 1977-10-06 1983-09-27 Colgate-Palmolive Company High bulk density carbonate-zeolite built heavy duty nonionic laundry detergent
US4414129A (en) * 1976-02-26 1983-11-08 Colgate Palmolive Company Free-flowing builder beads and detergents
US4462804A (en) * 1980-11-26 1984-07-31 Colgate Palmolive Company High bulk density particulate heavy duty laundry detergent
DE3339092A1 (de) * 1983-07-09 1985-01-24 Blaser, René, Luzern Vorrichtung zum transportieren von containern zwischen containerlagern und mindestens einem verfahrbaren brueckenkran und umschlagen der container vom kran zu einer transporteinrichtung und umgekehrt
US4537708A (en) * 1983-08-30 1985-08-27 Fmc Corporation Homogeneous laundry detergent slurries containing nonionic surface-active agents
US4597889A (en) * 1984-08-30 1986-07-01 Fmc Corporation Homogeneous laundry detergent slurries containing polymeric acrylic stabilizers
GB2340050A (en) * 1998-07-31 2000-02-16 Karl Cornelius Mccarthy Mixing detergent composition for stable storage in deformable plastic containers

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3133024A (en) * 1961-03-14 1964-05-12 Monsanto Chemicals Heat-dried detergent processes
US3174934A (en) * 1961-04-24 1965-03-23 Monsanto Co Hydration of sodium tripolyphosphate

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3133024A (en) * 1961-03-14 1964-05-12 Monsanto Chemicals Heat-dried detergent processes
US3174934A (en) * 1961-04-24 1965-03-23 Monsanto Co Hydration of sodium tripolyphosphate

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4414129A (en) * 1976-02-26 1983-11-08 Colgate Palmolive Company Free-flowing builder beads and detergents
US4276326A (en) * 1976-02-26 1981-06-30 Colgate-Palmolive Company Free flowing builder beads and detergents
US4115308A (en) * 1976-12-27 1978-09-19 The Procter & Gamble Company High-shear process for preparing silicate-containing paste-form detergent compositions
US4264464A (en) * 1977-10-06 1981-04-28 Colgate-Palmolive Company High bulk density particulate heavy duty laundry detergent
US4399048A (en) * 1977-10-06 1983-08-16 Colgate-Palmolive Company High bulk density particulate heavy duty laundry detergent
US4406808A (en) * 1977-10-06 1983-09-27 Colgate-Palmolive Company High bulk density carbonate-zeolite built heavy duty nonionic laundry detergent
US4330424A (en) * 1978-12-28 1982-05-18 Colgate Palmolive Company Free flowing builder beads and detergents
US4462804A (en) * 1980-11-26 1984-07-31 Colgate Palmolive Company High bulk density particulate heavy duty laundry detergent
DE3339092A1 (de) * 1983-07-09 1985-01-24 Blaser, René, Luzern Vorrichtung zum transportieren von containern zwischen containerlagern und mindestens einem verfahrbaren brueckenkran und umschlagen der container vom kran zu einer transporteinrichtung und umgekehrt
US4537708A (en) * 1983-08-30 1985-08-27 Fmc Corporation Homogeneous laundry detergent slurries containing nonionic surface-active agents
US4597889A (en) * 1984-08-30 1986-07-01 Fmc Corporation Homogeneous laundry detergent slurries containing polymeric acrylic stabilizers
GB2340050A (en) * 1998-07-31 2000-02-16 Karl Cornelius Mccarthy Mixing detergent composition for stable storage in deformable plastic containers
GB2340050B (en) * 1998-07-31 2002-12-11 Karl Cornelius Mccarthy A process for manufacturing liquid products

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BE712428A (xx) 1968-09-19
AT288570B (de) 1971-03-10
ES366684A1 (es) 1971-04-16
GB1223613A (en) 1971-02-24
NL6704145A (xx) 1968-09-23
FR1556820A (xx) 1969-02-07
ES351808A1 (es) 1969-12-01
CH498194A (de) 1970-10-31
LU55733A1 (xx) 1969-10-02
DE1767002A1 (de) 1971-08-19

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