GB2171414A - Granulating detergent additives - Google Patents
Granulating detergent additives Download PDFInfo
- Publication number
- GB2171414A GB2171414A GB08604573A GB8604573A GB2171414A GB 2171414 A GB2171414 A GB 2171414A GB 08604573 A GB08604573 A GB 08604573A GB 8604573 A GB8604573 A GB 8604573A GB 2171414 A GB2171414 A GB 2171414A
- Authority
- GB
- United Kingdom
- Prior art keywords
- granules
- less
- temperature
- granulated solids
- antifoam
- 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.)
- Granted
Links
- 239000003599 detergent Substances 0.000 title claims description 18
- 239000000654 additive Substances 0.000 title 1
- 239000007787 solid Substances 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000002245 particle Substances 0.000 claims abstract description 14
- 239000012530 fluid Substances 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 238000002844 melting Methods 0.000 claims abstract description 9
- 230000008018 melting Effects 0.000 claims abstract description 9
- 239000004615 ingredient Substances 0.000 claims abstract description 8
- 239000008187 granular material Substances 0.000 claims description 32
- 239000002518 antifoaming agent Substances 0.000 claims description 27
- 239000000843 powder Substances 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000001816 cooling Methods 0.000 description 15
- 239000003795 chemical substances by application Substances 0.000 description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 229930195733 hydrocarbon Natural products 0.000 description 10
- 150000002430 hydrocarbons Chemical class 0.000 description 10
- 239000000203 mixture Substances 0.000 description 9
- 239000004215 Carbon black (E152) Substances 0.000 description 6
- 239000006260 foam Substances 0.000 description 6
- 239000002826 coolant Substances 0.000 description 5
- 230000002209 hydrophobic effect Effects 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 238000003860 storage Methods 0.000 description 5
- 239000011162 core material Substances 0.000 description 4
- 230000009849 deactivation Effects 0.000 description 4
- 238000010348 incorporation Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 150000002194 fatty esters Chemical class 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000013019 agitation Methods 0.000 description 2
- 125000000129 anionic group Chemical group 0.000 description 2
- 239000012876 carrier material Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 239000002736 nonionic surfactant Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 230000002028 premature Effects 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- -1 fatty acid ester Chemical class 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 238000010412 laundry washing Methods 0.000 description 1
- 150000002646 long chain fatty acid esters Chemical class 0.000 description 1
- 238000012261 overproduction Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 239000000126 substance Substances 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/0005—Other compounding ingredients characterised by their effect
- C11D3/0026—Low foaming or foam regulating compositions
-
- 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
- B01J2/30—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic using agents to prevent the granules sticking together; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
-
- 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
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)
- Detergent Compositions (AREA)
Abstract
A process for the manufacture of granulated solids, having at least one ingredient with a melting point of at least 10 DEG C, in order to facilitate classification to provide granulated solids of which less than 5% by weight have an average particle diameter of <400 mu m comprises contacting the granulated solids in order to cool them with a fluid having a temperature of less than -50 DEG C for a time and under conditions of mixing such that the temperature of the granulated solids does not fall below -20 DEG C.
Description
SPECIFICATION
Processing of granulated solids
The invention relates to a process for the manufacture of granulated solids, in particular antifoam granules which are suitable for addition to detergent powder products.
Detergent products comprising anionic and/ or nonionic surfactants which are particularly suitable for fabric washing generally have a tendency in use to produce excessive foam.
This can be a problem particularly with drumtype washing machines, and it is accordingly usual to include an antifoam agent in the detergent formulation to reduce or eliminate this tendency to produce excessive foam.
Excessive foam derived from detergent products containing in particular anionic and/or nonionic surfactants can for example be controlled to a limited extent by the addition of soap, or by the incorporation of certain hydrocarbons, silicone oils or hydrophobic silica, or mixtures thereof.
It has for example been proposed in FP-A-2 416 946 to provide a suds regulating (i.e.
antifoam) agent containing a special mixture of liquid hydrocarbon with either a solid hydrocarbon or a fatty acid ester, together with a hydrophobic silica. An example of such an agent contains 30 to 98% by weight of a liquid hydrocarbon, 2 to 70% by weight of an auxiliary substance selected from normally solid hydrocarbons having a melting point of from 35 to 100"C and long chain fatty acid esters of fatty alcohols, or mixtures thereof, together with from 0.1 to 25% by weight of hydrophobic silica.
Such antifoam agents are however difficult to incorporate in a detergent powder in such a manner that their ability to control excessive foam production in a laundry washing process is retained, particularly after storage of the detergent powder prior to use. It is accordingly desirable to incorporate the antifoam agents in the detergent powder during manufacture in a form in which they are protected against premature deactivation, that is migration throughout the powder or even the packaging, so that their effectiveness in controlling excessive foam production, both at low and at high washing temperatures, is maximised.
One means for incorporating such antifoam agents into a detergent powder, while ensuring some measure of protection against premature deactivation, is to provide antifoam particles in the form of granulated solids comprising a water-dispersible core material as a carrier for the antifoam agents, such as the oily materials suggested above.
Although such antifoam granules are highly effective in reducing the tendency of a freshly manufactured detergent product to produce excessive foam, there is still a risk that the antifoam activity will diminish on storage in a detergent powder. This is believed to be due to migration of some of the hydrocarbon material or fatty esters or other oily antifoam active substances from the core material. This can happen more rapidly when such powders are stored at temperatures above room temperature (20"C), and after a period of storage of a few weeks the activity of the antifoam agent can be severely impaired.
It has furthermore been shown that deactivation of the antifoam agent in this way is most rapid when a relatively large proportion of such antifoam granules is present in a detergent powder as fines, that is particles having a mean particle diameter of < 400,um.
From this observation, it has now been shown that the ability of the antifoam agent to remain active in a powdered detergent product during extended storage prior to use can be greatly enhanced if care is taken to ensure that the antifoam granules prior to incorporation into a detergent powder contains a very low level of fines.
This can be achieved for example by classification with air or by sieving, but both procedures have problems particularly when the granules are slightly sticky following granulation, for example due to the presence of a low melting ingredient such as the hydrocarbon material, fatty esters or other oil antifoam actives referred to above.
We have now discovered that the proportion of fines can be reduced if the antifoam agent is subjected to a special cooling step in order to render them less sticky. This also facilitates classification.
If granules containing the antifoam active are cooled to a temperature which is too low, they can become fragible and are more prone to breakdown with the formation of an unacceptable level of "fines".
If however such a cooling step in the manufacture of the antifoam granules is carefully controlled such that the granules themselves are not permitted to harden sufficiently to become frangible, then the yield of granulated solids having a particle size of at least 400Hm is thereby increased.
This process is also applicable to the manufacture of granulated solids of other types which can contain a sticky ingredient where classification to provide particles of a desired size is important.
Accordingly, the invention provides a process for the manufacture of granulated solids, having at least one ingredient with a melting point of at least 10 C, in order to facilitate classification to provide granulated solids of which less than 5% by weight have an average particle diameter of < 400,um, characterised in that the process comprises the step of contacting the granulated solids in order to cool them with a fluid medium having a temperature of less than -50"C for a time and under conditions of mixing such that the tem perature of the granulated solids does not fall below --20"C.
The granulated solids manufactured according to the invention have at least one ingredient with a melting point of at least 10 C, which can render the particles slightly sticky and difficult to handle, particularly at higher temperatures. This can, for example, occur immediately after granulation involving incorporation of the ingredient having a melting point of at least 10 C onto a suitable carrier material.
Examples of such ingredients having a melting point of at least 10 C include certain hydrocarbon materials, fatty esters and other oils, the presence of which can render the granulated solids sufficiently sticky during the early stages of manufacture such that classification to separate fines or oversized granules can be difficult.
It is moreover desirable to ensure that the percentage by weight of fines is not substantially increased during the cooling step.
The granulated solids are mixed in order to cool them with a fluid medium having a temperature of less than 50 C for a time sufficient and under conditions of mixing such that the temperature of the cooled granules does not fall below 2000.
Preferably, the fluid medium has a temperature of less than - 10000. A preferred fluid medium is liquid nitrogen.
It is also preferred that the granulated solids are cooled to a final temperature, before classification as necessary, of at least 0 C, most preferably at least 5"C and ideally at least 10 C.
The choice of final temperature to which the granules are cooled will depend upon their tendency to become frangible and therefore breakdown to form fines.
The final temperature to which the granulated solids are cooled can be selected by simple trial during which the hardness and frangibility of the granular solids is checked at different temperatures of from -20"C to 10 C, and a suitable final temperature selected accordingly.
Although the aim of the special cooling step is to ensure that the percentage by weight of fines is less than 5% by weight of the total, it is preferred to achieve a level of fines which is less than 3% by weight.
The process of cooling can be carried out in any suitable apparatus adapted to mix the fluid medium coolant with the granulated solids. Examples of suitable apparatus include a fluidised bed in which the coolant fluid is introduced below a bed of granules and is forced up through it, or a cooling chamber fitted with a screw conveyer or paddles for agitation which ensure passage of the granules substantially without countercurrent flow thereof that would unduly delay their residence time in the cooling chamber thereby running the risk of cooling the granules to an unacceptably low temperature with the possible overproduction of fines.
Preferably, a cooling chamber is adapted to provide an inlet and an outlet for the fluid coolant medium, the granulated solids being passed through the chamber in the same direction as that of the coolant medium with gentle agitation to ensure even mixing with the coolant to provide uniform cooling, the granules moving, most preferably under gravity from an entry station to an exit station by a conveyer means or under gravity flow.
The invention will be further described with reference to a preferred embodiment which concerns a step in the manufacture of antifoam granules suitable for incorporation into a detergent powder product.
Antifoam granules comprising a core of a carrier material, such as starch, impregnated or coated with liquid and solid hydrocarbons and hydrophobic silica can be prepared by a process which includes the steps of:
i) forming a molten mixture of the liquid and normally solid hydrocarbons together with the hydrophobic silica, the mixture having a melting point which is at least 10 C, and
(ii) spraying the molten mixture onto agitated particles of the core material carried for example in a pan granulator.
The granules so produced as the molten mixture cools will usually be somewhat sticky, while still warm, and in order to classify them to separate fines of them and oversized granules of > 2000,zm, it is necessary to cool them.
According to the process of the invention, the still warm granules from the pan granulator at a temperature of at least 30"C, and usually frm 35-40 C, are conveyed to a cooling station where they are contacted with liquid nitrogen under such conditions that uniform cooling is achieved without undue residence in the cooling station, to ensure that the granules are not cooled to a temperature of less than O"C. This can be achieved by ensuring that there is substantially no countercurrent movement or reworking of the granules within the cooling station to avoid increasing unduly the formulation of fines by attrition between the particles or the internal walls and conveyer means, if any, within the cooling station.
Preferably the granules are cooled to a temperature of from 5 to 10 C to facilitate to subsequent classification in order to select a desired range of particle size which is usually from 400,um to 2,000,us, preferably from 600,um to 1,500,um.
Fines and oversized particles after crushing can be recycled via a further batch of warm granules following granulation, the proportion of fines eventually produced forming 10%, preferably less than 5%, and most preferably less than 3% by weight of the antifoam granules so manufactured.
The antifoam granules so produced having a very low level of fines, show excellent storage properties when incorporated in a detergent powder product, such that deactivation of the antifoam granules and consequent loss of antifoam activity when the detergent product is eventually used is not apparent.
Claims (8)
1. A process for the manufacture of granulated solids, having at least one ingredient with a melting point of at least 10 C, in order to facilitate the classification to provide granulated solids less than 5% by weight of which have an average particle diameter of less than 400m,u, characterised in that the process comprises the step of mixing the granules in order to cool them with a fluid medium having a temperature of less than -50"C for a time and under conditions of mixing such that the temperature of the granules does not fall be low -20"C.
2. A process according to claim 1, in which the fluid medium has a temperature of less than - 1000C.
3. A process according to claim 1 or 2, in which the fluid medium is liquid nitrogen.
4. A process according to claim 1, 2, or 3, in which the granules have an initial temperature of at least 20"C.
5. A process according to any preceding claim, in which the granules have a final temperature of not less than 0 C.
6. A process according to any preceding claim, in which less than 5% by weight of the granulated solids produced by the process have a particle size of less than 400mid.
7. Granulated solids manufactured by the process according to any preceding claim.
8. Granulated solids according to claim 9, which are antifoam granules for addition to a detergent powder product.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB858505062A GB8505062D0 (en) | 1985-02-27 | 1985-02-27 | Processing granulated solids |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| GB8604573D0 GB8604573D0 (en) | 1986-04-03 |
| GB2171414A true GB2171414A (en) | 1986-08-28 |
| GB2171414B GB2171414B (en) | 1988-11-02 |
Family
ID=10575168
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB858505062A Pending GB8505062D0 (en) | 1985-02-27 | 1985-02-27 | Processing granulated solids |
| GB08604573A Expired GB2171414B (en) | 1985-02-27 | 1986-02-25 | Processing of granulated solids |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB858505062A Pending GB8505062D0 (en) | 1985-02-27 | 1985-02-27 | Processing granulated solids |
Country Status (2)
| Country | Link |
|---|---|
| FR (1) | FR2577821A1 (en) |
| GB (2) | GB8505062D0 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0349201A2 (en) * | 1988-06-29 | 1990-01-03 | The Procter & Gamble Company | Detergent granules from cold dough using fine dispersion granulation |
| EP0349200A2 (en) * | 1988-06-29 | 1990-01-03 | The Procter & Gamble Company | Process for making concentrated surfactant granules |
| US5096608A (en) * | 1985-05-13 | 1992-03-17 | The Procter & Gamble Company | Ultra mild skin cleansing composition |
| US5496486A (en) * | 1994-06-30 | 1996-03-05 | Amway Corporation | Process for increasing liquid surfactant loading in free flowing powder detergents |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3721725A (en) * | 1970-08-14 | 1973-03-20 | Du Pont | Process for preparing powder blends |
| GB1340015A (en) * | 1970-02-16 | 1973-12-05 | Eastman Kodak Co | Process for converting a fusible material into solid particles |
-
1985
- 1985-02-27 GB GB858505062A patent/GB8505062D0/en active Pending
-
1986
- 1986-02-25 GB GB08604573A patent/GB2171414B/en not_active Expired
- 1986-02-25 FR FR8602575A patent/FR2577821A1/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1340015A (en) * | 1970-02-16 | 1973-12-05 | Eastman Kodak Co | Process for converting a fusible material into solid particles |
| US3721725A (en) * | 1970-08-14 | 1973-03-20 | Du Pont | Process for preparing powder blends |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5096608A (en) * | 1985-05-13 | 1992-03-17 | The Procter & Gamble Company | Ultra mild skin cleansing composition |
| EP0349201A2 (en) * | 1988-06-29 | 1990-01-03 | The Procter & Gamble Company | Detergent granules from cold dough using fine dispersion granulation |
| EP0349200A2 (en) * | 1988-06-29 | 1990-01-03 | The Procter & Gamble Company | Process for making concentrated surfactant granules |
| US4925585A (en) * | 1988-06-29 | 1990-05-15 | The Procter & Gamble Company | Detergent granules from cold dough using fine dispersion granulation |
| EP0349201A3 (en) * | 1988-06-29 | 1990-06-20 | The Procter & Gamble Company | Detergent granules from cold dough using fine dispersion granulation |
| EP0349200A3 (en) * | 1988-06-29 | 1990-06-20 | The Procter & Gamble Company | Process for making concentrated surfactant granules |
| US5496486A (en) * | 1994-06-30 | 1996-03-05 | Amway Corporation | Process for increasing liquid surfactant loading in free flowing powder detergents |
| US5635467A (en) * | 1994-06-30 | 1997-06-03 | Amway Corporation | Powdered composition exhibiting increased liquid surfactant loading for free flowing powder detergents |
Also Published As
| Publication number | Publication date |
|---|---|
| GB8505062D0 (en) | 1985-03-27 |
| GB2171414B (en) | 1988-11-02 |
| FR2577821A1 (en) | 1986-08-29 |
| GB8604573D0 (en) | 1986-04-03 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PCNP | Patent ceased through non-payment of renewal fee |