GB2445939A - Detergent granules and process for manufacturing said granules - Google Patents
Detergent granules and process for manufacturing said granules Download PDFInfo
- Publication number
- GB2445939A GB2445939A GB0701561A GB0701561A GB2445939A GB 2445939 A GB2445939 A GB 2445939A GB 0701561 A GB0701561 A GB 0701561A GB 0701561 A GB0701561 A GB 0701561A GB 2445939 A GB2445939 A GB 2445939A
- Authority
- GB
- United Kingdom
- Prior art keywords
- pas
- granules
- vrv
- drier
- less
- 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.)
- Withdrawn
Links
- 239000008187 granular material Substances 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 15
- 230000008569 process Effects 0.000 title claims abstract description 15
- 239000003599 detergent Substances 0.000 title claims abstract description 5
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- 239000002253 acid Substances 0.000 claims abstract description 19
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 10
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 5
- 229910000323 aluminium silicate Inorganic materials 0.000 claims abstract description 4
- 230000015556 catabolic process Effects 0.000 claims abstract description 4
- 238000006731 degradation reaction Methods 0.000 claims abstract description 4
- 239000010409 thin film Substances 0.000 claims abstract 4
- 239000003795 chemical substances by application Substances 0.000 claims abstract 3
- 230000003472 neutralizing effect Effects 0.000 claims abstract 3
- 239000003792 electrolyte Substances 0.000 claims abstract 2
- 238000011065 in-situ storage Methods 0.000 claims abstract 2
- 239000002243 precursor Substances 0.000 claims abstract 2
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 235000017550 sodium carbonate Nutrition 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims 3
- 229920006395 saturated elastomer Polymers 0.000 claims 1
- 238000000354 decomposition reaction Methods 0.000 description 9
- 229910021536 Zeolite Inorganic materials 0.000 description 6
- 239000010457 zeolite Substances 0.000 description 6
- 238000006386 neutralization reaction Methods 0.000 description 4
- 125000000217 alkyl group Chemical group 0.000 description 3
- 239000003945 anionic surfactant Substances 0.000 description 3
- WUBBRNOQWQTFEX-UHFFFAOYSA-N 4-aminosalicylic acid Chemical compound NC1=CC=C(C(O)=O)C(O)=C1 WUBBRNOQWQTFEX-UHFFFAOYSA-N 0.000 description 2
- -1 alkyl sulphate Chemical compound 0.000 description 2
- LVKZSFMYNWRPJX-UHFFFAOYSA-N benzenearsonic acid Natural products O[As](O)(=O)C1=CC=CC=C1 LVKZSFMYNWRPJX-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 235000012149 noodles Nutrition 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229920006012 semi-aromatic polyamide Polymers 0.000 description 2
- 229910021653 sulphate ion Inorganic materials 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 125000003342 alkenyl group Chemical group 0.000 description 1
- 150000004996 alkyl benzenes Chemical class 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 150000003138 primary alcohols Chemical class 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 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
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
-
- 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
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/14—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
- C11D1/146—Sulfuric acid esters
-
- 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
-
- 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
- C11D11/04—Special methods for preparing compositions containing mixtures of detergents by chemical means, e.g. by sulfonating in the presence of other compounding ingredients followed by neutralising
-
- 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
- C11D3/046—Salts
-
- 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
- C11D3/10—Carbonates ; Bicarbonates
-
- 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
- C11D3/12—Water-insoluble compounds
- C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
- C11D3/1246—Silicates, e.g. diatomaceous earth
- C11D3/128—Aluminium silicates, e.g. zeolites
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
Detergent granules, comprising: <SL> <LI>i) 30-60% of PAS: <LI>ii) 10-20% aluminosilicate(s): <LI>iii) 20-60% of one or more inorganic electrolytes, such as sodium carbonate: <LI>iv) <5% MOISTURE </SL> characterised in that they contain less than 1 wt% of PAS degradation components. Also disclosed is a single stage process for making the granules in a horizontal thin-film evaporator/drier provided with agitating means and at least three heat transfer jackets, comprising neutralizing PAS-precursor acid in-situ using a stoichiometric excess of a neutralizing agent, whereby water is removed from the evaporator/drier by co-current air-flow until the water content of the granules is less than 5 wt %.
Description
Granulation of PAS using a VRV
Technical field
This invention relates to a process to make PAS granules using a VRV flash reactor/drier.
Background
The horizontal Flash Drier (VRV) from VRV SpA Impianti Industriali may also be used as a flash reactor. The drying zone of a VRV may have a heat transfer area of at least m2. The cooling zone of the VRV desirably has a heat transfer area of at least 5 m2.
Use of a VRV for the dry neutralisation and granulation of anionic surfactant acid, in particular primary alkyl sulphate acid, (PAS acid) is known from W096/06917 and W097/32002. In each case, at least 20% Zeolite is present in the granules.
In W02005/054422, a VRV equipment is used together with exemplified LAS acid neutralisation in a modification of the process said to address malodour problems. It is stated that the anionic surfactant can be any of the known anionic surfactants. However, there is a preference for the salts of LAS and PAS surfactants. LAS being long chain alkyl benzene sulphonates and PAS being primary alkyl suiphates.
The solution to the malodour problem is taught to be the addition of particular types of antioxidents. Such materials are costly arid may not be compatible with all compositions to which the granule may be added.
W002/24853 discloses LAS acid neutralisation processes using a VRV flash dryer. Aluminosilicate (Zeolite) is added at specific places during the VRV processing in order to affect the quality of the product. It is disclosed that an alternative surfactant system could be alkyl and/or alkenyl sulphuric acid half-esters (i.e. the sulphation products of primary alcohols) which give alkyl and/or alkenyl suiphates upon neutralisation. The invention is said to have especial applicability in the production of detergent particles comprising PAS having a chain length of C10-22, preferably C12-14; Coco PAS is disclosed to be particularly desirable.
PAS pastes are known as materials used in non tower route (NTR) processing: US5712242, EP0929651, and EP1025199.
Conventional (non flash dryer) NTR processing of PAS-acid with Zeolite is known from EP0506184, 5P0707632, and EP0436240.
High active PAS noodles are commercially available; these are manufactured from PAS paste. These noodles require further processing to produce granules suitable for inclusion in a laundry detergent powder.
A disadvantage of the prior art processes when using PAS acid is the known high rate of decomposition of PAS acid.
This can be partially solved by locating the VRV flash reactor / drier / granulator close to the suiphonation plant that produces the PAS acid. By such close proximity, possible decomposition of the PAS before processing may be reduced. The reaction heat may nevertheless lead to decomposition of PAS acid during processing inside the VRV flash reactor I drier. Thus, there remains a need for a single-stage process to granulate PAS, starting from PAS acid which is also capable of forming granules with greater than 20 wt% PAS without undue decomposition of the PAS acid.
Under conventional VRV processing conditions, severe decomposition of PAS occurs. This gives rise to colour and odour formation, as well as making the resulting granules softer and stickier.
Summary of the Invention
This decomposition problem may be solved by sufficient removal of the reaction heat from the VRV. According to the present invention, this is done in several synergistically operating ways.
Firstly, addition of water (up to 3% on PAS acid) into the reaction zone removes heat by evaporation and lowers product temperature. This consequently reduces the amount of decomposition and also gives improved granule properties.
The temperature reduction at the outlet has been found to have particular significance in this regard.
Secondly, increasing the air flow rate through the VRV, particularly when the exhaust air is close to moisture saturation, has been found to give lower decomposition.
Thirdly, for removal of the heat of reaction provision of cooling on all three jackets of the VRV is preferred.
Fourthly, splitting the PAS acid addition along the length of the VRV reactor enables a reduction of up to 10% in soda ash requirement.
Using a suitable combination of these process improvements, a PAS granule may be produced with low degradation during the reaction whilst maintaining an economically feasible granule production rate (based on 100% active PAS) at value.
For best granule properties Zeolite is desirably present at <5 wt% of the total solids present in the final jacket stage of the VRV reactor.
The process according to the invention gives a good colour, odour, and low stickiness, high active content PAS granules from PAS acid in a single process operation, and with a low level of Zeolite, to minimise cost.
Examples
Showing effect of water addition, increase of air flow and heating of jacket 2 of the VRV. Also, the throughput benefit resulting from split PAS addition to different port of the VRV.
Example number 1 2 3 4 5 6 PASA split YIN. N N N N N Y Water, % of PASA flow 0.0 0.0 8.2 7.3 9.9 3.7 Air flow, kg/hr N/A N/A 7.8 15.6 19 20 Jacket 1, C 84 16 16 16 130 15 Jacket 2, C 84 16 130 160 127 16 Jacket 3, C 16 16 16 16 16 17 Total t'put, kg/hr 60 42 40 46 111 126 Nominal %NaPAS 34.1 47.7 44.5 43.5 38.1 40.7 Nom % Soda ash 11 33 42.0 28.1 56.4 54.1 Nom % Zeolite 53 16 12.0 27.1 4.3 4.0 Product temp, C 64 42 45 42 65 48 % SO4 ( decomp) 5.2 3.8 1.9 1.5 0.5 0.3 Product quality Too Fine Poor Good Good V Good V Good Pass/Fail Fail Fail Pass Pass Pass Pass Examples 1-2 fail because of no water addition leading to excessive decomposition, (>3%) . Examples 3-6 pass.
The amount of sulphate in the product was analysed and is considered to be a good indication of the extent of degradation of the PAS. Levels below 2wt%, based on product weight, are considered to be acceptable within the definition of this invention.
Claims (6)
1. Detergent granules, comprising 1. from 30-60% of PAS ii. from 10-20% aluminosilicate(s) iii. from 20-60% of one or more inorganic electrolytes, such as sodium carbonate iv. <5% moisture characterised in that they contain less than 1 wt% of PAS degradation components.
2. A single stage process for manufacturing the granules of claim 1, the process being carried out in a VRV horizontal thin film evaporator I drier, provided with agitating means and with at least three heat transfer jackets and preferably having a ratio between granular product throughput (in kg/hr) and total heat transfer jacket area (in ni2) of at least 75, whereby the PAS-precursor acid feedstock is neutralised in-situ by a stoichiometric excess of a fine powdered neutralising agent, preferably selected from Na2CO3, NaOH, optionally in the presence of 2 to 10 wt% water (on product) and preferably having a mean particle size of 150 to 250j, and whereby water is removed from the horizontal thin film evaporator I drier by co-current airflow until the water content of the particles is less than 5 wt%, preferably less than 2 wt%, characterised in that up to 3 wt%, based on PAS acid, water is added into the reaction zone to remove heat by evaporation and thereby lower product temperature.
3. A process according to claim 2 wherein a layering agent, in particular an aluminosilicate, is added to the horizontal thin film evaporator I drier in an amount of less than 30 wt %, preferably less that 20 wt% of the product.
4. A process according to claim 2 or claim 3 in which at least the final, preferably the first and third and most preferably all of the at least three heat transfer jackets are operated at a temperature of below 20 C.
5. A process according to any one of claims 2 to 4 in which the air flow rate through the VRV is set to be high enough to ensure that the exhaust air is not saturated with moisture.
6. A process according to any one of claims 2 to 5 in which the PAS acid addition is split to be made in at least two places along the length of the VRV reactor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB0701561A GB2445939A (en) | 2007-01-27 | 2007-01-27 | Detergent granules and process for manufacturing said granules |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB0701561A GB2445939A (en) | 2007-01-27 | 2007-01-27 | Detergent granules and process for manufacturing said granules |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| GB0701561D0 GB0701561D0 (en) | 2007-03-07 |
| GB2445939A true GB2445939A (en) | 2008-07-30 |
Family
ID=37872876
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB0701561A Withdrawn GB2445939A (en) | 2007-01-27 | 2007-01-27 | Detergent granules and process for manufacturing said granules |
Country Status (1)
| Country | Link |
|---|---|
| GB (1) | GB2445939A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5490954A (en) * | 1993-07-05 | 1996-02-13 | Lever Brothers Company, Division Of Conopco, Inc. | Detergent composition or component containing anionic surfactant and process for its preparation |
| US5646107A (en) * | 1994-08-26 | 1997-07-08 | Lever Brothers Company, Division Of Conopco, Inc. | Production of anionic surfactant granules |
| US5856294A (en) * | 1996-02-26 | 1999-01-05 | Lever Brothers Company, Division Of Conopco, Inc. | Production of anionic detergent particles |
| WO2002024853A1 (en) * | 2000-09-25 | 2002-03-28 | Unilever Plc | Production of anionic surfactant granules by in situ neutralisation |
-
2007
- 2007-01-27 GB GB0701561A patent/GB2445939A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5490954A (en) * | 1993-07-05 | 1996-02-13 | Lever Brothers Company, Division Of Conopco, Inc. | Detergent composition or component containing anionic surfactant and process for its preparation |
| US5646107A (en) * | 1994-08-26 | 1997-07-08 | Lever Brothers Company, Division Of Conopco, Inc. | Production of anionic surfactant granules |
| US5856294A (en) * | 1996-02-26 | 1999-01-05 | Lever Brothers Company, Division Of Conopco, Inc. | Production of anionic detergent particles |
| WO2002024853A1 (en) * | 2000-09-25 | 2002-03-28 | Unilever Plc | Production of anionic surfactant granules by in situ neutralisation |
Also Published As
| Publication number | Publication date |
|---|---|
| GB0701561D0 (en) | 2007-03-07 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| WAP | Application withdrawn, taken to be withdrawn or refused ** after publication under section 16(1) |