GB2568867A

GB2568867A - Dishwashing detergent gel comprising bleach

Info

Publication number: GB2568867A
Application number: GB1717978.9A
Authority: GB
Inventors: Chevalier Olivier; Luca Mascio
Original assignee: McBride SA
Current assignee: McBride SA
Priority date: 2017-10-31
Filing date: 2017-10-31
Publication date: 2019-06-05
Also published as: GB201717978D0

Abstract

A non-aqueous liquid detergent composition comprises a fluid continuous phase and a suspended solid phase. The fluid phase comprises more than 50% by weight glycerol, between 1 and 3% sodium sulphate and less than 1% water. The solid phase comprises an oxygen bleach providing between 0.2 and 5% available oxygen and anhydrous sodium sulphate. The fluid phase may be a saturated solution of sodium sulphate. The oxygen bleach, which may be sodium bicarbonate, may be present as a granule comprising the anhydrous sodium sulphate. The composition, as a whole, many comprise from 1 to 10% water, and the water may be present as water of crystallisation of the sodium sulphate. The sodium sulphate may be between 1 and 15% of the composition. Between 100 and 90% of the sodium sulphate may be anhydrous sodium sulphate. Also claimed are a method of preparing the composition and a detergent product comprising the composition enclosed in a poly vinyl alcohol sachet. The composition may provide improved bleach stability and reduced sedimentation on storage.

Description

Dishwashing Detergent Gel Comprising Bleach

TECHNICAL FIELD OF THE INVENTION

The present invention relates to a Dishwashing detergent gel comprising bleach. More particularly, the invention relates to a detergent gel comprising:

Glycerol;

Inorganic bleaching agent; and

Gelling agent.

The dishwashing composition of the present invention provides one or more of a stable inorganic bleach detergent composition; a stable suspension of solid inorganic bleach in liquid gel detergent composition and a more storage stable or better dispensing inorganic bleach detergent composition in the form of the composition enclosed in a water-soluble sachet.

BACKGROUND OF THE INVENTION

Detergent formulations typically contain a number of different active components, including surfactants, builders, enzymes and bleaching agents.

WO2017148990 discloses a detergent composition comprising a fluid phase and suspended particles, wherein the fluid phase comprises water, glycerol, builder and structuring biopolymer.

WO2017153528 discloses a pourable detergent suspension comprising a bleaching agent and bleach catalyst.

EP-A 1 129 160 discloses liquid aqueous cleaning compositions containing water, glycerol, builder, enzyme and thickener.

WO 2013/092276 discloses a detergent formulation containing GLDA, water, citric acid, nonionic surfactant, coated spray-dried percarbonate, manganese catalyst granule and other ingredients.

WO 2014/107578 discloses s detergent compositions containing water, glycerol, polyaminocarboxylic acid (chelating agent) and nonionic surfactant.

WO 2008/064935 discloses a method for producing bleach catalyst granules comprising.

DE-A 10 2014 212643 discloses a liquid detergent composition comprising a solid enzyme formulation.

Liquid detergent formulations offer the advantage over powdered formulations that they can be easy to dose, may contain higher concentrations of active ingredients per unit volume and are more easily dispersed into water. However, they are difficult to formulate with a stable bleaching agent. In order to provide liquid, particularly dishwashing, detergent compositions that deliver cleaning, spotting and filming performance equivalent to that of a powdered formulation it is required to include components that remain undissolved in the liquid product matrix. These undissolved components, such as in the form of discrete particles, are best homogeneously suspended throughout the liquid to guarantee consistent. Although this may be realised by instructing the user to shake the product before use, it is preferable to provide the liquid detergent formulation in the form of a suspension that remains stable during the lifecycle of the product. This is particularly so for sachets and low ullage bottles as the lack of any air pocket reduces mixing on shaking. Such stability, is however, very difficult to achieve as suspensions demix over time because suspended particles are subject to sedimentation, syneresis and creaming or floating phenomena.

Detergent formulations typically contain a number of different active components, including surfactants, builders, enzymes and bleaches. Surfactants are used to emulsify oily components and to disperse solids particles in water during washing. In dishwashing, surfactants also provide de-wetting effects to give shiny and dry dishes at the end of washing. Enzymes act to degrade proteins and lipids into more soluble components hydrolysis.

Bleaches are available in many forms and serve to oxidise materials, laundry and dishes not generally being significantly oxidised, and hence soil components to be removed on cleaning are preferentially degraded and, becoming more soluble are more easily removed in the cleaning process. A bleach may comprise a primary source of oxidising agent and a supplementary agent to reduce the activation energy of the bleaching reaction. Examples being percarbonate and tera acetyl ethylene diamine.

Bleaches of whatever type, at least in their active forms, degrade in the presence of water - which is necessary for their activity in a wash - on storage before washing. Since completely anhydrous compositions are expensive and energy intensive to make and will adsorb water on storage in most packaging formats there is an ongoing need to provide storage stable yet wash active bleach containing detergents.

The problem is greater in liquids compositions as many of the complex mix of components used in formulating detergents are provided in water containing forms or, if not, in particle sizes that need comminution before being small enough to be dispersible and suspendable in a liquids composition. Hence the inorganic bleaches, such as the persalts present a particular problem but are desirable due to their weight effectiveness and dual action in providing alkalinity in a wash to enhance soil suspension.

SUMMARY OF THE INVENTION

The present invention in its various aspects is as set out in the appended claims.

The present invention provides: a non-aqueous liquid detergent composition, the composition comprising:

a fluid continuous phase comprising: more than 50% by weight glycerol; between 1 and 3% sodium sulphate; less than 1 % by weight water;

a suspended solid phase; the phase comprising:

an oxygen bleach providing between 0.2 and 5% available oxygen; and anhydrous sodium sulphate.

A non-aqueous liquid is a liquid in which water not bound to a solid phase is less than 1 % by weight of the liquid phase. This is determined by centrifugation and KarlFisher titration of the continuous phase. The

The fluid of the continuous phase is a liquid. The liquid comprises more than 50% by weight glycerol andless than 1% by weight water. This fluid preferably comprises 90% glycerol, more preferably more than 92% glycerol, optionally more than 95% glycerol. This fluid preferably comprises less than 99% glycerol, more preferably less than 98% glycerol, most preferably less than 95% glycerol. The fluid continuous phase comprises dissolved solids. For these purposes polymers are considered as solids. The dissolved solids comprise between 1 and 3% sodium sulphate. Sodium sulphate provides a saturated solution in commercial grade glycerine at about 10.1 g/l. In a fully formulated detergent composition a solubility of about 12.5 g/l can occur. To be saturated a solution must be in equilibrium with undissolved solids.

Unlike known compositions, the sodium sulphate is present as a saturated solution. The solution is therefore in equilibrium with solid anhydrous sodium sulphate to maintain that saturated solution. Given the relatively high solubility of sodium sulphate in glycerol this cannot be achieved with small amounts of coating materials. Indeed, bleach granules stabilised with sodium sulphate, whilst effective in air are ineffective in glycerol as the sulphate dissolves away leaving the bleach exposed to any ambient water/water ingress. The composition of the present invention provides a more bleach stable composition as a result.

The composition of the present invention comprise oxygen bleach providing between 0.2 and 5% available oxygen, as calculated below. This oxygen bleach is preferably in the form of a granule. The granule preferably comprises stabilising components and in particular anhydrous sodium sulphate. The use of a saturated sodium sulphate solution is thought to serve to stop the sulphate in the granule being dissolved away and the protection lost for the bleach. Hence, incoming moisture must first pass the physical and chemical barrier of anhydrous sodium sulphate, as opposed to randomly encountering either the sulphate or the bleach.

The following compositions were prepared (50g of liquid, 10g of solid and left exposed in a 70% RH environment at 20°C for 1 week. A control with glycerol and a closed vessel gave no appreciable decomposition. Decomposition is means appreciable loss of available oxygen. Stable means low loss of available oxygen. Using a 10% by weight sodium percarbonate suspension of 100pm granules.

Continuous phase ->	Glycerol	Glycerol + 1 % water	Glycerol + 1% water; saturated sodium sulphate solution	Detergent composition 1
Sodium Percarbonate	Decomposition	Decomposition	Stable	Decomposition
Sodium Percarbonate with sodium sulphate coating	Stable	Decomposition	Decomposition	Stable

A granule is a solid particle of size between 1 and 1000pm. preferably between 2 and 100pm. Size may be determined by light microscopy. Size is preferably determined using a Malvern™ mastersizer particle size analyser. In case of doubt particle size is the D3,2 particle size measure. The saturated sodium sulphate solution is in equilibrium with 1% anhydrous sodium sulphate solid.

The composition when prepared is preferably prepared using only sodium sulphate in the anhydrous form. However, practical considerations allow that up to 10% of the sodium carbonate may be hydrated.

The composition, as a whole, may comprise from 1 to 10% by weight water. To remain stable this water is present as water of crystallisation, for example, primarily as water of crystallisation of the sodium sulphate. Water bound to the dissolved sodium sulphate is for the purposes of this document termed water of crystallisation. The presence of water may due to moisture in the raw material or because of deliberate inclusion so as to assist in structuring the liquid, such as to hinder sedimentation of the solids in the fluid.

Between 100% and 50% of the sodium sulphate present in the composition may be anhydrous sodium sulphate, preferably between 95% and 70% most preferably between 80% and 90%. Some hydration is desirable as the hydrated salt appears to promote suspension stability. Over time on storage in the presence of ambient moisture the amount of hydrated material will increase and the level of hydrated sulphate will increase, this percentage is therefore the initial percentage. However, initial a portion of the sulphate may be hydrated, either due to moisture in the raw material or because of deliberate inclusion so as to assist in structuring the liquid.

The composition may comprise an alkaline agent capable of neutralising at least 0.1 mol of hydrogen ions per 100g of composition. Sodium percarbonate may constitute that agent as well as being the bleach.

The composition of the present invention may be used as part of a packaging system. Specifically, the composition may be used in the form of a water-soluble pouch, the pouch comprising a water-soluble film containing the composition of the present invention. A specific advantage of the present invention is the improved stability of the bleach means that there is negligible release of oxygen gas due to decomposition in the bleach. Such release of gas in a pouch, which is a sealed vessel, on gives rise to splitting or bursting. The present invention therefore provides a detergent product in the form of the composition of the present invention encapsulated in a water-soluble film in the form of a pouch. A pouch will typically hold between 5 and 200 ml_ of the composition, more preferably between 20 and 100 mL. The volume of the pouch is significant as the surface area to volume ratio changes radically with pouch size. Larger pouches have proportionally less surface and are more prone to breakage whereas smaller pouches are less prone but may not convey sufficient material in a single pouch to undertake a normal detergent wash, such as for automatic dishwashing machine. It would also appear that the sodium sulphate when present as particles in the bulk of the continuous phase (as opposed to being combined with any other specific granule in localised form) give some degree of protection for the PVA film from softening due to hydration over time. This can be particular problematic due to storage in a humid environment. Softened PVA films can give rise to breakage of the pouch, such as when picked up by a consumer.

A further advantageous product form is in the form of a Tottle, otherwise known as a bottle configured to be sold in what would normally be considered an inverted form. The evolution of gas from a bleach containing composition in this product form forces the contents of the Tottle out of the container, which is undesirable. The present invention therefore gives a preferred detergent product in the form of a Tottle in combination with the composition of the present invention. The Tottle is desiable as the rate of moisture ingress is reduced by liquid sealing the outlet of the vessel, in use this liquid tends to harden (localised ‘drying’) and provide an effective seal.

A composition of the present invention comprises a detergent component to provide a source of alkalinity.

Sodium Sulphate Coarse, Anhydrous present in the composition in the physical form of suspended Particles. A specific commercially available material fulfilling the requirements being SODIUM SULFATE ANH T350 (MINERA SANTA MARTA) this may be present in the range 1 to 20%, preferably 5 To 15%, most preferably in the range 5 to 10%.

A composition of the present invention comprises a detergent component to provide an inorganic bleach.

The preferred inorganic bleach is Sodium percarbonate. Various proprietary materials are available, a material having an available oxygen of 12% or higher is preferred. The inorganic bleach is present in the composition in the physical form of Suspended particles. A specific commercially available material fulfilling the requirements being available from Solvay. The sodium percarbonate is preferably present in the range 10% To 30%; more preferably 15% To 25%; most preferably between 16% and 18%.

A composition of the present invention comprises a detergent component to provide a source of alkalinity. The preferred material is Sodium carbonate dense, Anhydrous present in the composition in the physical form of suspended particles. A specific commercially available material fulfilling the requirements being SODIUM CARBONATE SD (NOVACARB). The sodium carbonate is preferably present at between 1 and 10%, preferably between 1 and 5%.

A composition of the present invention comprises a detergent component to act as a builder. The commonly known builders are within the scope of the present invention. The preferred builder of the present invention is tri-Sodium Citrate, Anhydrous present in the composition in the physical form of Suspended particles. A specific commercially available material fulfilling the requirements being TSA F6000 (JUNGBUNZLAUER). The builder may be present in the composition in the range 10% To 30%, Preferably 15% To 25%; and most preferably 18 to 20%.

A composition of the present invention comprises a detergent component to act as a surfactant. The commonly known surfactants are within the scope of the present invention. The preferred surfactant of the present invention is a non-ionic surfactant. The nonionic surfactant is preferably a low foaming non-ionic surfactant. The surfactant is preferably an alcohol ethoxylate surfactant.

Nonionic surfactant present in the composition in the physical form of a Liquid. A specific commercially available material fulfilling the requirements being GENAPOL EC50 (CLARIANT). If present, the surfactant is present in the range 0.5 to 10%, preferably in the range 0.5 to 5%.

A composition of the present invention comprises a detergent component to provide a bleach activator. The commonly known breach activators are within the scope of the present invention. The preferred breach activator of the present invention is TAED.

A composition of the present invention comprises a detergent component to provide a bleach catalyst. The commonly known bleach catalysts are within the scope of the present invention. The preferred bleach catalyst of the present invention is MnTACN.

The breach activator and bleach catalyst are preferably present as a TAED/MnTACN Co-Granule. This is preferably a Polyvinyl Alcohol Coated co-granule present in the composition in the physical form of Suspended particles. A specific commercially available material fulfilling the requirements being PERACTIVE FDOX-P (WEYLCHEM). This is preferably present at between 1 and 15%, preferably between 1 and 10% most preferably between 2 and 5%.

A composition of the present invention comprises a detergent component to provide enzymes.

A preferred enzyme is a Protease Enzyme present in the composition in the physical form of Suspended particles. A specific commercially available material fulfilling the requirements being EXCELLENZ P1000 (DUPONT). This enzyme is preferably present at a level of between 0.1 and 10%, more preferably between 0.2 and 5%.

A further preferred Amylase Enzyme present in the composition in the physical form of Suspended particles. A specific commercially available material fulfilling the requirements being EXCELLENZ S2000 (DUPONT). This enzyme is preferably present at a level of between 0.1 and 10%, more preferably between 0.2 and 5%.

A composition of the present invention may further comprise a number of subsidiary components such as:

a metal corrosion inhibitor. A suitable material is available as Benzotriazole, such is dissolved in honour surfactant, present in the composition in the physical form of a liquid. A suitable material being DEHYPON E126 TT (BASF). This material is preferably present at between 0.1 and 2%, more preferably between 0.2 and 1%.

A composition of the present invention comprises a detergent component to provide a liquid continuous phase. The liquid continuous phase primary component of the present invention is Glycerol. A suitor material is GLYCERINE 99% (OLEON) this is present between 30 and 70%, preferably between 40 and 60%, preferably between 50 and 56%.

A composition of the present invention comprises a detergent component to provide suspension stabilisation, this can take several forms:

a polymer to adsorb on suspended particles and provide electrostatic charge to provide into particle repulsion and promote stabilisation of the suspension. A suitable material being a sulphonate modified polycarboxylate. A suitable material being SOKALAN CP50 (BASF). This is preferably present, as active between 1 and 15%, preferably between 2 and 10%, most preferably between 4 and 8%.

A polymer to act as an associative thickener to provide a network within the liquid continuous phase to increase the effective viscosity of that continuous phase. An example being a Cellulose Derivate such as available from (CP KELCO) such material may be present between 0.1 and 15%, most preferably between 0.2% and 1%, most preferably between 0.4 and 0.6%.

A polymer to thicken the liquid continuous phase by forming an effective solution and increasing the liquid. A suitable thickener being Xanthan Gum, understood to be an associative thickener. A suitable commercial material is available as KELCOVIS DG (CP KELCO).

EXPERIMENTAL

The framework composition 1 as set out below was prepared:

Table 1

DESCRIPTION	PHYSICAL FORM	PROTOTYPE SAMPLE C LEVEL OF INCLUSION (parts)
Sodium carbonate dense, Anhydrous	Suspended particles	3.5
Sodium sulphate coarse, Anhydrous	Suspended particles	5
Tri-sodium citrate, Anhydrous	Suspended particles	20
Sodium percarbonate, coated 12,4% Avox	Suspended particles	15
Xanthan Gum	Liquid @ RT	0.04
Glycerol	Liquid (a) RT	55.96
Sodium DTPM Phosphonate 33%	Liquid @ RT	0.5

The composition was prepared using a low shear mixer with the following order of addition:

Process of manufacture. No high shear needed.

a. Glycerine and Xanthan Gum under moderate agitation

b. Further liquids - none in this example

c. Agitation stopped. The viscosity network takes 1 hour to build up the viscosity.

d. Low/Moderate agitation add anhydrous sodium sulphate.

e. Low/Moderate agitation add Carbonate/HEDP granule/Citrate granule/Dye

f. DTPMP liquid to ensure any transition metal is sequestrated.

g. Wait 15 min to allow sequestration (Traces of transition metal catalyses the decomposing of H2O2).

h. Add any bleach activator or catalyst - none in this example

i. Control pH to ph1O using sodium carbonate/citric acid if required.

j. Add the enzyme granules - none in this example

k. Any other components- none in this example

l. Add the Coated percarbonate granule.

Comparative composition 2 does not include sodium sulphate. Citrate and carbonate increased in proportion.

All percentages in the composition in this document are percentages by weight.

the above composition was prepared as follows:

After leaving for 24 hours the viscosity of the prepared product was checked using a Brookfield LVF-04viscometer with spindle 4. The shear rate was variable with a measurement interval 1 minute between readings

The following tests were performed on the Compositions 1 and 2.

Product viscosity Table 2

Speed (rpm)	Viscosity (cPs)
	Acceleration	Deceleration
0.3	260000	244000
0.6	220000	182000
1.5	162000	131000
3.0	126000	104000
6.0	97000	93000
10.0	EE	EE

The results are shown in Figure 5.

This shows that the sodium sulphate contributes to structuring the liquid composition of the invention. It is believed that this contributes towards the stability of the composition against sedimentation and syneresis.

Bleach stability

Method

Parameters for calculation to determine the amount of Percarbonate or Perborate in a detergent product.

Percarbonate has the formula 2Na2CO3, SHaChand contains 13.5% active oxygen. Perborate, of formula NaBCh, nhhO, tends to disappear because it is harmful for the environment. This can be:

- monohydrate when n ~ 1, it then contains 15% of active oxygen

- Tetrahydrate when n = 4, it then contains 10% of active oxygen.

Samples of the composition were taken at regular intervals as listed in the data table and titrated with potassium permanganate solution using the following procedure. 4 g of composition are placed into a 600 mL Erlenmeyer flask. Add 200 mL of demineralized water and 20 mL of 25% sulfuric acid. Homogenize the solution. Titrate immediately with KMnO4 until pink (MnO⁴' is then in excess because H2O2 has been completely consumed); the coloring should persist for 30 seconds with stirring. This is the end point for the titration. In which P is the test sample in g and V_eq: volume of KMnO4 at L equivalence.

2MNO₄- + 5H₂O₂ + 6H⁺ 2MN²⁺ + 8H2O + 5O₂

Available oxygen is calculated as follows :

n(O₂) = n(H₂O₂) = 5/2 n(Mn²⁺) or n(Mn²⁺) = C(KMnO₄) * V_eq

From which :

n(O₂) = 5/2 * C(KMnO₄) * V_eq and :

m(O₂) = 5/2 * C(KMnO₄) * V_eq * M(O₂); avec M(O₂) = 32 g.mol·¹

Hence :

%O₂ = (5/2 * C(KMnO₄) * V_eq * M(O₂) * 100) / P %O₂ = (5/2 * 0.2 * V_eq * 32 * 100) I P

Avox =% 0 active SO Avox =% O₂12

Avox = (800 * Veq) I P

Composition 1 according to the present invention- Results shown graphically in

Figures 1 and 2

Values of Residual available Oxygen - Tables 3 to 9

RT	Value 1	Value 2	Average	Residual Avox
0	1.98	2.00	1.99	100.0 %
2	1.95	1.95	1.95	98.0
4	1.92	1.92	1.92	96.5
6	1.90	1.89	1.90	95.2
17	1.88	1.86	1.87	94.0

40°C	Value 1	Value 2	Average	Residual Avox %
0	1.98	2.00	1.99	100.0
2	1.95	1.92	1.94	97.2
4	1.90	1.91	1.91	95.7
6	1.87	1.90	1.89	94.7
17	1.76	1.77	1.77	88.7

4°C			Average	Residual Avox %
0	1.98	2.00	1.99	100.0
2	1.95	1.96	1.96	98.2
4	1.94	1.95	1.95	97.7
6	1.95	1.92	1.94	97.2
17	1.93	1.90	1.92	96.2

io

Comparative composition 2 - Results shown graphically in Figures 3 and 4

Residual Av Ox

20°C	Value 1	Value 2	Average	Residual Avox %
0	2.41	2.33	2.37	100.0
2	2.00	2.06	2.03	85.5
5	1.91	2.01	1.96	82.6
7	1.87	2.00	1.94	81.6
9	1.88	1.90	1.89	79.7
11	1.90	1.91	1.91	80.4
17	1.87	1.85	1.86	78.5

40°C	Value 1	Value 2	Average	Residual Avox %
0	2.41	2.33	2.37	100.0
2	1.96	1.89	1.93	81.3
5	1.76	1.82	1.79	75.4
7	1.86	1.78	1.82	76.8
9	1.88	1.72	1.80	75.9
11	1.85	1.81	1.83	77.2
17	1.84	1.80	1.82	76.8

4°C	Value 1	Value 2	Average	Residual Avox %
0	2.41	2.33	2.37	100.0
2	2.17	2.10	2.14	90.1
5	1.99	2.20	2.10	88.4
7	1.99	2.00	2.00	84.2
9	1.99	1.95	1.97	83.1
11	1.95	2.00	1.98	83.3
17	1.98	1.92	1.95	82.3

This shows that sodium sulphate anhydrous stabilises the sodium percarbonate in the composition of the invention. Similar results are observable with perborate in place of percarbonate.

The test Composition 1 according to the present invention using was repeated at 20°C and analysed after 6 days with various levels of water being introduced with gentle mixing. The results are shown in Figure 6.

This shows that the composition of the present invention has high bleach stability until the sodium sulphate has been saturated.

Storage stability against sedimentation

The composition shown in Figure 6 was observed to show sedimenttion over time by measuring syneresis. 150ml of the compositions were placed in 200ml measuring cylinders with a sealed top to stop water ingress and the level of syneresis, the height of clear(er) liquid at the top of the liquid column was measured. Provisional results on samples (from left to right as 1 to 8, in the graph) are:

Table 10

Sample	Syneresis
1	<5mm
2	<1mm
3	<1mm
4	None
5	None
6	None
7	None
8	<1mm

It appears that some water serves to structure the composition and reduces syneresis. This phenomena was not observed fior the equivalent composition without anhydrous sodium sulphate.

Fully formulated composition 3, according to the present invention - Table 11

DESCRIPTION	FUNCTION	LEVEL OF INCLUSION (%)
Sodium carbonate dense, Anhydrous	ALKALIN AGENT - QSP pH ENHANCER	3.50
Sodium sulphate coarse, Anhydrous	FILLER - CAPTURE FREE WATER	5.00
Tri-sodium citrate, Anhydrous	BUILDER	20.00
Nonionic surfactant	SURFACTANT	3.74
TAED/Mn-TACN co-granule, polyvinyl alcohol coated	BLEACHING ACTIVATOR & BLEACHING CATALYST	2.00
Protease enzyme	ENZYME	1.00
Amylase enzyme	ENZYME	0.50
Sodium percarbonate, coated 12,4% Avox	BLEACHING SOURCE	16.00
Sodium polycarboxylate, modified 40% active	DISPERSING POLYMER	6.00
Nonionic surfactant & Benzotriazole	SURFACTANT AND METAL CORROSION INHIBITOR	0.50
Cellulose derivate 0,5% solution in propylene glycol	SUSPENSING AGENT	5.00
Xanthan Gum		0.04
Sodium HED Phosphonate 85%	CA/MG SEQUESTRING AGENT	4.40
Dye solution	DYE	0.25
Glycerol	SOLVENT	31.43
Sodium DTPM Phosphonate 33%	STABILIZER	0.50
Perfume	PERFUME	0.18

100.00

This composition showed bleach and storage stability substantially the same as for the test composition 1.

The fully formulated composition was prepared using a low shear mixer with the following order of addition:

Process of manufacture. No high shear needed.

m. Glycerine and cellulose under moderate agitation

n. All Liquids under low agitation

o. Agitation stopped. The Cellulose network takes 1 hour to build up the viscosity.

p. Low/Moderate agitation Add sodium sulfate to further dehydrate the liquid Something different from UL IP

q. Low/Moderate agitation Carbonate/HEDP granule/Citrate granule/Dye

r. DTPMP liquid to ensure any transition metal is sequestrated.

s. Wait 15 min to allow sequestration (Traces of transition metal catalyses the decomposing of H2O2). Something different from UL IP

t. Add the coated granule of MN TACN catalyst

u. Control pH

v. Add the enzyme granules

w. Any other components

x. Add the Coated percarbonate granule.

Properties pH 1% = 10.60

Viscosity Brookfield Spindle LVF 3/ speed 0.3) = 158000 - Tooth paste liquid still fluid

Specific Gravity = 1.44 g/mL

Comparative composition 4 following WO 2017/148990. This showed resuced chemical and physical stability as compared to the compositions of the present invention.

Claims

1. A non-aqueous liquid detergent composition, the composition comprising:

a fluid continuous phase comprising:

more than 50% by weight glycerol;

between 1 and 3% sodium sulphate; and less than 1 % by weight water;

a suspended solid phase; the phase comprising:

2. The composition of claim 1 wherein the fluid continuous phase is a saturated solution of sodium sulphate.

3. The composition of claim 1 or claim 2 wherein the oxygen bleach is present as a granule comprising anhydrous sodium sulphate.

4. The composition of claim 3, wherein the granule has core of oxygen bleach and an outer coating comprising the anhydrous sodium sulphate.

5. The composition of claim 3 of claim 4 wherein the oxygen bleach is sodium percarbonate.

6. The composition of any preceding claim wherein the composition, as a whole, comprises from 1 to 10% by weight water.

7. The composition of claim 6 wherein the water is present as water of crystallisation of the sodium sulphate.

8. The composition of any preceding claim wherein the sodium sulphate is present between 1 and 15% of the composition.

9. The composition of claim 8 wherein between 100 and 90% of the sodium sulphate is present as anhydrous sodium sulphate.

10. A method of preparing a non-aqueous liquid detergent composition, the composition comprising:

a fluid continuous phase comprising:

more than 50% by weight glycerol;

between 1 and 3% sodium sulphate;

less than 1 % by weight water;

a suspended solid phase; the phase comprising:

an oxygen bleach providing between 0.2 and 5% available oxygen;

anhydrous sodium sulphate; the method having the steps:

i) mixing the liquid components of the composition;

ii) adding anhydrous sodium sulphate with mixing;

iii) the sodium sulphate being added until the solution is a saturated sodium sulphate solution;

iv) adding further anhydrous sodium sulphate until, at equilibrium, anhydrous sodium sulphate is present;

v) adding an oxygen bleach granule providing between 0.2 and 5% available oxygen to the composition.

11. The method of claim 12 wherein the oxygen bleach granule comprises anhydrous sodium sulphate.

12. The method of claim 10 or claim 11 wherein the oxygen bleach is sodium percarbonate.

13. The method of claim 11 or claim 12, wherein the granule has a core of oxygen bleach and an outer coating comprising the anhydrous sodium sulphate and the mixing does not significantly reduce the particle size of the granules.

14. The method of any of claims 10 to 13 wherein any addition components of the composition, are added after step iv).

15. A detergent product comprising the composition of any of claims 1 to 9 enclosed in a water-soluble poly vinyl alcohol sachet comprising.