EP3596194A1 - Complex capsule-in-capsule detergent - Google Patents

Complex capsule-in-capsule detergent

Info

Publication number
EP3596194A1
EP3596194A1 EP18722251.8A EP18722251A EP3596194A1 EP 3596194 A1 EP3596194 A1 EP 3596194A1 EP 18722251 A EP18722251 A EP 18722251A EP 3596194 A1 EP3596194 A1 EP 3596194A1
Authority
EP
European Patent Office
Prior art keywords
range
capsule
phase
sodium
foil
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
Application number
EP18722251.8A
Other languages
German (de)
French (fr)
Other versions
EP3596194B1 (en
Inventor
Zbigniew BABELEK
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Octagon International Trade Zbigniew Babelek
Original Assignee
Octagon International Trade Zbigniew B Belek
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Octagon International Trade Zbigniew B Belek filed Critical Octagon International Trade Zbigniew B Belek
Publication of EP3596194A1 publication Critical patent/EP3596194A1/en
Application granted granted Critical
Publication of EP3596194B1 publication Critical patent/EP3596194B1/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

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
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0039—Coated compositions or coated components in the compositions, (micro)capsules
    • 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
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/04—Detergent materials or soaps characterised by their shape or physical properties combined with or containing other objects
    • C11D17/041—Compositions releasably affixed on a substrate or incorporated into a dispensing means
    • C11D17/042—Water soluble or water disintegrable containers or substrates containing cleaning compositions or additives for cleaning compositions
    • C11D17/045—Multi-compartment
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/37—Polymers
    • C11D3/3703—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C11D3/3707—Polyethers, e.g. polyalkyleneoxides
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/37—Polymers
    • C11D3/3746—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C11D3/3753—Polyvinylalcohol; Ethers or esters 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
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/38—Products with no well-defined composition, e.g. natural products
    • C11D3/384—Animal products
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/38—Products with no well-defined composition, e.g. natural products
    • C11D3/386—Preparations containing enzymes, e.g. protease or amylase

Definitions

  • the two-phase laundry agents currently available on the market are constructed such that the components are placed in separate chambers which undergo dissolution/activation simultaneously, independently of each other.
  • the delay in adding the enzymes to wash causes that the enzymes released from the inner phase start affecting the articles which were already wetted with the detergent base. Due to this fact, the enzymes function significantly better.
  • a process of producing the complex detergent comprises producing an inner phase comprising enzymes or percarbonate and TAED, or another component in a liquid form or a solid form, e.g. powder or granules.
  • an inner phase comprising enzymes or percarbonate and TAED, or another component in a liquid form or a solid form, e.g. powder or granules.
  • a membrane element for said inner phase a PVOH foil or other material which dissolves in contact with water is used.
  • the time of dissolution of the smaller inner phase is delayed in relation to the time of dissolution of the outer phase by means of using a proper thickness of coating of the smaller capsule.
  • the thicker the capsule coating the longer the dissolution time.
  • Example 1 is presented ranges of mass concentrations of the used components of the individual phases of the complex detergent as well as examples of carrying out the invention.
  • a method of producing a capsule-in-capsule (PEG + granulated enzymes)
  • a method of producing a multicompartment capsule-in-capsule comprising one or more inner compartments and one outer compartment, wherein the outer compartment surrounds 100% of the outer surface of the inner compartment(s), completely surrounded with at least one layer which dissolves in contact with water, characterized in that it comprises the stages of:
  • a method of producing a multicompartment capsule-in-capsule comprising one or more inner compartments and one outer compartment, wherein the outer compartment surrounds 100% of the outer surface of the inner compartment(s), completely surrounded with at least one layer which dissolves in contact with water, characterized in that it comprises the stages of:
  • a complex capsule-in-capsule detergent was obtained according to Example 1
  • a complex capsule-in-.capsule detergent was obtained according to Example Outer liquid phase
  • a complex capsule-in-capsule detergent was obtained according to Example 3 Outer powder phase
  • a complex capsule-in-capsule detergent was obtained according to Example 4 Outer powder phase
  • a complex capsule-in-capsule detergent was obtained according to Example 1
  • a complex capsule-in-capsule detergent was obtained according to Example 2
  • a complex capsule-in-capsule detergent was obtained according to Example 4 Outer phase/powder Content [%]

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)
  • Zoology (AREA)
  • Detergent Compositions (AREA)
  • Cosmetics (AREA)

Abstract

A complex capsule-in-capsule detergent characterized in that it consists of at least two phases: an inner phase and an outer phase separated from each other with an inner foil, while the outer phase is surrounded with an outer foil, wherein the inner phase comprises active substances. A method of producing the multicompartment capsule-in-capsule comprising one or more inner compartments and one outer compartment, which dissolves in contact with water, the method comprising: a) producing the smaller capsule coated with PVOH or gelatin, then placing PEG400 mixed with liquid or granulated enzymes in it; b) forming the larger capsule of PVOH foil by vacuum forming and sealing methods.

Description

Complex capsule-in-capsule detergent
The invention relates to a complex capsule-in-capsule detergent comprising at least two phases separated with an inner foil, a method of producing thereof, and use of the capsule-in-capsule detergent as laundry detergent or dishwasher detergent.
There are known many kinds and solutions of detergent formulations for household use. However, consumer requirements are constantly rising as regards the effectiveness of such agents, convenience of use and reliability. The users complain about the ineffectiveness of the used agents as regards their ability to remove dirt or to provide the desired visual and palpatory effect. Additionally, the used agents may cause possible occurrence of stains and discoloration. As results from a series of experiments and information delivered by the enzymes producers, there is a serious problem related to the time of release of the active substances from detergent formulations. It is known that when enzymes and other active substances are included in a detergent base, i.e. a mixture of surface-active compounds showing a synergic effect in wash, they lose about 20% of their effectiveness after 8 weeks, but if they are introduced to wash separately, excluded from the detergent base, they retain their activity for a long time.
Although the currently used solutions take into account the problem of separating the component groups, the two-phase laundry agents currently available on the market are constructed such that the components are placed in separate chambers which undergo dissolution/activation simultaneously, independently of each other.
There are no two-phase systems which enable controlling the dissolution time of particular components, so that the agents are activated gradually, as required by the cleaning stage, supporting further stages and simultaneously preventing undesired interactions. A multi-compartment system constructed in such way enables dosing of individual components or component groups from the base, such that the'¾e*mi£al mixture contained in the base would not have a negative influence on said component or component group, for example would not cause premature degradation. Surprisingly, the present solution solves the problems experienced by the users and provides an effective and reliable washing agent fulfilling those needs.
The subject-matter of the invention is a complex capsule-in-capsule detergent, which consists of at least two phases: an inner phase and an outer phase separated from each other with an inner foil while the outer phase is surrounded with an outer foil, wherein the inner phase comprises active substances, especially selected from: enzymes, bleaching agents, especially percarbonate and tetraacetylethylenediamine (TAED), and other active agents. Preferably, the foil is made of polyvinyl alcohol, gelatin, polyacrylamide or hydroxypropylcellulose. The thickness of the inner foil is greater than the thickness of the outer foil, preferably the inner foil has thickness ranging from 90 μηι to 1 mm and the outer foil has thickness ranging from 60 μιτι to 90 μιη.
In a preferred variant of the complex detergent the outer phase is a liquid phase and the inner phase is a liquid phase or the outer phase is a liquid phase and the inner phase is a solid phase in the form of powder or granulate. In a preferred embodiment the agent of the invention comprises a solid outer phase in the form of powder or granulate and an inner liquid phase, more preferably the inner phase comprises percarbonate and TAED in powder form .
The subject-matter of the invention is also a complex capsule-in-capsule detergent according to any of claims 1-7 for use in washing fabrics or for use in a dishwasher.
The foil is made of PVOH (i.e. polyvinyl alcohol), gelatin, or other material which dissolves in contact with water, such as e.g. Polyacrylamide, hydroxypropylcellulose.
In a particular embodiment, the subject-matter of the invention is a complex capsule-in- capsule laundry detergent comprising a chemical mixture according to the enclosed specification, which has an inner phase comprising enzymes, or percarbonate and TAED, or two capsules simultaneously, one comprising enzymes and the other one e.g. percarbonate and TAED, or some other component which if placed in the base would undergo degradation due to negative influence of the base.
In a particular embodiment, the subject-matter of the invention is a complex capsule-in- capsule detergent for dishwashers. A preferred complex capsule-in-capsule dishwasher detergent preferably comprises an outer liquid phase and an inner liquid or solid phase - in the form of powder or granules.
In the solution according to the invention the enzymes comprised in the inner phase are added to wash with a predetermined delay, from 1 to 5 minutes in relation to the detergent base, which can be controlled with the use of a modified separating foil. A 90 μιη thick foil, for example, will dissolve within about 1-1.5 minutes while a 500 μηι foil will dissolve within about 4-5 minutes.
The delay in adding the enzymes to wash causes that the enzymes released from the inner phase start affecting the articles which were already wetted with the detergent base. Due to this fact, the enzymes function significantly better.
In an another embodiment, the percarbonate and TAED present in the inner phase are in the form of powder. Such form of washing agents provides a delayed release of percarbonate and TAED from the inner phase. The time of adding percarbonate and TAED to wash can be controlled by adjusting the thickness of the foil surrounding the inner phase. This enables use of a solution that delays adding percarbonate and TAED to an already ongoing washing process with the detergent base.
A process of producing the complex detergent comprises producing an inner phase comprising enzymes or percarbonate and TAED, or another component in a liquid form or a solid form, e.g. powder or granules. As a membrane element for said inner phase a PVOH foil or other material which dissolves in contact with water is used.
Next, the inner phase protected with the inner foil is introduced into the outer phase; alternatively two or more separate inner phases comprising active substances are used. The inner phase can be liquid or solid (powder), the outer phase can be liquid or solid as well, so that both phases are liquid or both phases are solid or a part of the phases is liquid and part is solid. The outer phase is then sealed with the outer foil. The manufactured product is a complex detergent, comprising at least two phases, each of which is surrounded by a foil. The foil is made of PVOH or other material that dissolves in contact with water.
The time of dissolution of the smaller inner phase is delayed in relation to the time of dissolution of the outer phase by means of using a proper thickness of coating of the smaller capsule. The thicker the capsule coating, the longer the dissolution time.
Below are presented ranges of mass concentrations of the used components of the individual phases of the complex detergent as well as examples of carrying out the invention. Example 1
A method of producing a capsule-in-capsule (PEG + liquid enzymes)
A method of producing a multicompartment capsule-in-capsule comprising one or more inner compartments and one outer compartment, wherein the outer compartment surrounds 100% of the outer surface of the inner compartment(s), completely surrounded with at least one layer which dissolves in contact with water, characterized in that it comprises the stages of:
a) producing the smaller capsule, whose coating is PVOH foil or gelatin, and then placing a non-ionic surfactant PEG400 mixed with liquid enzymes in it;
b) forming the larger capsule of PVOH foil, wherein in the forming process the foil is sucked in to the sockets in a forming drum to create a hollow coated with the PVOH foil, and then using feeders to place in said hollow the smaller capsule obtained in stage a), after which the larger capsule, in which the smaller capsule is already placed, is filled with a liquid whose possible composition is presented in further examples, which completes the whole capsule formulation, and then the hollow is sealed with a second foil to form the finished product.
Example 2
A method of producing a capsule-in-capsule (PEG + granulated enzymes)
A method of producing a multicompartment capsule-in-capsule comprising one or more inner compartments and one outer compartment, wherein the outer compartment surrounds 100% of the outer surface of the inner compartment(s), completely surrounded with at least one layer which dissolves in contact with water, characterized in that it comprises the stages of: a) producing the smaller capsule, whose coating is PVOH foil or gelatin, and then placing a non-ionic surfactant PEG400 mixed with granulated enzymes in it;
b) forming the larger capsule of PVOH foil, wherein in the forming process the foil is sucked in to the sockets in a forming drum to create a hollow coated with the PVOH foil, and then using feeders to place in said hollow the smaller capsule obtained in stage a), after which the larger capsule, in which the smaller capsule is already placed, is filled with a liquid whose possible composition is presented in further examples, which completes the whole capsule formulation, and then the hollow is sealed with a second foil to form the finished product.
Example 3
A method of producing a capsule-in-capsule (PEG + granulated enzymes)
A method of producing a multicompartment capsule-in-capsule comprising one or more inner compartments and one outer compartment, wherein the outer compartment surrounds 100% of the outer surface of the inner compartment(s), completely surrounded with at least one layer which dissolves in contact with water, characterized in that it comprises the stages of:
a) producing the smaller capsule, whose coating is PVOH foil or gelatin, and then placing a non-ionic surfactant PEG400 mixed with liquid enzymes in it;
b) forming the larger capsule of PVOH foil, wherein in the forming process the foil is sucked in to the sockets in a forming drum to create a hollow coated with the PVOH foil, and then using feeders to place in said hollow the smaller capsule obtained in stage a), after which the larger capsule, in which the smaller capsule is already placed, is filled with a granulate whose possible composition is presented in further examples, which completes the whole capsule formulation, and then the hollow is sealed with a second foil to form the finished product.
Example 4
A method of producing a capsule-in-capsule (PEG + granulated enzymes)
A method of producing a multicompartment capsule-in-capsule comprising one or more inner compartments and one outer compartment, wherein the outer compartment surrounds 100% of the outer surface of the inner compartment(s), completely surrounded with at least one layer which dissolves in contact with water, characterized in that it comprises the stages of:
a) producing the smaller capsule, whose coating is PVOH foil or gelatin, and then placing a non-ionic surfactant PEG400 mixed with granulated enzymes in it;
b) forming the larger capsule of PVOH foil, wherein in the forming process the foil is sucked in to the sockets in a forming drum to create a hollow coated with the PVOH foil, and then using feeders to place in said hollow the smaller capsule obtained in stage a), after which the larger capsule, in which the smaller capsule is already placed, is filled with a granulate whose possible composition is presented in further examples, which completes the whole capsule formulation, and then the hollow is sealed with a second foil to form the finished product.
Dishwasher capsule
Variant 1
A complex capsule-in-capsule detergent was obtained according to Example 1
Outer liquid phase
Inner liquid phase
Example 1A
Outer liquid ph
No. Chemical name Mass %
100,0
1 L-glutamic acid, Ν,Ν-diacetic acid tetrasodium salt 53,1 1 No. Chemical name Mass %
2 Glycerin 15,0
3 Monopropylene glycol 10,0
4 Water 7,5
5 Polycarboxylanes 5,0
6 D-glucopyranose , C8-C10 oligomers, alkyl glycosides 5,0
7 Alcohols, C10-16, etoxylated 2,5
8 Sodium hydroxide 0,5
9 Citric acid 0,5
10 Sodium citrate 0,5
11 1 -octyl-2-pyrrolidone 0,1
12 Fragrance composition "Lemon Ice" 0,1
13 Liquitint Bright yellow 0,1
14 Isocil Ultra 1.5 0,09
Inner liquid phase
Example IB
Outer liquid phase
Lp. Nazwa chemiczna % masowy
100,0
1 L-glutamic acid, Ν,Ν-diacetic acid tetrasodium salt 40,0
2 Glycerin 30,0
3 Monopropylene glycol 20,0
4 Water 10,0
5 Polycarboxylanes 5,0
6 D-glucopyranose , C8-C10 oligomers, alkyl glycosides 5,0
7 Alcohols, C10-16, etoxylated 2,5
8 Sodium hydroxide 1 ,0
9 Citric acid 1 ,5
10 Sodium citrate 0,5 11 1 -octyl-2-pyrrolidone 0,1
12 Fragrance composition "Lemon Ice" 0, 1
13 Liquitint Bright yellow 0,1
14 Isocil Ultra 1.5 0,09
Inner liquid phase
Variant 2
A complex capsule-in-.capsule detergent was obtained according to Example Outer liquid phase
Inner powder phase
Content [%]
No. Chemical name
Min mass % Max mass %
1 Sodium percarbonate 60,0 80,0
2 TAED 20,0 40,0 Example 2A
Outer liquid phase
No. Chemical name Mass %
100,0
1 L-glutamic acid, Ν,Ν-diacetic acid tetrasodium salt 53, 1 1
2 Glycerin 15,0
3 Monopropylene glycol 10,0
4 Water 7,5
5 Polycarboxylanes 5,0
6 D-glucopyranose , C8-C10 oligomers, alkyl glycosides 5,0
7 Alcohols, C10-16, etoxylated 2,5
8 Sodium hydroxide 0,5
9 Citric acid 0,5
10 Sodium citrate 0,5
11 1 -octyl-2-pyrrolidone 0,1
12 Fragrance composition "Lemon Ice" 0,1
13 Liquitint Bright yellow 0,1
14 Isocil Ultra 1.5 0,09
Inner powder phase
No. Chemical name Mass %
100,0
1 Sodium percarbonate 60,0
2 TAED 40,0
Example 2B
Outer liquid phase
No. Chemical name Mass %
100,0
1 L-glutamic acid, Ν,Ν-diacetic acid tetrasodium salt 40,0
2 Glycerin 30,0
3 Monopropylene glycol 20,0
4 Water 10,0
5 Polycarboxylanes 5,0 6 D-glucopyranose , C8-C10 oligomers, alkyl glycosides 5,0
7 Alcohols, C10-16, etoxylated 2,5
8 Sodium hydroxide 1 ,0
9 Citric acid 1 ,5
10 Sodium citrate 0,5
11 1 -octyl-2-pyrrolidone 0,1
12 Fragrance composition "Lemon Ice" 0,1
13 Liquitint Bright yellow 0,1
14 Isocil Ultra 1.5 0,09
Inner powder phase
Variant 3
A complex capsule-in-capsule detergent was obtained according to Example 3 Outer powder phase
Inner liquid phase
Content [%]
No. Chemical name
Min mass % Max mass % 1 Protease 20,0 40,0
2 Amylase 20,0 40,0
3 Propylene glycol 20,0 60,0
Example 3A
Outer powder phase
No. Chemical name Mass %
100,0
1 Sodium chloride 40,0
2 Sodium sulfate 15,0
3 Sodium citrate 15,0
4 Water 0,5
5 Sodium silicate 0,5
6 Alcohols, C10-16, etoxylated 0,5
7 Sodium carbonate 20,0
8 Sodium percarbonate 7,5
9 Polikarboxylanes 0,5
10 Xiameter APW 4248 0,01
12 Fragrance composition Maurice 0,1
13 Liquitint Blue MC 0,49
Inner liquid phase
No. Chemical name Mass %
100,0
1 Protease 20,0
2 Amylase 20,0
3 Propylene glycol 60,0
Example 3B
Outer powder phase
No. Chemical name Mass %
100,0
1 Sodium chloride 15,0
2 Sodium sulfate 25,0 3 Sodium citrate 30,0
4 Water 0,5
5 Sodium silicate 0,5
6 Alcohols, C10-16, etoxylated 0,5
7 Sodium carbonate 20,0
8 Sodium percarbonate 7,5
9 Polikarboxylanes 0,5
10 Xiameter APW 4248 0,01
12 Fragrance composition Maurice 0,1
13 Liquitint Blue MC 0,49
Inner liquid phase
Variant 4
A complex capsule-in-capsule detergent was obtained according to Example 4 Outer powder phase
Content [%]
No. Chemical name
Min mass % Max mass %
1 Sodium chloride 15,0 40,0
2 Sodium sulfate 10,0 30,0
3 Sodium citrate 10,0 30,0
4 Water 0,5 1 ,0
5 Sodium silicate 0,5 5,0
6 Alcohols, C10-16, etoxylated 0,5 5,0
7 Sodium carbonate 10,0 30,0
8 Sodium percarbonate 5,0 10,0
9 Polikarboxylanes 0,5 5,0
10 Xiameter APW 4248 0,01 0,1
12 Fragrance composition 0, 1 1 ,0
13 Dyes 0,1 0,5 Inner powder phase
Example 4A
Outer powder phase
Inner powder phase
No. Chemical name Mass %
100,0
1 Amylase 30,0
2 Protease 45,0
3 TAED 20,0
4 Mn-complex 5,0 Example 4B
Outer powder phase
Inner powder phase
Laundry capsule
Variant 1
A complex capsule-in-capsule detergent was obtained according to Example 1
Outer phase/liquid
Content [%]
No. Chemical name
Min % w/w Max % w/w
1 Alcohols, C10-16, etoxylated 15,0 25,0
2 Fatty acids, coco, ethanolamine compounds 10,0 20,0 3 Dodecyl sulfonic acid, compound with 2- 10,0 20,0 aminoethanol (1 :1)
4 Glycerin 10,0 20,0
5 Tainted ethyl alcohol 5,0 10,0
6 Monopropylene glycol 3,0 6,0
7 Water 1 ,0 5,0
8 Alcohols, C12-14, etoxylated, sulfated, sodium 1 ,0 5,0
salts
9 L-glutamic acid, terasodium salt, Ν,Ν-diacetic acid 1 ,0 3,0
10 D-Glucopyranose, oligomers C8-C10, alkyl 1 ,0 3,0
glycosides
11 Citric acid 0, 1 1 ,0
12 Fragrance composition 0, 1 1 ,0
13 CM IT/MIT preservative 0,01 0,5
14 Dyes 0,0 0,5
15 Optical brightener 0,0 0,5
16 vinylpyrrolidone/vinylimidazole copolymer 0,0 0,5
Inner phase/liquid
Content [%]
No. Chemical name
Min % w/w Max % w/w
1 Protease 10,0 20,0
2 Amylase 10,0 20,0
3 Cellulase 5,0 15,0
4 Pectinase 5,0 15,0
5 Lipase 5,0 15,0
6 Mannanase 5,0 15,0
7 Propylene glycol 15,0 65,0 Example 1A
Outer phase/liquid
No. Chemical name % w/w
100,0
1 Alcohols, C10-16, etoxylated 15,0
2 Fatty acids, coco, ethanolamine compounds 25,0
3 Dodecyl sulfonic acid, compound with 2- 19,87 aminoethanol (1 :1)
4 Glycerin 10,0
5 Tainted ethyl alcohol 10,0
6 Monopropylene glycol 6,0
7 Water 5,0
8 Alcohols, C12-14, etoxylated, sulfated, sodium salts 5,0
9 L-glutamic acid, terasodium salt, Ν,Ν-diacetic acid 1 ,0
10 D-Glucopyranose, oligomers C8-C10, alkyl 1 ,0 glycosides
11 Citric acid 0,1
12 Arie Fresh Mountain 1 ,5
13 Isocil Ultra 1.5 0,01
1 Liquitint Blue HP 0,02
15 Optical brightener 0,0
16 vinylpyrrolidone/vinylimidazole copolymer 0,5
Inner phase/liquid
No. Chemical name % w/w
100,0
1 Protease 40,0
2 Amylase 25,0
3 Cellulase 5,0
4 Pectinase 5,0
5 Lipase 5,0
6 Mannanase 5,0
7 Propylene glycol 15,0 Example IB
Outer phase/liquid
No. Chemical name % w/w
100,0
1 Alcohols, C10-16, etoxylated 20,0
2 Fatty acids, coco, ethanolamine compounds 15,0
3 Dodecyl sulfonic acid, compound with 2- 20,0 aminoethanol (1 :1)
4 Glycerin 15,0
5 Tainted ethyl alcohol 9,39
6 Monopropylene glycol 6,0
7 Water 5,0
8 Alcohols, C12-14, etoxylated, sulfated, sodium salts 5,0
9 L-glutamic acid, terasodium salt, Ν,Ν-diacetic acid 1 ,0
10 D-Glucopyranose, oligomers C8-C10, alkyl 1 ,0 glycosides
11 Citric acid 0,1
12 Arie Fresh Mountain 1 ,5
13 Isocil Ultra 1.5 0,01
14 Liquitint Blue HP 0,5
15 Optical brightener 0,5
16 vinylpyrrolidone/vinylimidazole copolymer 0,0
Inner phase/liquid
Lp. Nazwa Chemiczna % w/w
100,0
1 Protease 20,0
2 Amylase 20,0
3 Cellulase 10,0
4 Pectin ase 10,0
5 Lipase 5,0
6 Mannanase 5,0
7 Propylene glycol 30,0 Variant 2
A complex capsule-in-capsule detergent was obtained according to Example 2
Outer phase/liquid
Content [%]
No. Chemical name
Min % w/w Max % w/w
1 Alcohols, C 10-16, etoxylated 15,0 25,0
2 Fatty acids, coco, ethanolamine compounds 10,0 20,0
3 Dodecyl sulfonic acid, compound with 2- 10,0 20,0
aminoethanol (1 :1)
4 Glycerin 10,0 20,0
5 Tainted ethyl alcohol 5,0 10,0
6 Monopropylene glycol 3,0 6,0
7 Water 1 ,0 5,0
8 Alcohols, C12-14, etoxylated, sulfated, sodium 1 ,0 5,0
salts
9 L-glutamic acid, terasodium salt, Ν,Ν-diacetic acid 1 ,0 3,0
10 D-Glucopyranose, oligomers C8-C10, alkyl 1 ,0 3,0
glycosides
11 Citric acid 0, 1 1 ,0
12 Fragrance composition 0,1 1 ,0
13 CMIT/MIT preservative 0,01 0,5
14 Dyes 0,0 0,5
15 Optical brightener 0,0 0,5
16 vinylpyrrolidone/vinylimidazole copolymer 0,0 0,5
Inner phase/powder
Content [%]
No. Chemical name
Min % w/w Max % w/w
1 Sodium percarbonate 60,0 80,0
2 TAED 20,0 40,0 Example 2A
Outer phase/liquid
No. Chemical name % w/w
100,0
1 Alcohols, C10-16, etoxylated 20,0
2 Fatty acids, coco, ethanolamine compounds 15,0
3 Dodecyl sulfonic acid, compound with 2- 20,0 aminoethanol (1 :1)
4 Glycerin 15,0
5 Tainted ethyl alcohol 9,39
6 Monopropylene glycol 6,0
7 Water 5,0
8 Alcohols, C12-14, etoxylated, sulfated, sodium salts 5,0
9 L-glutamic acid, terasodium salt, Ν,Ν-diacetic acid 1 ,0
10 D-Glucopyranose, oligomers C8-C10, alkyl 1 ,0 glycosides
11 Citric acid 0,1
12 Arie Fresh Mountain 1 ,5
13 Isocil Ultra 1.5 0,01
14 Liquitint Blue HP 0,5
15 Optical brightener 0,5
16 vinylpyrrolidone/vinylimidazole copolymer 0,0
Inner phase/powder
No. Chemical name . % w/w
100,0
1 Sodium percarbonate 60,0
2 TAED 40,0 Example 2B
Outer phase/liquid
Variant 3
A complex capsule-in-capsule detergent was obtained according to Example 4 Outer phase/powder Content [%]
No. Chemical name
Min % w/w Max % w/w
1 Sodium chloride 10,0 40,0
2 Sodium sulfate 10,0 40,0
4 Sodium carbonate 5,0 15,0
5 Sodium citrate 5,0 15,0
6 ABS acid sodium salt 1 ,0 5,0
7 Alcohols, C10-16, etoxylated 0,5 5,0
8 L-glutamic acid, terasodium salt, Ν,Ν-diacetic acid 0,5 5,0
9 Soap 1 ,0 5,0
10 Sodium percarbonate 5,0 15,0
11 Polycarboxylanes 0,5 5,0
13 Fragrance composition 0,1 1 ,0
14 Dyes 0,0 0,5
15 Optical brightener 0,0 0,5
16 vinylpyrrolidone/vinylimidazole copolymer 0,0 0,5
Inner phase/powder
Content [%]
No. Chemical name
Min % w/w Max % w/w
1 TAED 20,0 40,0
2 Protease 10,0 30,0
3 Amylase 10,0 30,0
4 Cellulase 5,0 15,0
5 Pectinase 5,0 15,0
6 Mannanase 5,0 15,0 Example 3A
Outer phase/powde
No. Chemical name % w/w
1 Sodium chloride 30,0
2 Sodium sulfate 25,0
4 Sodium carbonate 11 ,4
5 Sodium citrate 15,0
6 ABS acid sodium salt 2,5
7 Alcohols, C10-16, etoxylated 2,5
8 L-glutamic acid, terasodium salt, Ν,Ν-diacetic acid 2,5
9 Soap 5,0
10 Sodium percarbonate 5,0
11 Polycarboxylanes 0,5
13 Fragrance composition Maurice 0,1
14 Dye 0,0
15 Optical brightener 0,0
16 vinylpyrrolidone/vinylimidazole copolymer 0,5
Inner phase/powder
No. Chemical name % w/w
100,0
1 TAED 20,0
2 Protease 25,0
3 " Amylase 25,0
4 Cellulase 10,0
5 Pectinase 10,0
Example 3B
Outer phase/powder
No. Chemical name % w/w
1 Sodium chloride 18,0
2 Sodium sulfate 25,0
4 Sodium carbonate 15,0
5 Sodium citrate 15,0
6 ABS acid sodium salt 3,5
7 Alcohols, C10-16, etoxylated 2,5
8 L-glutamic acid, terasodium salt, Ν,Ν-diacetic acid 2,5
9 Soap 5,0
10 Sodium percarbonate 10,0"
11 Polycarboxylanes 2,5
13 Fragrance composition Maurice 0,5
14 Dye 0,0
15 Optical brightener 0,5
16 vinylpyrrolidone/vinylimidazole copolymer 0,0
Inner phase/powder
No. Chemical name % w/w
100,0
1 TAED 30,0
2 Protease 25,0 3 Amylase 25,0
4 Cellulase 10,0
5 Pectinase 5,0
6 Mannanase 5,0
Example 5
Enzyme stability test
An evaluation of enzyme stability in PEG 400 and Acusol 445N under the following conditions has been conducted:
Testing conditions:
Storage conditions:
Formulations:
If a mixture was added:
The results of the tests are presented in Figs. 1, 2 and 3 for different enzymes: amylase, protease and cellulase. The test results clearly indicate that PEG 400 does not influence enzyme stability in the composition.

Claims

Patent claims
1. A complex capsule-in-capsule detergent characterized in that it consists of at least two phases: an inner phase and an outer phase separated from each other with an inner foil, while the outer phase is surrounded with an outer foil, wherein the inner phase comprises active substances, especially selected from: enzymes, bleaching agents, in particular percarbonate and tetraacetylethylenediamine (TAED), and other active agents.
2. A complex capsule-in-capsule detergent according to claim 1, characterized in that the foil is made of polyvinyl alcohol, gelatin, polyacrylamide or hydroxypropylcellulose.
3. A complex capsule-in-capsule detergent according to claim 2, characterized in that the thickness of the inner foil is greater than the thickness of the outer foil.
4. A complex capsule-in-capsule detergent according to claim 2, characterized in that the thickness of the outer foil and the inner foil is the same.
5. A complex capsule-in-capsule detergent according to claims 1-4, characterized in that the inner foil has thickness ranging from 90 μηη to 1 mm and the outer foil has thickness ranging from 60 μιη to 90 μιτι, to provide the delay of release of the active substances from 1 to 5 minutes.
6. A complex capsule-in-capsule detergent according to claims 1-5, characterized in that the outer phase is a liquid phase and the inner phase is a liquid phase, or the outer phase is a liquid phase and the inner phase is a solid phase in the form of powder or granulate.
7. A complex capsule-in-capsule detergent according to claims 1-6, characterized in that the inner phase comprises percarbonate and TAED in powder form .
8. A complex capsule-in-capsule detergent according to claims 1-5, characterized in that it comprises the outer solid phase in the form of powder or granulate and the inner liquid phase.
9. A complex capsule-in-capsule detergent according to any of the claims 1-8 for use in washing fabrics.
10. A complex capsule-in-capsule detergent according to claim 9, characterized in that it comprises: in the outer phase: alcohols, ClO-16, etoxylated in a range of 15.0-25.0% w/w, fatty acids, coco, ethanolamine compounds in a range of 10.0-20.0% w/w, dodecyl sulfonic acid, 2-aminoethanol compound (1:1) in a range of 10.0-20.0% w/w, glycerin in a range of 10.0-20.0% w/w/, tainted ethyl alcohol in a range of 5.0-10.0% w/w, monopropylene glycol in a range of 3.0-6.0% w/w, water in a range of 1.0-5.0% w/w, alcohols etoxylated, sulphated, sodium salts in a range of 1.0-5.0% w/w, L- glutamic acid, tetrasodium salt, Ν,Ν-diacetic acid in a range of 1.0-3.0% w/w, D-glucopyrranose, oligomers C8-C10, alkyl glycosides in a range of 1.0-3.0% w/w, citric acid in a range of 0.1-1.0% w/w, fragrance composition in a range of 0.1-1.0% w/w, CMIT/MIT preservative in a range of 0.01-0.5% w/w, dyes in a range of 0.0-0.5% w/w, optical brightener in a range of 0.0-0.5% w/w, vinylpyrrolidone/vinylimidazole copolymer in a range of 0.0-0.5% w/w,
in the inner phase I: protease in a range of 10.0-20.0% w/w, amylase in a range of 10-20% w/w, and/or cellulase in a range of 5-15% w/w; and/or pectinase 5-15% w/w; and/or lipase in a range of 5-15% w/w and/or mannanase in a range of 5-15% w/w; and propylene glycol in a range of 15-65% w/w; and/or in the inner phase II: sodium percarbonate in a range of 60-80; and/or TAED in a range of 20-40% w/w.
11. A complex capsule-in-capsule detergent according to claim 9, characterized in that it comprises: in the outer phase: sodium chloride in a range of 10.0-40.0% w/w, sodium sulfate in a range of 10.0- 40.0% w/w, sodium carbonate in a range of 5.0-15.0% w/w, sodium citrate in a range of 5.0-15.0% w/w, ABS acid sodium salt in a range of 1.0-5.0% w/w, alcohols, C10-C16, etoxylated in a range of 0.5-5.0% w/w, L-glutamic acid, tetrasodium salt, of Ν,Ν-diacetic acid in a range of 0.5-5.0% w/w, soap in a range of 1.0-5.0% w/w, sodium percarbonate in a range of 5.0-15.0% w/w, polycarboxylanes in a range of 0.5-5.0% w/w, fragrance composition in a range of 0.1-1.0% w/w, dyes in a range of 0.0- 0.5% w/w, optical brightener in a range of 0.0-0.5% w/w, vinylpyrrolidone/vinylimidazole copolymer in a range of 0.0-0.5% w/w,
in the inner phase: protease in a range of 10.0-30.0% w/w, amylase in a range of 10-30% w/w, and/or cellulase in a range of 5-15% w/w; and/or pectinase 5-15% w/w; and/or mannanase in a range of 5- 15% w/w.
12. A complex capsule-in-capsule detergent according to any of claims 1-8 for use in dishwashers.
13. A complex capsule-in-capsule detergent according to claim 12, characterized in that it comprises: in the outer phase: L-glutamic acid, Ν,Ν-diacetic acid tetrasodium salt in a range of 15.0-60.0% w/w, glycerine in a range of 10.0-30.0% w/w; monopropylene glycol in a range of 10.0-20.0% w/w, water in a range of 5.0-15.0% w/w, polycarboxylanes in a range of 1.0-10.0% w/w, D-glucopyrranose, C8- C10 oligomers, alkyl glycosides in a range of 1.0-10.0% w/w, alcohols, ClO-15, etoxylated in a range of 0.5-5.0% w/w, sodium hydroxide in a range of 0.5-5.0% w/w, citric acid in a range of 0.5-5.0% w/w, sodium citrate in a range of 0.5-5.0% w/w, l-octyl-2-pyrrolidone acid in a range of 0.1-3.0% w/w, fragrance composition in a range of 0.1-2.0% w/w, dyes in a range of 0.01-0.5% w/w, preservatives in a range of 0-0.5% w/w,
in the inner phase I: sodium percarbonate in a range of 60-80; and/or TAED in a range of 20-40% w/w; and/or in the inner phase II: protease in a range of 10-40% w/w, amylase in a range of 10-40% w/w.
14. A complex capsule-in-capsule detergent according to claim 12, characterized in that it comprises: in the outer phase: sodium chloride in a range of 15.0-40.0% w/w, sodium sulfate in a range of 10.0- 30.0% w/w, sodium citrate in a range of 10.0-30.0% w/w, water in a range of 0.5-1.0% w/w, silicic acid sodium salt in a range of 0.5-5.0% w/w, alcohols, ClO-16, etoxylated in a range of 0.5-5.0% w/w, sodium carbonate in a range of 10.0-30.0% w/w, sodium percarbonate in a range of 5.0-10.0% w/w, polycarboxylanes in a range of 0.5-5.0% w/w, silicates in a range of 0.01-0.1% w/w, fragrance composition in a range of 0.1-1.0% w/w, dyes in a range of 0.1-0.5% w/w,
in the inner phase I: Mn-complex in a range of 0.5-20% w/w, protease in a range of 40-80% w/w, amylase in a range of 30-60% w/w; and/or in the phase II: percarbonate 60-90% w/w and/or TAED in a range of 20-40% w/w.
15. A method of producing the multicompartment capsule-in-capsule comprising one or more inner compartments and one outer compartment, wherein the outer compartment surrounds 100% of the outer surface of the inner compartment(s), completely surrounded with at least one layer which dissolves in contact with water, characterized in that it comprises the stages of:
a) producing the smaller capsule, whose coating is PVOH foil or gelatin, and then placing a non-ionic surfactant PEG400 mixed with liquid or granulated enzymes in it;
b) forming the larger capsule of PVOH foil, wherein in the forming process the foil is sucked in to the sockets in a forming drum to create a hollow coated with the PVOH foil, and then using feeders to place in said hollow the smaller capsule obtained in stage a), after which the larger capsule, in which the smaller capsule is already placed, is filled with a liquid or granulate which completes the whole capsule formulation, and then the hollow is sealed with a second foil to form the finished product.
16. A method according to claim 15, characterized in that it comprises:
in the outer phase: alcohols, ClO-16, etoxylated in a range of 15.0-25.0% w/w, fatty acids, coco, ethanolamine compounds in a range of 10.0-20.0% w/w, dodecyl sulfonic acid, 2-aminoethanol compound (1:1) in a range of 10.0-20.0% w/w, glycerin in a range of 10.0-20.0% w/w/, tainted ethyl alcohol in a range of 5.0-10.0% w/w, monopropylene glycol in a range of 3.0-6.0% w/w, water in a range of 1.0-5.0% w/w, alcohols etoxylated, sulphated, sodium salts in a range of 1.0-5.0% w/w, L- glutamic acid, tetrasodium salt, Ν,Ν-diacetic acid in a range of 1.0-3.0% w/w, D-glucopyrranose, oligomers C8-C10, alkyl glycosides in a range of 1.0-3.0% w/w, citric acid in a range of 0.1-1.0% w/w, fragrance composition in a range of 0.1-1.0% w/w, CMIT/MIT preservative in a range of 0.01-0.5% w/w, dyes in a range of 0.0-0.5% w/w, optical brightener in a range of 0.0-0.5% w/w, vinylpyrrolidone/vinylimidazole copolymer in a range of 0.0-0.5% w/w,
in the inner phase I: protease in a range of 10.0-20.0% w/w, amylase in a range of 10-20% w/w, and/or cellulase in a range of 5-15% w/w; and/or pectinase 5-15% w/w; and/or lipase in a range of 5-15% w/w and/or mannanase in a range of 5-15% w/w; and propylene glycol in a range of 15-65% w/w; and/or in the inner phase II: sodium percarbonate in a range of 60-80; and/or TAED in a range. of 20-40% w/w.
17. A method according to claim 15, characterized in that it comprises:
in the outer phase: sodium chloride in a range of 10.0-40.0% w/w, sodium sulfate in a range of 10.0- 40.0% w/w, sodium carbonate in a range of 5.0-15.0% w/w, sodium citrate in a range of 5.0-15.0% w/w, ABS acid sodium salt in a range of 1.0-5.0% w/w, alcohols, C10-C16, etoxylated in a range of 0.5-5.0% w/w, L-glutamic acid, tetrasodium salt, of Ν,Ν-diacetic acid in a range of 0.5-5.0% w/w, soap in a range of 1.0-5.0% w/w, sodium percarbonate in a range of 5.0-15.0% w/w, polycarboxylanes in a range of 0.5-5.0% w/w, fragrance composition in a range of 0.1-1.0% w/w, dyes in a range of 0.0- 0.5% w/w, optical brightener in a range of 0.0-0.5% w/w, vinylpyrrolidone/vinylimidazole copolymer in a range of 0.0-0.5% w/w,
in the inner phase: protease in a range of 10.0-30.0% w/w, amylase in a range of 10-30% w/w, and/or cellulase in a range of 5-15% w/w; and/or pectinase 5-15% w/w; and/or mannanase in a range of 5-15% w/w.
18. A method according to claim 15, characterized in that it comprises:
in the outer phase: L-glutamic acid, Ν,Ν-diacetic acid tetrasodium salt in a range of 15.0-60.0% w/w, glycerin in a range of 10.0-30.0% w/w; monopropylene glycol in a range of 10.0-20.0% w/w, water in a range of 5.0-15.0% w/w, polycarboxylanes in a range of 1.0-10.0% w/w, D-glucopyrranose, C8-C10 oligomers, alkyl glycosides in a range of 1.0-10.0% w/w, alcohols, C10-15, etoxylated in a range of 0.5-5.0% w/w, sodium hydroxide in a range of 0.5-5.0% w/w, citric acid in a range of 0.5-5.0% w/w, sodium citrate in a range of 0.5-5.0% w/w, l-octyl-2-pyrrolidone acid in a range of 0.1-3.0% w/w, fragrance composition in a range of 0.1-2.0% w/w, dyes in a range of 0.01-0.5% w/w, preservatives in a range of 0-0.5% w/w,
in the inner phase I: sodium percarbonate in a range of 60-80; and/orTAED in a range of 20-40% w/w; and/or in the inner phase II: protease in a range of 10-40% w/w, amylase in a range of 10-40% w/w.
19. A method according to claim 15, characterized in that it comprises:
in the outer phase: sodium chloride in a range of 15.0-40.0% w/w, sodium sulfate in a range of 10.0- 30.0% w/w, sodium citrate in a range of 10.0-30.0% w/w, water in a range of 0.5-1.0% w/w, silicic acid sodium salt in a range of 0.5-5.0% w/w, alcohols, ClO-16, etoxylated in a range of 0.5-5.0% w/w, sodium carbonate in a range of 10.0-30.0% w/w, sodium percarbonate in a range of 5.0-10.0% w/w, polycarboxylanes in a range of 0.5-5.0% w/w, silicates in a range of 0.01-0.1% w/w, fragrance composition in a range of 0.1-1.0% w/w, dyes in a range of 0.1-0.5% w/w,
in the inner phase I: Mn-complex in a range of 0.5-20% w/w, protease in a range of 40-80% w/w, amylase in a range of 30-60% w/w; and/or in the phase II: percarbonate 60-90 and/orTAED in a range of 20-40% w/w.
EP18722251.8A 2017-03-14 2018-03-13 Complex capsule-in-capsule detergent Active EP3596194B1 (en)

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Publication number Priority date Publication date Assignee Title
US11659838B2 (en) 2021-04-01 2023-05-30 Sterilex, Llc Quat-free powdered disinfectant/sanitizer
EP4442358A2 (en) 2023-03-19 2024-10-09 Capsule Minimal Ltd. Multilayered capsule with controllable arrangement of layers and industrial systems and processes of fabricating the same

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DE102018220189A1 (en) 2018-11-23 2020-05-28 Henkel Ag & Co. Kgaa Detergent for automatic dosing
GB202003424D0 (en) * 2020-03-10 2020-04-22 Reckitt Benckiser Calgon Bv Composition for the removal and prevention of deposition of limescale

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DE10104841A1 (en) * 2001-02-01 2002-09-12 Henkel Kgaa Capsule-in-capsule system and method for its production
GB0305666D0 (en) * 2003-03-12 2003-04-16 Unilever Plc A water soluble delivery product
EP2924105A1 (en) * 2014-03-28 2015-09-30 The Procter and Gamble Company Water soluble unit dose article
EP3249037B1 (en) * 2016-05-23 2020-04-22 The Procter & Gamble Company Detergent composition comprising an encapsulated enzyme

Cited By (3)

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Publication number Priority date Publication date Assignee Title
US11659838B2 (en) 2021-04-01 2023-05-30 Sterilex, Llc Quat-free powdered disinfectant/sanitizer
US12274267B2 (en) 2021-04-01 2025-04-15 Sterilex, Llc Quat-free powdered disinfectant/sanitizer
EP4442358A2 (en) 2023-03-19 2024-10-09 Capsule Minimal Ltd. Multilayered capsule with controllable arrangement of layers and industrial systems and processes of fabricating the same

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PL247916B1 (en) 2025-09-15
PT3596194T (en) 2024-03-25

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