Title of Invention

"AN ANTIMICROBIAL CONSTRUCTION".

Abstract A construction comprises a substrate incorporating an activatable antimicrobial composition. The antimicrobial composition includes a peroxygen donor and an acid and/or an acid-producing substance. The peroxygen donor is incorporated separately and in a different portion of the substrate from the other component or components of the antimicrobial composition. Preferably, the antimicrobial composition comprises a peroxygen donor in the form of sodium perborate as a mono or tetra hydrate, or sodium percarbonate and an acid-producing substance in the form of tetra acetyl ethylene diamine. Such an antimicrobial composition can be activated by wetting the substrate with water.
Full Text WO 2005/112631 PCT/GB2005/001878
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AN ANTIMICROBIAL CONSTRUCTION
The present invention relates to a construction comprising a substrate incorporating an activatable antimicrobial composition for use, for example, as a pad, a wipe, or as a means of dosing the composition.
The term "substrate" used herein and in the claims is intended to include cloth, paper and other nonwoven materials as well as woven or knitted textile fabrics. In addition, the term "substrate" is intended to cover naturally occurring materials such as animal skins.
Antimicrobial compositions must exhibit a range of properties to be useful. Many of these properties are as follows.
1. The composition should act rapidly - European standards require a
contact time of five minutes.
2. The composition should be biocidal and not merely biostatic.
3. The composition should have a wide spectrum of activity against
bacteria, including all Gram-positive and Gram-negative bacteria, as
well as mycobacteria.
4. The composition should be active against all types of fungi.
5. The composition should be virucidal, against both enveloped and non-
enveloped viruses.
6. The composition should be effective in both clean and dirty conditions
and be able to penetrate biofilms.
7. The composition should be rapidly effective against bacterial
endospores.
8. The mechanism of activity of the composition should not give rise to
resistance.
9. The composition should be of low toxicity to non-target life forms.
10. The composition should be adequately stable to allow ease of use and
storage.
11. The composition should be simple to use.

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12. The effect and residue chemistry of the composition should be
environmentally benign.
13. The composition should remain rapidly effective down to low
temperatures of around 4°C or lower.
14. The composition should embody an indicator of its performance.
15. The composition should be cost effective in use.
To produce an antimicrobial composition with all of these properties is extremely difficult as such products, by their nature, are toxic and reactive. Many are comprised of complex organic molecules, the residues of which resist environmental breakdown or may bio-accumulate. Others react with organic matter and may be knocked out in the presence of high soil levels or may react with organic soil to produce toxic or carcinogenic compounds. Many are unstable or of limited spectrum.
It is an object of the present invention to provide a construction comprising a substrate incorporating with an activatable antimicrobial composition which exhibits most and, in specific formulations, all of the aforementioned properties. Such a substrate must retain the antimicrobial composition in a stable manner ready for use, at which time the composition can be activated, for example by wetting the substrate with water or other appropriate liquid.
According to the present invention there is provided a construction comprising a substrate incorporating an activatable antimicrobial composition that includes a peroxygen donor and at least one of an acid and an acid-producing substance, the peroxygen donor being incorporated separately and in a different portion of the substrate from the other component or components of the composition.
In such a construction, the peroxygen donor is incorporated separately and in a different portion of the substrate from the other components of the composition in order that the antimicrobial composition

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is only formed and activated once the substrate is wetted, preferably with water.
Advantageously, the substrate is constructed as a laminate, such as a nonwoven laminate, comprising layers bonded together by a bonding medium which may be applied as a powder, net or sheet, the peroxygen donor being incorporated in the substrate in between different layers from the other components, or otherwise separated by application in a different zone or area of the substrate, for instance in parallel scatterings or in different parts of a scatter pattern.
Preferably also, the substrate comprises a nonwoven material made from cellulosic fibres, for example cotton, viscose, regenerated wood pulp cellulose or similar material. Alternatively or in addition, the material comprises fibres including at least one of polyester, polyamide, polyethylene, and polypropylene fibres. Where the fibres of the nonwoven have physical properties, for example bi-component fibres, which allow the substrate to be thermally or physically bonded or entangled in a discreet layer or web, it may be possible to dispense with all or most of the bonding medium.
Preferably also, the substrate is impregnated with an oxygen-sensitive dye, such as a vat dye, which acts to indicate activity of the antimicrobial composition.
Preferably also, the acid comprises a carboxylic acid.
In some embodiments, the antimicrobial composition additionally incorporates an organometallic manganese containing catalyst, for example a manganese-trimethyltriazacyclononane complex.
Preferably also, the acid may comprise a bidentate acid and preferably oxalic acid. Such acids can influence the nuclearity and redox potential of the metal centres in the catalyst which, in turn, improves the spectrum and

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speed of biocidal activity. Alternatively, however, other acids such as fumaric, ascorbic, succinic, glutaric and mixtures thereof may also be used. In addition, combinations of acid and salts of the acid may also be used, for instance, oxalic acid and sodium oxalate. A combination of oxalic acid and pH buffers such as sodium phosphate may also be used.
Combinations of acids may also be used, for example a combination of oxalic acid and citric acid. Also, reaction between the peroxygen donor and a bleach activator, such as tetra acetyl ethylene diamine (TAED) would beneficially produce peracetic acid. Such a reaction will occur on activation of the composition. Hence, advantageously, the acid of the composition may be a separate component of the composition or may be generated in situ in the substrate on activation.
The peroxygen donor may be chosen from any of those compounds exhibiting strong redox potential by generation of hydrogen peroxide or other mechanism. Preferably, therefore, the peroxygen donor comprises any of sodium perborate as mono or tetra hydrate, sodium percarbonate, and sodium persulphate. It is also possible to generate an effective composition in situ by activating the substrate using a hydrogen peroxide solution.
In order to most completely meet the above list of desirable properties, rapidly at low temperatures, in particular at temperatures below 4°C, the substrate is preferably additionally incorporates the aforesaid organometallic manganese containing catalyst. - Advantageously, the organometallic manganese containing catalyst comprises a manganese-trimethyltriazacyclononane complex, such as that known commercially as catalyst NP 1033, CAS No 116633-52-4. This is a manganese compound of the ligand 1,4,7-trimethyl-1,4,7-triazacyclononane. However, other manganese catalysts with related ligand structures and other biomimetic manganese containing catalysts may also be used.

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The catalyst to peroxygen donor ratio may be as high as 1:100000, however, preferably, the preferred ratio is between 1:100 and 1:3000 inclusive.
Likewise, the catalyst to acid ratio, preferably when using bidentate carboxylic acid, can be in the range 1:1 to 1:100 but preferably the preferred ratio is between 1: 3 and 1:50 inclusive.
Other. components may usefully be added to the composition according to the invention. These may comprise one or more of anionic or nonionic surfactants such as sodium laxiryl sulphate or linear alcohol ethoxylates; corrosion inhibitors, pH buffers, chelating agents or sequestrants, stabilizers, dyes, fragrances and odour masking agents.
Two examples of formulations of antimicrobial compositions in accordance with the invention will now be described.
Example 1
Sodium perborate tetrahydrate 1.05 parts
Tetra acetyl ethylene diamine 0.014 parts
Oxalic acid 0.35 parts
NP 1033 0.01 parts
Example 2
Sodium percarbonate 50 parts
Tetra acetyl ethylene diamine 25 parts
Sequestrant 2 parts
Anionic surfactant 5 parts
Citric acid 1 part

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The antimicrobial performance of each these formulations can be demonstrated by adding l part formulation to 10 parts of water. The ensuing solutions both meet the requirements of the European suspension test EN1276:1997. This test is a quantitative suspension test for the evaluation of bactericidal activity of chemical disinfectants and antiseptics used in foods, industrial, domestic and institutional areas. To meet the test a greater than log 5 kill of all test organisms must occur within a 5 minute contact time and at temperatures of both 20° C and 40 C in both clean and dirty conditions. The test organisms used are Pseudomonas aeruginosa, Escherichia coli, Staphyldcoccus aureus and Enterococcus hirae.
Both of the formulations also show excellent sporicidal, fungicidal and virucidal properties in standard tests. In addition, it should be noted that the residue products of Example 1 are environmentally benign. It is known that in formulations containing peroxygen donors and bleach activators such as TAED that a very wide range of ratios of the two components can be used determined by requirements such as the concentration of peracetic acid generated, the rate of generation, the pH of the system, the stability, solubility and other factors. Hence in constructions in accordance with this invention a wide range of ratios of the antimicrobial composition and quantitative loadings of the substrate is possible.
An additional formulation of antimicrobial composition in accordance with the invention will now be described.
Example 3
Sodium perborate tetrahydrate 1.05 parts
Oxalic acid 0.35 parts
NP 1033 0.01 parts
This formulation excludes the bleach accelerator. It also passes the European suspension test EN1276:1997 for all test organisms at a

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temperature of 20°C but not at a temperature of 4°C. Hence although useful, it may have more limited applications than other formulations of the composition.
A change in the oxidation state of the manganese catalyst where used in these formulations is also accompanied by a colour change. These formulations therefore embody an indicator of their performance.
The components of the antimicrobial composition are preferably produced in the form of powders or granules for ease of incorporation into separate portions of the body of the substrate, as described above, in order that the construction can remain in a stable condition ready for use. At this time, the antimicrobial composition can be activated by wetting the substrate with water. Such wetting may occur when a wipe construction according to the invention is wetted or is used to wipe a wet or damp surface; or is used to absorb a spillage containing an aqueous component; or is used as a filter for water which may be contaminated; or is moistened by water vapour, perspiration or other means.
Three embodiments of construction in accordance with the present invention are as follows.
Embodiment 1
The substrate comprises a nonwoven laminate construction comprising two layers of hydroentangled nonwoven containing viscose and polyester fibres separated by a thermoplastic bonding medium in sheet form. The layer between the bottom nonwoven and the bonding medium contains the peroxygen donor. The layer between the bonding medium and the top nonwoven contains the tetra acetyl ethylene diamine, surfactant, acid and other components of the antimicrobial composition. The chemical components of the formulation being present at quantitative levels and in such ratios and at such a pH as to generate levels of peracetic acid when the

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substrate is wetted, which levels of peracetic acid are appropriate to the biocidal task required.
Embodiment 2
The substrate comprises a nonwoven laminate construction as described above in Embodiment l but wherein the bonding medium is a low melting point thermoplastic powder and the peroxygen donor component of the formulation is separated from the other components by virtue of being applied by scattering or other means which ensure the peroxygen donor powder is restricted to areas of the substrate not covered by other components with which it might react.
Embodiment 3
The substrate comprises a nonwoven laminate construction made up of highly absorbent airlaid fibres as one of the nonwoven layers, in which the peroxygen donor is sodium perborate monohydrate present at 15 g per square metre. The other components of the antimicrobial composition, which include TAED present at 8.0 g per square metre, are separated by virtue of two discreet patterns of powder scattering in combination with a thermoplastic powder bonding adhesive. The complete construction, on wetting, is capable of generating 5ooppm of peracetic acid in one litre of water.

9
CLAIMS
1. A construction comprising a substrate incorporating an activatable
antimicrobial composition that includes a peroxygen donor and at
least one of an acid and an acid-producing substance, the substrate
comprising a laminate having at least two layers which are bonded
together by a thermoplastic bonding medium, and the peroxygen
donor being incorporated in the laminate such that it is retained
separate from the other component or components of the composition
by the thermoplastic bonding medium.
2. A construction as claimed in Claim i, wherein the laminate comprises
at least two layers bonded together by the thermoplastic bonding
medium which is applied as a powder, net or sheet prior to a bonding
process.
3. A construction as claimed in Claim 1 or Claim 2, wherein the
peroxygen donor is incorporated and retained between different
layers of the laminate than the other components of the composition
by the thermoplastic bonding medium being in sheet form.
4. A construction as claimed in Claim 1 or Claim 2, wherein the
peroxygen donor is separated from the other components of the
composition by virtue of its application and retention in a different
zone of the substrate by the thermoplastic bonding medium.
5. A construction as claimed in Claim 1 or Claim 2, wherein the
peroxygen donor is in powder form and is retained separate from the
other component or components of the composition by powder
scattering in combination with a thermoplastic powder bonding
medium.
AMENDED PAGEj

ID
6. A construction as claimed in any of Claims 1 to 5, wherein the
substrate comprises a nonwoven material made from at least one of
cellulosic fibres, polyester fibres, polyamide fibres, polyethylene
fibres, and polypropylene fibres.
7. A construction as claimed in any of Claims 1 to 6, wherein the
substrate is impregnated with an oxygen-sensitive dye that which acts
to indicate activity of the antimicrobial composition.
8. A construction as claimed in any of Claims 1 to 7, wherein the acid
comprises a carboxylic acid.
9. A construction as claimed in any of Claims 1 to 7, wherein the acid
comprises at least one of a bidentate acid, oxalic acid, fumaric acid,
ascorbic acid, succinic acid, glutaric acid and any mixture of the
aforesaid acids.
10. A construction as claimed in any of Claims 1 to 7, wherein the acid
comprises a mixture of an acid and a salt.
11. A construction as claimed in any of Claims 1 to 10, wherein the acid-
producing substance comprises a bleach activator.
12. A construction as claimed in Claim 11, wherein the bleach activator
comprises tetra acetyl ethylene diamine.
13. A construction as claimed in any of Claims 1 to 12, wherein the
peroxygen donor comprises at least one of sodium perborate as mono
or tetra hydrate, sodium percarbonate, and sodium persulphate.
14. A construction as claimed in any of Claims 1 to 13, in which the
antimicrobial composition additionally comprises an organometallic
manganese containing catalyst.


15- A construction as claimed in Claim 14, wherein the organometallic manganese containing catalyst comprises a manganese-trimethyltriazacyclononane complex.
16. A construction as claimed in Claim 14 or Claim 15, wherein the
catalyst to peroxygen donor ratio is in the range between 1:100 and
1:3000 inclusive.
17. A construction as claimed in any of Claims 14 to 16, wherein the
catalyst to acid ratio is in the range between 1:3 and 1:50 inclusive.
18. A construction as claimed in any of Claims 1 to 17, that further
comprises one or more additives selected from a group comprising
surfactants, corrosion inhibitors, pH buffers, sequestrants, stabilizers,
dyes, fragrances, odour masking agents, and mixtures thereof.
19. A construction as claimed in any of Claims 1 to 18, wherein the
activatable antimicrobial composition is formulated in accordance
with any one of Examples 1 to 3 as follows:-


Example 1
Sodium perborate tetrahydrate 1.05 parts
Tetra acetyl ethylene diamine 0.014 parts
Oxalic acid 0.35 parts
NP1033 0.01 parts
Example 3
Sodium percarbonate 50 parts
Tetra acetyl ethylene diamine 25 parts
Sequestrant 2 parts
Anionic surfactant 5 parts
Citric acid lpart

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Example 3
Sodium perborate tetralrydrate 1.05 parts
Oxalic acid 0.35 parts
NP1033 0.01 parts


Documents:

03383-kolnp-2006-abstract.pdf

03383-kolnp-2006-claims.pdf

03383-kolnp-2006-correspondence others.pdf

03383-kolnp-2006-correspondence-1.1.pdf

03383-kolnp-2006-description (complete).pdf

03383-kolnp-2006-form1.pdf

03383-kolnp-2006-form13.pdf

03383-kolnp-2006-form3.pdf

03383-kolnp-2006-form5.pdf

03383-kolnp-2006-general power of authority.pdf

03383-kolnp-2006-international publication.pdf

03383-kolnp-2006-international search authority report.pdf

03383-kolnp-2006-other document.pdf

03383-kolnp-2006-pct form.pdf

03383-kolnp-2006-priority document.pdf

3383-KOLNP-2006-ABSTRACT 1.1.pdf

3383-KOLNP-2006-ABSTRACT.pdf

3383-KOLNP-2006-AMANDED CLAIMS.pdf

3383-KOLNP-2006-CANCELLED PAGES.pdf

3383-kolnp-2006-claims 1.1.pdf

3383-KOLNP-2006-DESCRIPTION (COMPLETE) 1.1.pdf

3383-KOLNP-2006-DESCRIPTION (COMPLETE).pdf

3383-KOLNP-2006-EXAMINATION REPORT REPLY RECIEVED 1.1.pdf

3383-KOLNP-2006-FORM 1 1.1.pdf

3383-KOLNP-2006-FORM 13.pdf

3383-kolnp-2006-form 18.pdf

3383-KOLNP-2006-FORM 2 1.1.pdf

3383-KOLNP-2006-FORM 2.pdf

3383-KOLNP-2006-FORM 3.pdf

3383-KOLNP-2006-FORM-27.pdf

3383-KOLNP-2006-OTHERS 1.1.pdf

3383-KOLNP-2006-OTHERS.pdf

3383-KOLNP-2006-PETETION UNDER RULE 137.pdf

3383-KOLNP-2006-REPLY TO EXAMINATION REPORT.pdf


Patent Number 244230
Indian Patent Application Number 3383/KOLNP/2006
PG Journal Number 48/2010
Publication Date 26-Nov-2010
Grant Date 24-Nov-2010
Date of Filing 15-Nov-2006
Name of Patentee FELLOWS, ADRIAN, NEVILLE
Applicant Address 1 SLATER BANK, HEBDEN BRIDGE, HX7 7DY, GREAT BRITAIN
Inventors:
# Inventor's Name Inventor's Address
1 FELLOWS, ADRIAN, NEVILLE 1 SLATER BANK, HEBDEN BRIDGE, HX7 7DY, GREAT BRITAIN
PCT International Classification Number A01N25/34; A01N37/04; A01N37/06;
PCT International Application Number PCT/GB2005/001878
PCT International Filing date 2005-05-18
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 0411304.9 2004-05-21 U.K.