# US 10,308,669 B2 · Laminated articles for microbial removal and low pressure drop filtration, methods of making, and methods of using same

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- Number: US 10,308,669 B2
- Document ID: US10308669B2
- Status: Granted
- Kind: B2
- Application number: 15/037,132
- Filed: 2014-12-12
- Published: 2016-10-06
- Granted: 2019-06-04
- Earliest claimed: 2013-12-19
- Assignees: 3M Innovative Properties Company
- Applicants: 3M Innovative Properties Company
- Inventors: Manjiri T. Kshirsagar; Bong Y. Yeom; Timothy J. Rowell; Satinder K. Nayar
- Web page: https://patentgrep.com/patent/US10308669B2

## CPC

- C07F 7/0836: {Compounds with one or more Si-OH or Si-O-metal linkage}
- B01D 39/086: {of inorganic material}
- B01D 39/14: Other self-supporting filtering material {; Other filtering material (non-woven fabrics in general D04H3/00)}
- B01D 39/1623: {of synthetic origin}
- B01D 39/2031: {the material being particulate}
- B32B 5/022: {Non-woven fabric}
- B32B 27/12: next to a fibrous or filamentary layer
- B32B 27/32: comprising polyolefins {(comprising vinyl (co)polymers or acrylic (co)polymers B32B27/30)}
- B32B 27/34: comprising polyamides
- B32B 27/36: comprising polyesters
- C07F 7/0838: {Compounds with one or more Si-O-Si sequences (compounds with a ring containing only alternating Si and O atoms, i.e. cyclosilanes C07F7/21)}
- C07F 7/1804: {Compounds having Si-O-C linkages (Si-O-acyl linkages C07F7/1896)}
- D04H 13/00: Other non-woven fabrics
- B01D 2239/0442: Antimicrobial, antibacterial, antifungal additives
- B01D 2239/0654: Support layers
- B32B 2264/102: Oxide or hydroxide
- C07F: ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM (metal-containing porphyrins C07D487/22)
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- B32B: LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- D04H: MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL (weaving D03; knitting D04B; braiding D04C; net-making D04G; sewing D05B; tufting D05C; finishing non-woven fabrics D06); FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING {; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION}(non-woven fabrics having an intermediate or external layer of a different kind, e.g. of woven fabric, B32B)

## Abstract

Laminated articles are provided including a porous fibrous nonwoven matrix and guanidine-functionalized metal silicate particles enmeshed within the porous fibrous nonwoven matrix. The laminated articles further include a first substrate and a second substrate sealed to the first substrate. Methods of making laminated articles and methods of using laminated articles are also provided.

## Claims

### Claim 1

A laminated article comprising:
a) a porous fibrous nonwoven matrix;
b) a plurality of guanidine-functionalized metal silicate particles enmeshed within the porous fibrous nonwoven matrix, the guanidine-functionalized metal silicate particles comprising:
a metal silicate particle that is modified with at least one silane having the formula
X3-nRanSi—Y-G,
wherein:
n is 0, 1, or 2;
each Ra, if present, is independently an alkyl, aralkyl, or aryl;
Y is a divalent group comprising an alkylene having 2 to 20 carbons;
G is a guanidine group of the formula —NH—C(═NH)—NH2; and
each X is independently alkoxy or acyloxy;
c) a first substrate; and
d) a second substrate sealed to the first substrate along at least a portion of a perimeter of the first substrate, wherein the porous fibrous nonwoven matrix is disposed between the first substrate and the second substrate.

### Claim 2 (depends on 1)

The laminated article of claim 1, wherein the first substrate and the second substrate are independently selected from a spunbond polypropylene, a spunbond polyamide, a spunbond blend of polyamide and polyester, a spunbond polyethylene, a spunbond polyester, a spunbond polybutylene terephthalate, and a spunbond polypropylene.

### Claim 3 (depends on 1)

The laminated article of claim 1, wherein the first substrate and the second substrate independently comprise a spunbond material comprising a gram per square meter basis weight (gsm) of 10 to 200 gsm, inclusive.

### Claim 4 (depends on 1)

The laminated article of claim 1, wherein the laminated article provides a turbidity of less than 0.2 nephelometric turbidity units (NTU) according to the Turbidity Test.

### Claim 5 (depends on 1)

The laminated article of claim 1, wherein the metal silicate particle is a magnesium silicate particle.

### Claim 6 (depends on 1)

The laminated article of claim 1, wherein each of the first substrate and the second substrate is liquid permeable.

### Claim 7

A method of making a laminated article, the method comprising:
a) providing a plurality of fibers;
b) providing a plurality of guanidine-functionalized metal silicate particles;
c) mixing the plurality of guanidine-functionalized metal silicate particles and the plurality of fibers together to form a porous fibrous nonwoven matrix having the guanidine-functionalized metal silicate particles enmeshed within the porous fibrous nonwoven matrix;
d) providing a first substrate;
e) providing a second substrate;
f) disposing the porous fibrous nonwoven matrix having the guanidine-functionalized metal silicate particles between the first substrate and the second substrate; and
g) sealing the second substrate to the first substrate along at least a portion of a perimeter of the first substrate.

### Claim 8 (depends on 7)

The method of claim 7, wherein the providing a plurality of guanidine-functionalized metal silicate particles comprises:
i) reacting an O-methylisourea salt with a linker comprising the formula
X3-nRanSi—Y—NH2,
wherein:
n is 0, 1, or 2;
each Ra, if present, is independently an alkyl, aralkyl, or aryl;
Y is a divalent group comprising an alkylene having 2 to 20 carbons; and
each X is independently alkoxy or acyloxy;
to form a guanidine-functionalized linker; and
ii) forming a mixture of the guanidine-functionalized linker and metal silicate particles, such that the guanidine-functionalized linker reacts with hydroxyl groups of the metal silicate particles to form covalent bonds between the guanidine-functionalized linker and the metal silicate particles, thereby forming the guanidine-functionalized metal silicate particles.

### Claim 9 (depends on 7)

The method of claim 7, wherein the sealing is performed using ultrasonic sealing, heat sealing, adhesive sealing, stitching, or a combination thereof.

### Claim 10 (depends on 7)

The method of claim 7, further comprising mixing at least one polymeric binder together with the plurality of guanidine-functionalized metal silicate particles and the plurality of fibers.

### Claim 11

A method of removing microorganisms from a fluid sample, the method comprising:
a) providing a laminated article, the laminated article comprising:
1) a porous fibrous nonwoven matrix;
2) a plurality of guanidine-functionalized metal silicate particles enmeshed within the porous fibrous nonwoven matrix, the guanidine-functionalized metal silicate particles comprising:
a metal silicate particle that is modified with at least one silane having the formula
X3-nRanSi—Y-G
wherein:
n is 0, 1, or 2;
each Ra, if present, is independently an alkyl, aralkyl, or aryl;
Y is a divalent group comprising an alkylene having 2 to 20 carbons;
G is a guanidine group of the formula —NH—C(═NH)—NH2; and
each X is independently alkoxy or acyloxy;
3) a first substrate; and
4) a second substrate sealed to the first substrate along at least a portion of a perimeter of the first substrate, wherein the porous fibrous nonwoven matrix is disposed between the first substrate and the second substrate;
b) providing a fluid sample containing at least one microorganism strain; and
c) contacting the fluid sample with the laminated article such that at least a portion of the at least one microorganism strain is removed from the fluid sample.

### Claim 12 (depends on 11)

The method of claim 11, wherein the contacting comprises passing the fluid sample at least once through the laminated article.

### Claim 13 (depends on 12)

The method of claim 12, wherein the contacting comprises passing the fluid sample through the laminated article at a pressure of 4.0 pounds per square inch (psi) (27.58 kilopascals (kPa)) or less.

### Claim 14 (depends on 11)

The method of claim 11, wherein the laminated article reduces the amount of microorganism in the fluid sample by at least a factor of 100.

### Claim 15

A filtration device comprising:
a) a container having inlet and outlet ports for liquid passage; and
b) a laminated article contained within the container, the laminated article comprising:
1) a porous fibrous nonwoven matrix;
2) a plurality of guanidine-functionalized metal silicate particles enmeshed within the porous fibrous nonwoven matrix, the guanidine-functionalized metal silicate particles comprising:
a metal silicate particle that is modified with at least one silane having the formula
X3-nRanSi—Y-G
wherein:
n is 0, 1, or 2;
each Ra, if present, is independently an alkyl, aralkyl, or aryl;
Y is a divalent group comprising an alkylene having 2 to 20 carbons;
G is a guanidine group of the formula —NH—C(═NH)—NH2; and
each X is independently alkoxy or acyloxy;
3) a first substrate; and
4) a second substrate sealed to the first substrate along at least a portion of a perimeter of the first substrate, wherein the porous fibrous nonwoven matrix is disposed between the first substrate and the second substrate.