# US 11,304,880 B2 · Glass ionomer compositions and methods including water-miscible, silane-treated, nano-sized silica particles

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- Number: US 11,304,880 B2
- Document ID: US11304880B2
- Status: Granted
- Kind: B2
- Application number: 16/613,368
- Filed: 2018-05-09
- Published: 2020-03-05
- Granted: 2022-04-19
- Earliest claimed: 2017-05-18
- Assignees: 3M Innovative Properties Company
- Applicants: 3M Innovative Properties Company
- Inventors: Mark B. Agre; Bradley D. Craig; Michael Jahns; Adrian S. Eckert
- Web page: https://patentgrep.com/patent/US11304880B2

## CPC

- A61K 6/889: Polycarboxylate cements; Glass ionomer cements
- A61K 6/17: Particle size
- A61K 6/54: Filling; Sealing
- A61K 6/816: comprising titanium oxide
- A61K 6/818: comprising zirconium oxide
- A61K 6/831: comprising non-metallic elements or compounds thereof, e.g. carbon
- C03C 3/062: with less than 40% silica by weight
- C03C 4/0021: {for dental use}
- A61K: PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES (devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms A61J3/00; chemical aspects of, or use of materials for deodorisation of air, for disinfection or sterilisation, or for bandages, dressings, absorbent pads or surgical articles A61L; soap compositions C11D)
- C03C: CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS

## Abstract

Disclosed herein are curable glass ionomer compositions that include a first paste and a second paste, and methods for using the disclosed compositions. The first paste includes water, a polyacid, and a non acid-reactive filler. The second paste includes water, an acid-reactive filler; and non-aggregated, water-miscible, nano-sized silica particles having at least 25% surface coverage of the particles with a silane. The composition is essentially free of a resin. In some embodiments, the water content of the first paste and the second paste of the paste/paste GI composition disclosed herein is less than 20% by weight, based on the total weight of the composition.

## Claims

### Claim 1

A curable glass ionomer composition comprising:
a first paste comprising:
water,
a polyacid, and
a non acid-reactive filler; and
a second paste comprising:
water,
an acid-reactive filler; and
non-aggregated, water-miscible, nano-sized silica particles having at least 25% surface coverage of the particles with a silane;
wherein the composition is essentially free of a resin.

### Claim 2 (depends on 1)

The composition of claim 1, or wherein the silane is essentially free of unsaturated polymerizable groups.

### Claim 3 (depends on 1)

The composition of claim 1, wherein the silane is represented by the formula:
(R1O)3—Si—(CH2)n—(O—R2)x—OR3,
wherein:
R1 is a C1-C3 alkyl group;
R2 is a C2-C3 alkylene group;
R3 is a C1-C10 alkyl group or 2,3-epoxypropyl;
n=2 to 6; and
x=0 to 200.

### Claim 4 (depends on 3)

The composition of claim 3, or wherein R2 represents —CH2CH2—.

### Claim 5 (depends on 3)

The composition of claim 3, wherein n=3.

### Claim 6 (depends on 1)

The composition of claim 1, wherein the non-aggregated, water-miscible, nano-sized silica particles are substantially free of fumed silica.

### Claim 7 (depends on 1)

The composition of claim 1, wherein at least one of the first paste and the second paste further comprises pyrogenic silica particles.

### Claim 8 (depends on 1)

The composition of claim 1, wherein the water content of the first paste and the second paste combined is less than 20% by weight, based on the total weight of the composition.

### Claim 9 (depends on 1)

The composition of claim 1, wherein the non acid-reactive filler comprises particles and/or fibers.

### Claim 10 (depends on 1)

The composition of claim 1, wherein the non acid-reactive filler is selected from the group consisting of quartz, nitrides, kaolin, borosilicate glass, strontium oxide based glass, barium oxide based glass, silica, alumina, titania, zirconia, and combinations thereof.

### Claim 11 (depends on 1)

The composition of claim 1, wherein the non acid-reactive filler comprises substantially crystalline inorganic fibers.

### Claim 12 (depends on 11)

The composition of claim 11, wherein the substantially crystalline inorganic fibers comprise ceramics and/or metal oxides.

### Claim 13 (depends on 11)

The composition of claim 11, wherein the substantially crystalline inorganic fibers have a crystallinity index of at least 0.05 as measured by the XRD Crystallinity Index Test Method.

### Claim 14 (depends on 1)

The composition of claim 1, wherein the acid-reactive filler comprises an inorganic filler selected from the group consisting of basic metal oxides, metal hydroxides, hydroxyapatite, aluminosilicate glasses, fluoroaluminosilicate glasses, glasses having a Si/Al weight percent ratio less than 1.5, and combinations thereof.

### Claim 15 (depends on 1)

The composition of claim 1, wherein the acid-reactive filler has a mean particle size of 3 micrometers to 10 micrometers.

### Claim 16 (depends on 1)

The composition of claim 1, wherein the first paste further comprises a complexing agent.

### Claim 17 (depends on 1)

The composition of claim 1, wherein the composition remains sufficiently workable or mixable to form a curable glass ionomer composition after storage at room temperature for at least one month.

### Claim 18 (depends on 1)

The composition of claim 1, wherein the composition remains sufficiently workable or mixable to form a curable glass ionomer composition after storage at room temperature for at least three months.

### Claim 19 (depends on 1)

A method of preparing a cured composition comprising:
providing a curable glass ionomer composition of claim 1;
combining the first paste and the second paste to form a mixture; and
allowing the mixture to cure to form the cured composition.

### Claim 20 (depends on 1)

A device for storing a composition of claim 1, the device comprising:
a first compartment containing the first paste; and
a second compartment containing the second paste.
