# US 4,399,237 A · Vesiculated polymer granules containing TiO.sub.2

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- Number: US 4,399,237 A
- Document ID: US4399237A
- Status: Granted
- Kind: A
- Application number: 06/441,756
- Filed: 1982-11-15
- Granted: 1983-08-16
- Earliest claimed: 1982-11-15
- Assignees: E. I. Du Pont de Nemours and Company
- Inventors: William H. Morrison, Jr.
- Web page: https://patentgrep.com/patent/US4399237A

## CPC

- C08J 9/283: {a discontinuous liquid phase emulsified in a continuous macromolecular phase}
- C08J 3/16: by coagulating dispersions {(C08J3/122 takes precedence)}
- C08J 3/215: at least one additive being also premixed with a liquid phase
- C08J 2367/06: Unsaturated polyesters
- C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29)

## Abstract

Vesiculated polymer granules having high refractive indices can be made from an aqueous slurry of particulate TiO.sub.2 if the slurry contains a phosphate ester.

## Claims

### Claim 1

A vesiculated pigment granule having a diameter of 1-50 microns, the granule comprising
(a) 1-60%, by weight, of TiO.sub.2 particles in a matrix of an unsaturated polyester resin cross-linked with a polymerizable unsaturated monomer,
(b) 5-95%, by volume, of voids, and
(c) 0.5-4.0%, by weight of the TiO.sub.2, of a phosphate ester represented by the structure
(R--O--(CH.sub.2).sub.y ].sub.n O).sub.x PO.sub.4-x Z.sub.3-x
where
R is an aliphatic hydrocarbon radical of 4-16 carbon atoms, an octylphenol radical or a nonylphenyl radical,
n is 4-12,
x is 1 or 2,
y is 2 or 3, and
z is H, Na or K.

### Claim 2 (depends on 1)

The granule of claim 1 in which the phosphate ester is a 75/25 weight mixture of esters represented by the structure
C.sub.10 H.sub.21 --OCH.sub.2 CH.sub.2).sub.6 OPO.sub.3 H.sub.2
and
[C.sub.10 H.sub.21 --OCH.sub.2 CH.sub.2 --.sub.6 O].sub.2 PO.sub.2 H.

### Claim 3 (depends on 1)

An aqueous slurry of granules according to claim 1.

### Claim 4 (depends on 2)

An aqueous slurry of granules according to claim 2.

### Claim 5 (depends on 1)

A coating composition comprising granules according to claim 1, a film-forming component and a liquid carrier.

### Claim 6 (depends on 2)

A coating composition comprising granules according to claim 2, a film-forming component and a liquid carrier.

### Claim 7 (depends on 1)

A method for preparing granules according to claim 1, the method comprising
(a) adding 0.5-4.0% of a phosphate ester represented by the structure
(R--O--(CH.sub.2).sub.y ].sub.n O).sub.x PO.sub.4-x Z.sub.3-x
where
R is an aliphatic hydrocarbon radical of 4-16 carbon atoms, an octylphenyl radical or a nonylphenol radical,
n is 4-12,
x is 1 or 2,
y is 2 or 3, and
z is H, Na or K, to an aqueous slurry of TiO.sub.2 particles which contains a hydrophilic surfactant stabilizer,
(b) forming a water-in-solution emulsion of the slurry in a solution of an unsaturated polyester resin in a liquid polymerizable unsaturated monomer cross-linking agent, and
(c) emulsifying the emulsion in (b) in water to form a slurry of the granules in water.

### Claim 8 (depends on 7)

The method of claim 7 having the additional step of separating the granules from the slurry.