WO1993006837A1

WO1993006837A1 - Process for preparing pvp-iodine product

Info

Publication number: WO1993006837A1
Application number: PCT/US1992/006921
Authority: WO
Inventors: John J. Merianos; Paul Garelick
Original assignee: ISP Investments LLC
Current assignee: ISP Investments LLC
Priority date: 1991-10-08
Filing date: 1992-08-21
Publication date: 1993-04-15
Anticipated expiration: 1994-04-08
Also published as: AU2511392A

Abstract

A proces for preparing a water-insoluble or water-soluble PVP-iodine product which comprises intimately mixing water-insoluble PVP or water-soluble PVP having a K-value of 10-20, about 10 to 20 % by weight of iodine powder and about 0.05 to 1 % by weight of isopropanol, heating the reaction mixture at a mixing temperature of room temperature to about 30-60 °C for about 0.5 to 6 hours, and heating the mixture at a reaction temperature of about 65 to 98 °C for about 10-24 hours, generally at least 18 hours, to form a stable, uniform, free-flowing powder.

Description

PROCESS FOR PREPARING PVP-IODINE PRODUCT

A process is described herein for preparing a uniform, free-flowing water-insoluble or water soluble PVP-iodine product which comprises intimately mixing water-insoluble or water soluble PVP of K-value 10-20, about 10 to 20% by weight iodine powders and about 0.05 to 1% by weight of isopropanol, heating the reaction mixture at a mixing temperature of from room temperature to about 30-60°C. for about 0.5 to 6 hours, until the reactants disappear as a separate phase, and heating the mixture at a reaction temperature of about 65 to 98°C. for about 10-24 hours, generally at least 18 hours, thereby forming a uniform, free-flowing powder.

The water-insoluble and water-soluble PVP starting materials are available from International Specialty Products Inc. (ISP) .

The process of preparing water-insoluble PVP-iodine involves preparing reaction powders by intimately mixing crospovidone, about 10 to 20% by wt. of iodine and about 0.5 to 1% by wt. of isopropanol, heating at a mixing temperature of about 30-60°C. for about 0.5-6 hours, and then heating the mixture at a reaction temperature of about 75-98°C. for about 10-24 hours, to form a uniform, free-flowing powder having an available iodine content of about 9-13% and an iodide content of about 4-6%. Representative reaction mixtures, process conditions and properties of the reaction product obtained by such process are shown in the TABLE below.

TABLE 1

Suitable Preferred Optimum

The invention will now be illustrated by the following example.

* Polyplasdone^® (ISP) EXAMPLE 1

50 g. of Polyplasdone^® (ISP) 10 g. of iodine (Japan crushed, 99.5%), and 0.12 g. isopropanol are charged into a pint-wide mouth glass jar with a Teflon-lined lid, and having a Teflon plate and wall indentations for effective baffling. The charged jars were placed in a forced air oven equipped with a motor driven rotary cage to allow rotation of the jars at 40 rpm. The reaction mixture in the jars were hand mixed for about 1/2 minute to disperse the iodine therein, and then the isopropanol was added dropwise, mixed again for 1/2 minute, rotated in the oven at 45°C. for 3 hours, and then heated at 90°C. for 16 hours. A yellow-brown, free-flowing powder was obtained. The available iodine content of the product was 12.15%; the iodide content was 4.45%; and the moisture content was 2.37%. The product lost was less than 10% iodine after heating at 75°C. for 6 hours.

The water-soluble PVP-iodine product of the invention is prepared by reacting 80-90% by wt. water-soluble PVP with 10-20% by wt. iodine at a temperature of about 65-85°C. , preferably about 75°C. , for a period of at least about 18 hours, and, in the presence of a small amount, e.g. 0.1-0.2, preferably, 0.2%, of isopropanol.

The parameters of the process of the invention, and the product produced thereby are summarized in the Table below. TABLE 2

Reaction Mixture and Ranges Process Conditions Suitable Preferred Optimum

Water-Soluble PVP (K = 10-20) I₂ C by wt.) Isopropanol (% by wt.) Room Temperature Mixing (hrs.) Reaction Temp (°C.)

Reaction Time (hrs.) at least 12 > 16 16-22

Reaction Product

K-Value 10-20 13-17 15

Avail I₂ (% by wt.) 9-13 10.5-11.5 11

Iodide (% by wt.) 4-6 4.5-5.5 5

Partition Coefficient >150 180-220 200

EXAMPLE 2

60 g. of water-soluble PVP (K-value 12-20) powder, 12.0 g. of iodine powder and 0.144 g. of isopropanol were mixed in a jar and the mixture was rotated with a motor driven rotary cage at 40 rpm at room temperature for 3-16 hours. The iodine powders disappeared as a separate phase and the reaction mixture was a uniform, nearly black powder which was flowable. This mixture then was rotated continuously at 75°C. for 22 hours. The product was a uniform, free-flowing, reddish-brown powder. The available iodine content was 10.99%, the iodide content was 4.80%; and the moisture content was 3.14%.

Stability was measured by % iodine loss after 6 hours at 75°C. from a 1% available iodine solution, only 3.64% of available iodine was lost. The partition coefficient of the product was 148.

Claims

WHAT IS CLAIMED IS:

1. A process for preparing a water-insoluble or water-soluble PVP-iodine product which comprises intimately mixing about 80 to about 90% by wt. of water-insoluble or water-soluble PVP, having a K-value of about 10-20, about 10 to about 20% by wt. iodine powders and about 0.05 to about 1% by wt. of isopropanol, heating the reaction mixture at a mixing temperature of from room temperature to about 30 to about 60°C. for about 0.5 to 6 hours, and heating the mixture at a reaction temperature of about 65 to about 98°C. for about 10 to about 24 hours, thereby forming a stable, uniform, free-flowing powder.

2. A process according to claim 1 wherein the water-insoluble product has an available iodine content of about 9 to about 13% and an iodide content of about 4 to about 6%.

3. A process according to claim 1 wherein iodine is charged in an amount of about 15-19% by wt.

4. A process according to claim 1 wherein isopropanol is charged in an amount of about 0.1-0.5% by wt.

5. A process according to claim 1 wherein said reaction temperature is about 85-95°C. and the reaction time is about 12-20 hours.

6. A process according to claim 1 wherein the product has an available iodine content of about 10 to 12% and an iodide content of about 4.5 to 5.5%.

7. A process according to claim 1 wherein the mixing temperature is about 35-55°C. and the mixing time is about 1-5 hours.

8. A process according to claim 1 wherein the moisture content of the product is about 1-5% by wt.

9. A process according to claim 1 wherein the iodine charge is 17% by wt. , the isopropanol is about 0.2% by wt., the mixing temperature is about 45°C, the mixing time is about 3 hours, the reaction temperature, is about 90°C, the reaction time is about 16 hours, and wherein the reaction product has about 11% by wt. available iodine, about 5% by wt. iodide and about 2% by wt. moisture.