# US 8,784,693 B2 · Method for making phosphorated composite

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- Number: US 8,784,693 B2
- Document ID: US8784693B2
- Status: Granted
- Kind: B2
- Application number: 13/711,427
- Filed: 2012-12-11
- Published: 2013-04-25
- Granted: 2014-07-22
- Earliest claimed: 2009-03-18
- Assignees: Tsinghua University; Hon Hai Precision Industry Co., Ltd.
- Applicants: Tsinghua University; Hon Hai Precision Industry Co., Ltd.
- Inventors: Li Wang; Xiang-Ming He; Jian-Guo Ren; Wei-Hua Pu; Jian-Jun Li; Jian Gao
- Web page: https://patentgrep.com/patent/US8784693B2

## CPC

- H01M 4/604: {containing aliphatic main chain polymers}
- C08F 8/40: Introducing phosphorus atoms or phosphorus-containing groups
- C08K 3/04: Carbon
- C08K 3/32: Phosphorus-containing compounds
- H01M 4/60: of organic compounds
- H01M 4/625: {Carbon or graphite}
- C08F 2810/30: leading to the formation or introduction of aliphatic or alicyclic unsaturated groups
- H01M 10/0525: Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
- Y02E 60/10: Energy storage using batteries
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- C08F: MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## Abstract

A method for making a phosphorated composite is provided. First, a mixture is obtained by mixing a source material with red phosphorus. The weight ratio of the source material to the red phosphorus ranges from about 1:10 to about 5:1. Second, the mixture is dried in an inert atmosphere or vacuum. Third, the mixture is heated in a reacting room filled with an inert atmosphere so that the red phosphorus sublimes. Finally, the reacting room is cooled down.

## Claims

### Claim 1

A method for making a phosphorated composite, the method comprising:
mixing a source material with red phosphorus to obtain a mixture, wherein a weight ratio of the source material to the red phosphorus ranges from about 1:10 to about 5:1; and
heating the mixture in a reacting room filled with an inert atmosphere so that the red phosphorus sublimes to form sublimed red phosphorous.

### Claim 2 (depends on 1)

The method of claim 1, wherein the source material is a polymer, and the polymer changes into a conductive polymer under catalysis of the red phosphorus and forms an in situ composite with the red phosphorus.

### Claim 3 (depends on 2)

The method of claim 2, wherein the polymer is selected from the group consisting of polypropylene, polyacrylonitrile, polystyrene, polyethylene oxide, polyvinyl alcohol, polyvinylidenechloride, polyvinylidene fluoride, polyvinyl fluoride, polyvinyl chloride, poly1,2-chloride ethylene, poly1,2-fluoride ethylene, polymethyl methacrylate, and phenolic resin.

### Claim 4 (depends on 2)

The method of claim 2, wherein the polymer is polyacrylonitrile, a heating temperature is about 500° C., and a heating time is about 12 hours.

### Claim 5 (depends on 2)

The method of claim 2, wherein the polymer is polyvinylidene chloride, a heating temperature is about 450° C., and a heating time is about 3 hours.

### Claim 6 (depends on 1)

The method of claim 1, wherein the source material is an organic matter, and the organic matter changes into a conductive amorphous carbon by dehydrogenation and form an in situ composite with the red phosphorus.

### Claim 7 (depends on 6)

The method of claim 6, wherein the organic matter is selected from the group consisting of cellulose and sugar.

### Claim 8 (depends on 1)

The method of claim 1, wherein the source material is a conductive carbonaceous material, and the conductive carbonaceous material absorbs the sublimed red phosphorus to form the phosphorated composite.

### Claim 9 (depends on 8)

The method of claim 8, wherein the conductive carbonaceous material is selected from the group consisting of active carbon, acetylene black, conductive graphite, and conductive amorphous carbon.

### Claim 10 (depends on 8)

The method of claim 8, wherein the conductive carbonaceous material is conductive graphite, a heating temperature is about 600° C. and a heating time is about 6 hours.

### Claim 11 (depends on 8)

The method of claim 8, wherein the conductive carbonaceous material is active carbon, a heating temperature is about 470° C. and a heating time is about 6 hours.

### Claim 12

A method for making a phosphorated composite, the method comprising steps of:
step (a), mixing a source material with red phosphorus to obtain a mixture, wherein a weight ratio of the source material to the red phosphorus ranges from about 1:10 to about 5:1;
step (b), drying the mixture in a first inert atmosphere or vacuum;
step (c), heating the mixture in a reacting room filled with a second inert atmosphere so that the red phosphorus sublimes to form sublimed red phosphorus; and
step (d), cooling the reacting room down.

### Claim 13 (depends on 12)

The method of claim 12, wherein in step (b), a drying temperature ranges from about 50° C. to about 120° C.

### Claim 14 (depends on 12)

The method of claim 12, wherein the source material is a polymer, and in step (c) the polymer changes into a conductive polymer under catalysis of the red phosphorus and forms an in situ composite with the red phosphorus.

### Claim 15 (depends on 14)

The method of claim 14, wherein the polymer is selected from the group consisting of polypropylene, polyacrylonitrile, polystyrene, polyethylene oxide, polyvinyl alcohol, polyvinylidenechloride, polyvinylidene fluoride, polyvinyl fluoride, polyvinyl chloride, poly1,2-chloride ethylene, poly1,2-fluoride ethylene, polymethyl methacrylate, and phenolic resin.

### Claim 16 (depends on 12)

The method of claim 12, wherein the source material is an organic matter, and in step (c) the organic matter changes into a conductive amorphous carbon by dehydrogenation and form an in situ composite with the red phosphorus.

### Claim 17 (depends on 16)

The method of claim 16, wherein the organic matter is selected from the group consisting of cellulose and sugar.

### Claim 18 (depends on 12)

The method of claim 12, wherein the source material is a conductive carbonaceous material, and in step (c) the conductive carbonaceous material absorbs the sublimed red phosphorus to form the phosphorated composite.

### Claim 19 (depends on 18)

The method of claim 18, wherein the conductive carbonaceous material is selected from the group consisting of active carbon, acetylene black, conductive graphite, and conductive amorphous carbon.

### Claim 20 (depends on 12)

The method of claim 12, wherein in step (c), a heating temperature ranges from about 250° C. to about 600° C.