# US 12,006,215 B2 · Method of carbonizate purification

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- Number: US 12,006,215 B2
- Document ID: US12006215B2
- Status: Granted
- Kind: B2
- Application number: 17/048,589
- Filed: 2019-04-15
- Published: 2021-05-27
- Granted: 2024-06-11
- Earliest claimed: 2018-04-17
- Assignees: Syntoil Spolka Akcyjna
- Applicants: Syntoil SpółKa Akcyjna
- Inventors: Marcin Banach; Jolanta Pullit-Prociak
- Web page: https://patentgrep.com/patent/US12006215B2

## CPC

- C01B 32/05: Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
- C09C 1/482: {Preparation from used rubber products, e.g. tyres (recovery of plastics or other constituents of waste material containing plastics B29B17/00)}
- C10G 1/10: from rubber or rubber waste
- C10L 9/10: by using additives
- C01P 2004/61: Micrometer sized, i.e. from 1-100 micrometer
- C01P 2006/80: Compositional purity
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- C09C: TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES (treatment of materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone C04B14/00, C04B18/00, C04B20/00); PREPARATION OF CARBON BLACK {; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS}
- C10G: CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION (cracking to hydrogen or synthesis gas C01B; cracking or pyrolysis of hydrocarbon gases to individual hydrocarbons or mixtures thereof of definite or specified constitution C07C; cracking to cokes C10B); RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10L: FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G OR C10K; LIQUIFIED PETROLEUM GAS; USE OF ADDITIVES TO FUELS OR FIRES; FIRE-LIGHTERS
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

A method of purification of carbonizate resulting from the thermal recycling process of rubber waste consists in that the carbonizate is mixed with sodium bicarbonate, then deionized water having increased temperature and strong mineral acid and/or mixture of mineral acids are introduced into the obtained mixture, and next the whole is stirred at increased temperature, and filtered at decreased pressure while washing with deionized water having increased temperature, the filtrate is discarded, the solution of a strong base is introduced into the solid residue, and the whole is stirred at increased temperature, then the obtained suspension is filtered at decreased pressure, and washed with deionized water having increased temperature, and next the filtrate is discarded, and the solid residue is dried.

## Claims

### Claim 1

A method of purification of carbonizate resulting from the thermal recycling process of rubber waste, characterized in that the carbonizate is mixed with sodium bicarbonate, then deionized water having increased temperature and strong mineral acid and/or mixture of mineral acids are introduced into the obtained mixture, and next the whole is stirred at increased temperature from 70 to 95° C., and filtered at decreased pressure while washing with deionized water having increased temperature, the filtrate is discarded, the solution of a strong base is introduced into the solid residue, and the whole is stirred at increased temperature, then the obtained suspension is filtered at decreased pressure, and washed with deionized water having increased temperature, and next the filtrate is discarded, and the solid residue is dried.

### Claim 2 (depends on 1)

The method according to claim 1, characterized in that the mixing of carbonizate with sodium bicarbonate is carried out wet or dry.

### Claim 3 (depends on 2)

The method according to claim 2, characterized in that the mixing of carbonizate with sodium bicarbonate is carried from 10 to 100 minutes.

### Claim 4 (depends on 1)

The method according to claim 1 characterized in that the hydrochloric acid or sulphuric (IV) acid and/or hydrofluoric acid and/or their mixture is used.

### Claim 5 (depends on 1)

The method according to claim 1, characterized in that the granulation of the carbonizate is from 0.02 to 0.3 millimeters.

### Claim 6 (depends on 1)

The method according to claim 1, characterized in that the mass ratio of sodium bicarbonate to carbonizate is from 0.3 to 1.5.

### Claim 7 (depends on 1)

The method according to claim 1, characterized in that the mass ratio of hydrochloric acid to raw carbonizate is from 0.5 to 2.0.

### Claim 8 (depends on 1)

The method according to claim 1, characterized in that the concentration of hydrochloric acid in the reaction mixture is from 2 to 10%.

### Claim 9 (depends on 1)

The method according to claim 1, characterized in that the mass ratio of sulphuric (IV) acid to carbonizate is from 2 to 10.

### Claim 10 (depends on 1)

The method according to claim 1, characterized in that the concentration of sulphuric (IV) acid in the reaction mixture is from 13 to 40%.

### Claim 11 (depends on 1)

The method according to claim 1, characterized in that the mass ratio of hydrofluoric acid to carbonizate is from 1 to 5.

### Claim 12 (depends on 1)

The method according to claim 1, characterized in that the concentration of hydrofluoric acid in the reaction mixture is from 7 to 20%.

### Claim 13 (depends on 1)

The method according to claim 1, characterized in that the strong base used is sodium hydroxide, ammonia water and/or their mixture.

### Claim 14 (depends on 1)

The method according to claim 1, characterized in that the mass ratio of sodium hydroxide to carbonizate is from 5 to 15.

### Claim 15 (depends on 1)

The method according to claim 1, characterized in that the concentration of sodium hydroxide in the etching solution is from 30 to 50%.

### Claim 16 (depends on 1)

The method according to claim 1, characterized in that the mass ratio of ammonia to raw carbonizate is from 0.5 to 2.

### Claim 17 (depends on 1)

The method according to claim 1, characterized in that the concentration of ammonia in the etching solution is from 1 to 25%.

### Claim 18 (depends on 1)

The method according to claim 1, characterized in that the time of stirring the mixture of carbonizate with sodium bicarbonate with the solution of acid and/or mixture of mineral acids and with the solution of base and/or mixture of bases is from 15 to 90 minutes.

### Claim 19 (depends on 1)

The method according to claim 1, characterized in that the solid residue is dried at the temperature from 90 to 120° C.
