CN108384287A - A method of preparing colour carbon black using waste tire - Google Patents
A method of preparing colour carbon black using waste tire Download PDFInfo
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- CN108384287A CN108384287A CN201810137664.0A CN201810137664A CN108384287A CN 108384287 A CN108384287 A CN 108384287A CN 201810137664 A CN201810137664 A CN 201810137664A CN 108384287 A CN108384287 A CN 108384287A
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- carbon black
- waste tire
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/482—Preparation from used rubber products, e.g. tyres
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- Organic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The present invention relates to a kind of methods preparing colour carbon black using waste tire, belong to waste reutilization technology field.The present invention carries out mixing and ball milling using waste tire as raw material, with auxiliary agent, and pyrolysis then is mixed through sodium hydroxide solution, glacial acetic acid, then carries out hybrid reaction with dimethylformamide, tyrosine etc., low-temperature oxidation is finally carried out, to prepare colour carbon black.The present invention takes full advantage of waste tire, avoids environmental pollution and the wasting of resources, when also avoiding carbon black and carrying out high-temperature oxydation, the problem of reducing the oxygen content of carbon blacksurface, it is made to be aoxidized at low temperature.
Description
Technical field
The present invention relates to a kind of methods preparing colour carbon black using waste tire, belong to waste reutilization technology neck
Domain.
Background technology
In the prior art, as the rapid development of auto industry, car ownership sharply increase, thus lead to waste tire
Amount is also being continuously increased.According to relevant information, waste tire is discarded substantially generally after renovating use twice, thus
So that a large amount of waste tires stockpile.Obviously, if effective recycling is not realized to waste tire, then will not only cause rubber
The significant wastage of glue resource, but also enormous pressure will be caused to environmental protection, in a natural environment, waste tire is to environment
Pollution is decades.Therefore, the research of waste tire recovery technology is at present by the most attention of countries in the world government, such as
What low energy consumption, efficient exploitation waste tire rubber recycling new technology are a urgent problems to be solved.Currently, domestic and international powder
Mainly there is method used by broken waste tire:Freezing, normal temperature crushing up, high-pressure process and solvent soak method etc. of quenching.It is external main
Liquid nitrogen frozen comminuting method is taken, after this method introduces China, due in liquid nitrogen storage and transport, tire merging and fragment taking-up etc.
Aspect is all relatively difficult, thus causes the crushing cost of waste tire higher, and enterprise using the technology when carrying out tire crushing
It is difficult to maintain normal production.
Colour carbon black is prepared currently with carbon black and mostly uses high-temperature oxidation, but as oxidizing temperature increases, carbon blacksurface
Carboxyl can be gradually decomposed into CO and CO2Volatilization is generated, takes away the oxygen of carbon blacksurface, it is believed that the carbon black table aoxidized under hot conditions
Face is coarse and porous, can reduce the oxygen content of carbon blacksurface instead.
Invention content
The technical problems to be solved by the invention:It cannot be fully utilized, result in waste of resources for current waste tire,
And processing cost is high, while during preparing colour carbon black at present, due to the presence of high temperature, easily causes the oxygen-containing of carbon blacksurface
The problem of amount reduces.
In order to solve the above technical problems, the present invention is using technical solution as described below:
A method of colour carbon black being prepared using waste tire, which includes the following steps:
(1)It takes waste tire to crush, is sieved, collect sieving particle, by sieving particle, auxiliary agent in mass ratio 7:1~3, it puts
Enter in ball mill with 300r/min 20~30min of ball milling, the acetone of sieving granular mass 15~20% is added, with 400r/min
45~50min of ball milling collects ball milling object;
(2)Ball milling object is put into reactor, the gas in reactor is discharged using carbon dioxide, is warming up to 756~763 DEG C
Under be pyrolyzed, then be down to room temperature, collect pyrolyzed mixture, pyrolyzed mixture is placed at 10~15 DEG C and is stood;
(3)After standing, by the pyrolyzed mixture and sodium hydroxide solution in mass ratio 1 after standing:4 progress ultrasounds are shaken
It swings, is put into container, using nitrogen protection, the glacial acetic acid of sodium hydroxide solution volume 40~45% is added, at 80~90 DEG C
Lower stirring;
(4)After stirring, stirring mixture is collected, freeze-drying collects dried object, counts in parts by weight, take 90~105
Part dimethylformamide, 40~45 parts of dried objects, 23~27 parts of tetraphenylporphyrins, 20~25 parts of methanol, 18~22 parts of tyrosine,
7~13 parts of additives, 2~4 parts of salicylic acids and 1~3 part of tannin;
(5)Dimethylformamide, dried object and tetraphenylporphyrin are put into reaction kettle first, added at 145~155 DEG C
1~2h of heat, adds methanol, additive continues 3~5h of heating, is cooled to 40~45 DEG C, and tyrosine and tannin, heat preservation 2 is added
~5h;
(6)It after heat preservation, discharges, is spray-dried while hot, collect spray-dried product, washing collects washings, and is put into appearance
In device, it is filled with oxygen, is pressurized to 1.5~1.7MPa, 4~6h is stirred at 70~80 DEG C, stirring thing is collected, mills, collects and grinds
Object is ground to get colour carbon black.
The step(1)Middle auxiliary agent is in mass ratio 4:1~3, sodium carbonate and ferric sulfate are mixed.
The additive is nitrobenzene, boric acid in mass ratio 7:1 mixes.
Compared with other methods, advantageous effects are the present invention:
(1)The present invention selects waste tire to act on raw material, on the one hand realizes making full use of for resource, on the other hand also reduces
The production cost of colour carbon black, first crushes waste tire, and carries out ball milling with auxiliary agent, and auxiliary agent is made in mechanical milling process
It takes disciplinary action and contacts with waste tire particle, and part carries out physical combination with particle, then be pyrolyzed at high temperature, in heat
Solution preocess is thermally decomposed due to sodium carbonates' presence in auxiliary agent, is released carbon dioxide and is carried out pore-creating to it, increases adsorptivity
Can, and ferric sulfate is adsorbed or is attached to the interior outside of pyrogen, so that it is impregnated with sodium hydroxide solution, is making iron
Ion is combined to be formed with hydroxyl, forms iron hydroxide, is that glacial acetic acid is reacted, and forms ferric acetate, is then adding
Under the action of adding agent, tetraphenylporphyrin iron complex is formed with tetraphenylporphyrin, then be combined with tyrosine and tannin, passed through
Tannin makes culture be combined with tyrosine, forms class hemoglobin construct, increases the conjugation with oxygen, avoid height
It temperature lower the problem of carrying out oxygenation, while the addition of tannin also improves the group on colour carbon black surface, further increases and oxygen
Conjugation;
(2)The present invention makes its recycling, avoids environmental pollution and the wasting of resources by taking full advantage of waste tire,
When also avoiding carbon black and carrying out high-temperature oxydation, the problem of reducing the oxygen content of carbon blacksurface, it is made to be aoxidized at low temperature.
Specific implementation mode
The preparation of auxiliary agent:In mass ratio 4:1~3, sodium carbonate and ferric sulfate are mixed.
The preparation of additive:By nitrobenzene, boric acid in mass ratio 7:1 mixes.
A method of colour carbon black being prepared using waste tire, which includes the following steps:
(1)It takes waste tire to clean, crushes, cross 200 mesh sieve, collect sieving particle, in mass ratio by sieving particle, auxiliary agent
7:1~3, it is put into ball mill and adds the acetone of sieving granular mass 15~20% with 300r/min 20~30min of ball milling,
With 400r/min 45~50min of ball milling, ball milling object is collected;
(2)Ball milling object is put into reactor, the gas in reactor is discharged using carbon dioxide, is warming up to 756~763 DEG C
Under carry out 4~7h of pyrolysis, then be down to room temperature, collect pyrolyzed mixture, pyrolyzed mixture is placed at 10~15 DEG C and is stood
40min;
(3)After standing, by the pyrolyzed mixture and sodium hydroxide solution in mass ratio 1 after standing:4 progress ultrasounds are shaken
It swings, is put into container, using nitrogen protection, the glacial acetic acid of sodium hydroxide solution volume 40~45% is added, at 80~90 DEG C
Lower stirring 1h;
(4)After stirring, stirring mixture is collected, freeze-drying collects dried object, counts in parts by weight, take 90~105
Part dimethylformamide, 40~45 parts of dried objects, 23~27 parts of tetraphenylporphyrins, 20~25 parts of methanol, 18~22 parts of tyrosine,
7~13 parts of additives, 2~4 parts of salicylic acids and 1~3 part of tannin;
(5)Dimethylformamide, dried object and tetraphenylporphyrin are put into reaction kettle first, added at 145~155 DEG C
1~2h of heat, adds methanol, additive continues 3~5h of heating, is cooled to 40~45 DEG C, and tyrosine and tannin, heat preservation 2 is added
~5h;
(6)It after heat preservation, discharges, is spray-dried while hot, collect spray-dried product, washed using water, acetone, ethyl alcohol
It washs, collects washings, and be put into container, be filled with oxygen, be pressurized to 1.5~1.7MPa, 4~6h is stirred at 70~80 DEG C,
Stirring thing is collected, is milled 20min with 400r/min, collection mills object to get colour carbon black.
Example 1
The preparation of auxiliary agent:In mass ratio 4:3, sodium carbonate and ferric sulfate are mixed.
The preparation of additive:By nitrobenzene, boric acid in mass ratio 7:1 mixes.
A method of colour carbon black being prepared using waste tire, which includes the following steps:
(1)It takes waste tire to clean, crushes, cross 200 mesh sieve, collect sieving particle, in mass ratio by sieving particle, auxiliary agent
7:3, it is put into ball mill and adds the acetone of sieving granular mass 20% with 300r/min ball milling 30min, with 400r/min balls
50min is ground, ball milling object is collected;
(2)Ball milling object is put into reactor, using carbon dioxide by reactor gas be discharged, be warming up at 763 DEG C into
Row pyrolysis 7h, then it is down to room temperature, pyrolyzed mixture is collected, pyrolyzed mixture is placed at 15 DEG C and stands 40min;
(3)After standing, by the pyrolyzed mixture and sodium hydroxide solution in mass ratio 1 after standing:4 progress ultrasounds are shaken
It swings, is put into container, using nitrogen protection, add the glacial acetic acid of sodium hydroxide solution volume 45%, 1h is stirred at 90 DEG C;
(4)After stirring, stirring mixture is collected, freeze-drying collects dried object, counts in parts by weight, take 105 part two
Methylformamide, 45 parts of dried objects, 23 parts of tetraphenylporphyrins, 25 parts of methanol, 22 parts of tyrosine, 13 parts of additives, 4 parts of salicylic acids
And 3 parts of tannin;
(5)Dimethylformamide, dried object and tetraphenylporphyrin are put into reaction kettle first, heating 2h is carried out at 155 DEG C,
Add methanol, additive continues to heat 5h, be cooled to 45 DEG C, tyrosine and tannin be added, keep the temperature 2~5h;
(6)It after heat preservation, discharges, is spray-dried while hot, collect spray-dried product, washed using water, acetone, ethyl alcohol
It washs, collects washings, and be put into container, be filled with oxygen, be pressurized to 1.7MPa, 6h is stirred at 80 DEG C, collect stirring thing, with
400r/min mills 20min, and collection mills object to get colour carbon black.
Example 2
The preparation of auxiliary agent:In mass ratio 4:2, sodium carbonate and ferric sulfate are mixed.
The preparation of additive:By nitrobenzene, boric acid in mass ratio 7:1 mixes.
A method of colour carbon black being prepared using waste tire, which includes the following steps:
(1)It takes waste tire to clean, crushes, cross 200 mesh sieve, collect sieving particle, in mass ratio by sieving particle, auxiliary agent
7:2, it is put into ball mill and adds the acetone of sieving granular mass 18% with 300r/min ball milling 25min, with 400r/min balls
48min is ground, ball milling object is collected;
(2)Ball milling object is put into reactor, using carbon dioxide by reactor gas be discharged, be warming up at 760 DEG C into
Row pyrolysis 5h, then it is down to room temperature, pyrolyzed mixture is collected, pyrolyzed mixture is placed at 13 DEG C and stands 40min;
(3)After standing, by the pyrolyzed mixture and sodium hydroxide solution in mass ratio 1 after standing:4 progress ultrasounds are shaken
It swings, is put into container, using nitrogen protection, add the glacial acetic acid of sodium hydroxide solution volume 43%, 1h is stirred at 85 DEG C;
(4)After stirring, stirring mixture is collected, freeze-drying collects dried object, counts in parts by weight, take 95 part two
Methylformamide, 43 parts of dried objects, 25 parts of tetraphenylporphyrins, 23 parts of methanol, 20 parts of tyrosine, 10 parts of additives, 3 parts of salicylic acids
And 2 parts of tannin;
(5)Dimethylformamide, dried object and tetraphenylporphyrin are put into reaction kettle first, heated at 150 DEG C
1.5h, adds methanol, additive continues to heat 4h, is cooled to 43 DEG C, tyrosine and tannin is added, keep the temperature 3h;
(6)It after heat preservation, discharges, is spray-dried while hot, collect spray-dried product, washed using water, acetone, ethyl alcohol
It washs, collects washings, and be put into container, be filled with oxygen, be pressurized to 1.6MPa, 4h is stirred at 75 DEG C, collect stirring thing, with
400r/min mills 20min, and collection mills object to get colour carbon black.
Example 3
The preparation of auxiliary agent:In mass ratio 4:1, sodium carbonate and ferric sulfate are mixed.
The preparation of additive:By nitrobenzene, boric acid in mass ratio 7:1 mixes.
A method of colour carbon black being prepared using waste tire, which includes the following steps:
(1)It takes waste tire to clean, crushes, cross 200 mesh sieve, collect sieving particle, in mass ratio by sieving particle, auxiliary agent
7:1, it is put into ball mill and adds the acetone of sieving granular mass 15% with 300r/min ball milling 20min, with 400r/min balls
45min is ground, ball milling object is collected;
(2)Ball milling object is put into reactor, using carbon dioxide by reactor gas be discharged, be warming up at 756 DEG C into
Row pyrolysis 4h, then it is down to room temperature, pyrolyzed mixture is collected, pyrolyzed mixture is placed at 10 DEG C and stands 40min;
(3)After standing, by the pyrolyzed mixture and sodium hydroxide solution in mass ratio 1 after standing:4 progress ultrasounds are shaken
It swings, is put into container, using nitrogen protection, add the glacial acetic acid of sodium hydroxide solution volume 40%, 1h is stirred at 80 DEG C;
(4)After stirring, stirring mixture is collected, freeze-drying collects dried object, counts in parts by weight, take 90 part two
Methylformamide, 40 parts of dried objects, 27 parts of tetraphenylporphyrins, 20 parts of methanol, 18 parts of tyrosine, 7 parts of additives, 2 parts of salicylic acids
And 1 part of tannin;
(5)Dimethylformamide, dried object and tetraphenylporphyrin are put into reaction kettle first, heating 1h is carried out at 145 DEG C,
Add methanol, additive continues to heat 3h, be cooled to 40 DEG C, tyrosine and tannin be added, keep the temperature 2h;
(6)It after heat preservation, discharges, is spray-dried while hot, collect spray-dried product, washed using water, acetone, ethyl alcohol
It washs, collects washings, and be put into container, be filled with oxygen, be pressurized to 1.5MPa, 4h is stirred at 70 DEG C, collect stirring thing, with
400r/min mills 20min, and collection mills object to get colour carbon black.
Comparative example 1
Commercially available colour carbon black.
Colour carbon black in colour carbon black and comparative example 1 prepared by Examples 1 to 3 carries out performance detection, as a result such as table
1。
Table 1
Blackness examination criteria and method:GB/T 7048-2012;Fluidity examination criteria and method GB/T 7052-2012
Tinting strength, tinting power examination criteria and method:GB/T 7050-2003;DBP value examination criteria and method:GB/T 7046-2003.
As seen from the above table, the performance for the more commercially available colour carbon black of colour carbon black that prepared by the present invention is all good.
Claims (3)
1. a kind of method preparing colour carbon black using waste tire, which is characterized in that the preparation method includes the following steps:
(1)It takes waste tire to crush, is sieved, collect sieving particle, by sieving particle, auxiliary agent in mass ratio 7:1~3, it puts
Enter in ball mill with 300r/min 20~30min of ball milling, the acetone of sieving granular mass 15~20% is added, with 400r/min
45~50min of ball milling collects ball milling object;
(2)Ball milling object is put into reactor, the gas in reactor is discharged using carbon dioxide, is warming up to 756~763 DEG C
Under be pyrolyzed, then be down to room temperature, collect pyrolyzed mixture, pyrolyzed mixture is placed at 10~15 DEG C and is stood;
(3)After standing, by the pyrolyzed mixture and sodium hydroxide solution in mass ratio 1 after standing:4 progress ultrasounds are shaken
It swings, is put into container, using nitrogen protection, the glacial acetic acid of sodium hydroxide solution volume 40~45% is added, at 80~90 DEG C
Lower stirring;
(4)After stirring, stirring mixture is collected, freeze-drying collects dried object, counts in parts by weight, take 90~105
Part dimethylformamide, 40~45 parts of dried objects, 23~27 parts of tetraphenylporphyrins, 20~25 parts of methanol, 18~22 parts of tyrosine,
7~13 parts of additives, 2~4 parts of salicylic acids and 1~3 part of tannin;
(5)Dimethylformamide, dried object and tetraphenylporphyrin are put into reaction kettle first, added at 145~155 DEG C
1~2h of heat, adds methanol, additive continues 3~5h of heating, is cooled to 40~45 DEG C, and tyrosine and tannin, heat preservation 2 is added
~5h;
(6)It after heat preservation, discharges, is spray-dried while hot, collect spray-dried product, washing collects washings, and is put into appearance
In device, it is filled with oxygen, is pressurized to 1.5~1.7MPa, 4~6h is stirred at 70~80 DEG C, stirring thing is collected, mills, collects and grinds
Object is ground to get colour carbon black.
2. a kind of method preparing colour carbon black using waste tire according to claim 1, which is characterized in that the step
(1)Middle auxiliary agent is in mass ratio 4:1~3, sodium carbonate and ferric sulfate are mixed.
3. a kind of method preparing colour carbon black using waste tire according to claim 1, which is characterized in that the addition
Agent is nitrobenzene, boric acid in mass ratio 7:1 mixes.
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Cited By (3)
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US10494573B2 (en) * | 2018-11-06 | 2019-12-03 | Warren Z McCarthy | Method for causing tires to recycle themselves |
WO2021005124A1 (en) | 2019-07-10 | 2021-01-14 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e. V. | Processing and purification of carbonaceous materials |
CN113667328A (en) * | 2021-07-09 | 2021-11-19 | 中国化学工业桂林工程有限公司 | Regenerated carbon black and preparation method and application thereof |
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CN1944543A (en) * | 2006-10-20 | 2007-04-11 | 清华大学 | Method for preparing carbon black filler using waste tire pyrolizing carbon slag |
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Publication number | Priority date | Publication date | Assignee | Title |
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US10494573B2 (en) * | 2018-11-06 | 2019-12-03 | Warren Z McCarthy | Method for causing tires to recycle themselves |
WO2021005124A1 (en) | 2019-07-10 | 2021-01-14 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e. V. | Processing and purification of carbonaceous materials |
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