CN103360799A - Refined carbon black and preparation method thereof - Google Patents
Refined carbon black and preparation method thereof Download PDFInfo
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- CN103360799A CN103360799A CN2013103122538A CN201310312253A CN103360799A CN 103360799 A CN103360799 A CN 103360799A CN 2013103122538 A CN2013103122538 A CN 2013103122538A CN 201310312253 A CN201310312253 A CN 201310312253A CN 103360799 A CN103360799 A CN 103360799A
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- carbon black
- aromatic hydrocarbons
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Abstract
The invention discloses a refined carbon black and a preparation method and a device thereof. The refined carbon black is characterized in that: by mass, the total content of polycyclic aromatic hydrocarbons is 0.005 to 0.3 ppm; wherein the content of benzo (a) pyrene is equal or less than 0.005 ppm, and the content of dibenz(a,h) anthracene is equal or less than 0.005 ppm. The refined carbon black can meet the application needs of the special fields such as medicine, color cosmetics and other fields, and has the advantages of simple equipment structure and convenient operation and great industrial value.
Description
Technical field
The present invention relates to a kind of highly purified carbon black and preparation method thereof.
Background technology
The carbon black black powder shape material that to be hydrocarbons under the processing condition of strict control form through gas phase incomplete combustion or pyrolysis.Its main component is elemental carbon.Carbon black of many uses is divided into two large class, that is: colour carbon black and rubber grade carbon blacks usually according to the purposes difference.Colour carbon black can be divided into again high-carbon black pigment, middle colour carbon black and low colour carbon black three classes.Colour carbon black is according to the different application of having nothing in common with each other of application system.But as pigment, colour carbon black is widely used in mill base, plastic color master grain, printing ink, coating and paint, also is used in a large number the black makeup such as Mascara.
Because carbon black in process of production, the incomplete cracking of hydrocarbons is so that still contain a small amount of hydro carbons, especially multiring aromatic hydrocarbon substance in the product.These materials are wrapped in the surface of carbon black pellet, so that carbon black pellet is assembled easily, have both increased the dispersed difficulty of carbon black as pigment, also owing to the impact of multiring aromatic hydrocarbon substance on HUMAN HEALTH, and have limited the use of carbon black in some industry.
And at present in the carbon black that is circulated in market, the total content of polycyclic aromatic hydrocarbons is more than the 100ppm, and therefore, the carbon black of circulation in the market can not satisfy the needs of some special dimensions, such as " colour cosmetic " field, as: brow powder,, eyebrow pencil etc.
Chinese patent application numbers 200980139332.5 discloses a kind of manufacture method of refining carbon black, thereby the method is made refining carbon black by remove metal from the aqueous carbon black dispersion liquid, and the method comprises that at least a kind of organic acid in making above-mentioned aqueous carbon black dispersion liquid and being selected from glycolic acid, xitix and propanedioic acid contacts, removes the operation of de-iron.This invention can reduce the impurity that contains in the carbon black--the metal ingredients such as iron, but is difficult to remove described organic substance.
Summary of the invention
Refining carbon black of purpose of the present invention and preparation method thereof, the defects that exists to overcome prior art, the needs of using to satisfy association area.
Refining carbon black of the present invention is characterized in that, adopts the method for the general test polycyclic aromatic hydrocarbons of U.S. FDA to detect, and in mass, the total content of polycyclic aromatic hydrocarbons is 0.005～0.3ppm;
Wherein:
Benzo (a) pyrene is≤0.005ppm that dibenzo (a, h) anthracene is≤0.005ppm;
Preferably, the total content of polycyclic aromatic hydrocarbons is 0.2～0.3ppm;
Wherein:
Benzo (a) pyrene is 0.002～0.03ppm, and dibenzo (a, h) anthracene is 0.003～0.04ppm;
Concrete detection method can be referring to SAMPLEPREPARATIONOFSAMPLESFORTHEANALYSISOFPAHsbyISOTOPE-DILUTIONHRGC﹠amp; HRMS, this is the method for the general test polycyclic aromatic hydrocarbons of U.S. FDA.
For the preparation of the reactor of refining carbon black of the present invention, the agitator, jet pipe and the recycle pump that comprise cylindrical shell, consisted of by stir shaft and agitating vane;
Described stir shaft is top-down to be arranged in the described cylindrical shell, and described agitating vane is arranged on the end of stir shaft, and the entrance of described recycle pump is connected with the material outlet of cylindrical shell bottom, and the circulation pump outlet is connected with the material inlet on cylindrical shell top;
Described jet pipe comprises reducing pipe, trunnion and the increaser that is connected in series successively; The other end of reducing pipe is connected with material inlet, and jet pipe is installed in the cylindrical shell vertically downward;
Adopt above-mentioned reactor to prepare the method for described refining carbon black, comprise the steps:
Raw material carbon black and hydrogen peroxide are dropped into described reactor, then start agitator and recycle pump, described recycle pump from the material inlet on cylindrical shell top, enters reactor by jet pipe after from reactor bottom the mixture of raw material carbon black and hydrogen peroxide being extracted out again;
The weight concentration of described hydrogen peroxide is 10～30%;
Weight concentration is that the weight consumption of 10～30% hydrogen peroxide is 3～5 times of raw material carbon black;
The material flow at increaser place is 10～50 meter per seconds, preferred 20～30 meter per seconds;
Reaction times is 1～5 hour;
Then discharge reaction product from outlet, the solid collected by filtration material, washing, 60～90 ℃ of dryings 3～5 hours are pulverized, and can obtain described refining carbon black;
The described reaction times refers to, raw material carbon black and the hydrogen peroxide residence time in reactor;
Adopt the method for the general test polycyclic aromatic hydrocarbons of U.S. FDA to detect, in the described raw material carbon black, in mass, the total content of polycyclic aromatic hydrocarbons is 100～7000ppm, wherein: benzo (a) pyrene is 0.9～60ppm, and dibenzo (a, h) anthracene is 0.1～70ppm;
Preferably, in the raw material carbon black, total polycyclic aromatic hydrocarbons is 101～105ppm;
Wherein:
Benzo (a) pyrene is 0.91～0.95ppm, and dibenzo (a, h) anthracene is 0.13～0.15ppm;
The applicant finds, whether the raw material carbon black can fully mix with hydrogen peroxide, it is an important factor that realizes purpose of the present invention, the method that the present invention has adopted jet pipe to combine with recycle pump, raw material carbon black and hydrogen peroxide are in jet pipe, and in reactor, obtained sufficient mixing, greatly improved reaction efficiency.
Refining carbon black of the present invention can satisfy special dimension, and such as the needs that use in the fields such as medicine, colour cosmetic, device structure is simple, and is easy to operate, has larger industrial value.
Description of drawings
Fig. 1 is the structure of reactor synoptic diagram.
Fig. 2 is the jet pipe structural representation.
Embodiment
Referring to Fig. 1, for the preparation of the reactor of refining carbon black of the present invention, the agitator 2, jet pipe 3 and the recycle pump 4 that comprise cylindrical shell, consisted of by stir shaft and agitating vane;
Described stir shaft is top-down to be arranged in the described cylindrical shell 1, and described agitating vane is arranged on the end of stir shaft, and the entrance of described recycle pump 4 is connected with the material outlet of cylindrical shell bottom, and the outlet of recycle pump 4 is connected with the material inlet on cylindrical shell top;
Described jet pipe 3 comprises reducing pipe 301, trunnion 302 and the increaser 303 that is connected in series successively; The other end of reducing pipe 301 is connected with material inlet, and jet pipe 3 is installed in the cylindrical shell 1 vertically downward;
The diameter D0 of described trunnion 302 is 40～60% of increaser 303 maximum dimension D 2, and the diameter D0 of trunnion 302 is 20～30% of reducing pipe 301 maximum dimension D 1;
Preferably, the quantity of described jet pipe 3 is 4～20, is evenly distributed in the cylindrical shell 1;
Embodiment
Among the embodiment, detection method adopts the method for FDA regulation.
Adopt the equipment of Fig. 1 and Fig. 2 to prepare described refining carbon black.
Device parameter:
The diameter D0 of trunnion 302 is 60% of increaser 303 maximum dimension D 2, and the diameter D0 of trunnion 302 is 30% of reducing pipe 301 maximum dimension D 1;
The quantity of jet pipe 3 is 20, is evenly distributed in the cylindrical shell 1;
The preparation method:
Be that 30% hydrogen peroxide drops into described reactor with raw material carbon black and weight concentration, then start agitator and recycle pump, recycle pump from the material inlet on cylindrical shell top, enters reactor by jet pipe after from reactor bottom the mixture of raw material carbon black and hydrogen peroxide being extracted out again;
Weight concentration is that the weight consumption of 30% hydrogen peroxide is 5 times of raw material carbon black;
The material flow at increaser place is 30 meter per seconds; Reaction times is 1 hour;
Then discharge reaction product from outlet, the solid collected by filtration material, washing, 60 ℃ of dryings 5 hours are pulverized, and can obtain described refining carbon black;
Detected result is as follows:
The raw material carbon black: total polycyclic aromatic hydrocarbons is 101ppm;
Wherein: benzo (a) pyrene=0.91ppm, dibenzo (a, h) anthracene=0.13ppm;
Product:
The total content of polycyclic aromatic hydrocarbons is 0.2ppm;
Wherein: benzo (a) pyrene is 0.002ppm, and dibenzo (a, h) anthracene is 0.003ppm.
Adopt the equipment of Fig. 1 and Fig. 2 to prepare described refining carbon black.
Device parameter:
The diameter D0 of trunnion 302 is 40% of increaser 303 maximum dimension D 2, and the diameter D0 of trunnion 302 is 20% of reducing pipe 301 maximum dimension D 1;
The quantity of jet pipe 3 is 4, is evenly distributed in the cylindrical shell 1;
The preparation method:
Be that 30% hydrogen peroxide drops into described reactor with raw material carbon black and weight concentration, then start agitator and recycle pump, recycle pump from the material inlet on cylindrical shell top, enters reactor by jet pipe after from reactor bottom the mixture of raw material carbon black and hydrogen peroxide being extracted out again;
Weight concentration is that the weight consumption of 30% hydrogen peroxide is 3 times of raw material carbon black;
The material flow at increaser place is 20 meter per seconds; Reaction times is 5 hours;
Then discharge reaction product from outlet, the solid collected by filtration material, washing, 90 ℃ of dryings 3 hours are pulverized, and can obtain described refining carbon black;
Detected result is as follows:
The raw material carbon black: total polycyclic aromatic hydrocarbons is 105ppm;
Wherein: benzo (a) pyrene=0.95ppm, dibenzo (a, h) anthracene=0.15ppm
Product:
The total content of polycyclic aromatic hydrocarbons is 0.3ppm;
Wherein: benzo (a) pyrene is 0.003ppm, and dibenzo (a, h) anthracene is 0.004ppm.
Claims (10)
1. refining carbon black is characterized in that in mass, the total content of polycyclic aromatic hydrocarbons is 0.005～0.3ppm; Wherein: benzo (a) pyrene is≤0.005ppm that dibenzo (a, h) anthracene is≤0.005ppm.
2. refining carbon black is characterized in that in mass, the total content of polycyclic aromatic hydrocarbons is 0.2～0.3ppm; Wherein: benzo (a) pyrene is 0.002～0.03ppm, and dibenzo (a, h) anthracene is 0.003～0.04ppm.
3. refining carbon black according to claim 1 and 2 is characterized in that, is to adopt the method for the general test polycyclic aromatic hydrocarbons of U.S. FDA to detect.
4. prepare the method for each described refining carbon black of claim 1～3, it is characterized in that, comprise the steps:
Raw material carbon black and hydrogen peroxide are dropped into reactor, then start agitator and recycle pump, described recycle pump from the material inlet on cylindrical shell top, enters reactor by jet pipe after from reactor bottom the mixture of raw material carbon black and hydrogen peroxide being extracted out again;
The weight concentration of described hydrogen peroxide is 10～30%;
Weight concentration is that the weight consumption of 10～30% hydrogen peroxide is 3～5 times of raw material carbon black;
The material flow at increaser place is 10～50 meter per seconds, preferred 20～30 meter per seconds;
Reaction times is 1～5 hour;
Then discharge reaction product from outlet, the solid collected by filtration material, washing, drying is pulverized, and can obtain described refining carbon black.
5. method according to claim 4 is characterized in that, described reactor, the agitator (2), jet pipe (3) and the recycle pump (4) that comprise cylindrical shell (1), be made of stir shaft and agitating vane;
Described stir shaft is top-down to be arranged in the described cylindrical shell, and described agitating vane is arranged on the end of stir shaft;
The entrance of described recycle pump (4) is connected with the material outlet (101) of cylindrical shell (1) bottom, and the outlet of recycle pump (4) is connected with the material inlet (102) on cylindrical shell (1) top;
Described jet pipe (3) comprises reducing pipe (301), trunnion (302) and the increaser (303) that is connected in series successively; The other end of reducing pipe (301) is connected with material inlet (102), and jet pipe (3) is installed in the cylindrical shell (1) vertically downward.
6. method according to claim 5 is characterized in that, the diameter D0 of described trunnion (302) is 40～60% of increaser (303) maximum dimension D 2, and the diameter D0 of trunnion (302) is 20～30% of reducing pipe (301) maximum dimension D 1.
7. each described method is characterized in that according to claim 4～6, in the described raw material carbon black, in mass, the total content of polycyclic aromatic hydrocarbons is 100～7000ppm, and wherein: benzo (a) pyrene is 0.9～60ppm, dibenzo (a, h) anthracene is 0.1～70ppm.
8. method according to claim 7 is characterized in that, in the raw material carbon black, total polycyclic aromatic hydrocarbons is 101～105ppm; Wherein: benzo (a) pyrene is 0.91～0.95ppm, and dibenzo (a, h) anthracene is 0.13～0.15ppm.
9. method according to claim 7 is characterized in that, is to adopt the method for the general test polycyclic aromatic hydrocarbons of U.S. FDA to detect.
10. method according to claim 8 is characterized in that, is to adopt the method for the general test polycyclic aromatic hydrocarbons of U.S. FDA to detect.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201310312253.8A CN103360799B (en) | 2013-07-23 | 2013-07-23 | Refined carbon black and preparation method thereof |
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| CN201310312253.8A CN103360799B (en) | 2013-07-23 | 2013-07-23 | Refined carbon black and preparation method thereof |
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| CN103360799B CN103360799B (en) | 2014-08-13 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108774415A (en) * | 2018-07-20 | 2018-11-09 | 宁波德泰化学有限公司 | A kind of manufacturing method of energy conservation and environmental protection carbon black |
| CN111808449A (en) * | 2020-07-22 | 2020-10-23 | 珠海格力绿色再生资源有限公司 | Modification method of tire pyrolysis carbon black, modified pyrolysis carbon black and tire |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4138471A (en) * | 1976-06-01 | 1979-02-06 | J. M. Huber Corporation | Process for reducing the polycyclic aromatic hydrocarbon content of carbon black |
| SU857194A1 (en) * | 1981-08-21 | 1981-08-23 | Предприятие П/Я А-1837 | Method of producing colloidal carbon black preparate |
| EP0622130A1 (en) * | 1993-04-28 | 1994-11-02 | Air Products Gmbh | Method and apparatus for decontaminating soil |
| DE19646552A1 (en) * | 1996-10-29 | 1998-04-30 | Delta Umwelt Technik Gmbh | High activity catalyst for wet oxidation of organic or inorganic contaminants |
| CN1251605A (en) * | 1997-01-29 | 2000-04-26 | 哥伦比亚化学公司 | Hydrogen peroxide oxidation of carbon black |
| CN1262227A (en) * | 1999-02-01 | 2000-08-09 | 山东矿业学院济南分院 | Process and equipment for preparing PFS and ferrite yellow by catalytic oxidization of coal-line troilite ore |
| JP2001354884A (en) * | 2000-06-14 | 2001-12-25 | Mitsubishi Chemicals Corp | Recording solution |
| CN1852804A (en) * | 2003-07-15 | 2006-10-25 | 出光统一科技株式会社 | Film, laminate and package |
| CN101573417A (en) * | 2006-11-07 | 2009-11-04 | 卡伯特公司 | Carbon blacks having low pah amounts and methods of making same |
| CN102060281A (en) * | 2009-09-28 | 2011-05-18 | 赢创德固赛有限公司 | Carbon black, method for its manufacture and application |
| CN102618095A (en) * | 2012-03-07 | 2012-08-01 | 无锡双诚炭黑有限公司 | Production method of environmentally-friendly carbon black |
| CN102702801A (en) * | 2012-05-31 | 2012-10-03 | 中橡集团炭黑工业研究设计院 | High-purity carbon black and production method thereof |
-
2013
- 2013-07-23 CN CN201310312253.8A patent/CN103360799B/en not_active Expired - Fee Related
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4138471A (en) * | 1976-06-01 | 1979-02-06 | J. M. Huber Corporation | Process for reducing the polycyclic aromatic hydrocarbon content of carbon black |
| SU857194A1 (en) * | 1981-08-21 | 1981-08-23 | Предприятие П/Я А-1837 | Method of producing colloidal carbon black preparate |
| EP0622130A1 (en) * | 1993-04-28 | 1994-11-02 | Air Products Gmbh | Method and apparatus for decontaminating soil |
| DE19646552A1 (en) * | 1996-10-29 | 1998-04-30 | Delta Umwelt Technik Gmbh | High activity catalyst for wet oxidation of organic or inorganic contaminants |
| CN1251605A (en) * | 1997-01-29 | 2000-04-26 | 哥伦比亚化学公司 | Hydrogen peroxide oxidation of carbon black |
| CN1262227A (en) * | 1999-02-01 | 2000-08-09 | 山东矿业学院济南分院 | Process and equipment for preparing PFS and ferrite yellow by catalytic oxidization of coal-line troilite ore |
| JP2001354884A (en) * | 2000-06-14 | 2001-12-25 | Mitsubishi Chemicals Corp | Recording solution |
| CN1852804A (en) * | 2003-07-15 | 2006-10-25 | 出光统一科技株式会社 | Film, laminate and package |
| CN101573417A (en) * | 2006-11-07 | 2009-11-04 | 卡伯特公司 | Carbon blacks having low pah amounts and methods of making same |
| CN102060281A (en) * | 2009-09-28 | 2011-05-18 | 赢创德固赛有限公司 | Carbon black, method for its manufacture and application |
| CN102618095A (en) * | 2012-03-07 | 2012-08-01 | 无锡双诚炭黑有限公司 | Production method of environmentally-friendly carbon black |
| CN102702801A (en) * | 2012-05-31 | 2012-10-03 | 中橡集团炭黑工业研究设计院 | High-purity carbon black and production method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 无: "Cabot’s High Purity Furnace Blacks:The Right Choice for Quality,Environmental Responsibility, and Purity!", 《WWW.CABOT-CORP.COM》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108774415A (en) * | 2018-07-20 | 2018-11-09 | 宁波德泰化学有限公司 | A kind of manufacturing method of energy conservation and environmental protection carbon black |
| CN111808449A (en) * | 2020-07-22 | 2020-10-23 | 珠海格力绿色再生资源有限公司 | Modification method of tire pyrolysis carbon black, modified pyrolysis carbon black and tire |
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| CN103360799B (en) | 2014-08-13 |
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