CN108342100A - Carbon black method for oxidation - Google Patents

Carbon black method for oxidation Download PDF

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Publication number
CN108342100A
CN108342100A CN201810059141.9A CN201810059141A CN108342100A CN 108342100 A CN108342100 A CN 108342100A CN 201810059141 A CN201810059141 A CN 201810059141A CN 108342100 A CN108342100 A CN 108342100A
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mentioned
carbon black
ozone
oxygen
reactor
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CN201810059141.9A
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CN108342100B (en
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李在锡
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OCI Holdings Co Ltd
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DC Chemical Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44Carbon
    • C09C1/48Carbon black
    • C09C1/56Treatment of carbon black ; Purification
    • C09C1/565Treatment of carbon black ; Purification comprising an oxidative treatment with oxygen, ozone or oxygenated compounds, e.g. when such treatment occurs in a region of the furnace next to the carbon black generating reaction zone

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The present invention provides carbon black method for oxidation, including:In ozone generator, ozone is generated using oxygen, the step of to obtain the mixed gas of oxygen and ozone;To after the reactor supply carbon black equipped with input port and outlet, the step of putting into above-mentioned mixed gas to above-mentioned input port, so that above-mentioned mixed gas is in contact with the carbon black in above-mentioned reactor, oxidation processes are carried out to above-mentioned carbon black;The gas that above-mentioned outlet by trapping device from the reactions above is discharged is come the step of obtaining the trapping object comprising oxygen and carbon black micro mist;The step of above-mentioned trapping object is filtered to remove above-mentioned carbon black micro mist by using filter;And the step of regenerating ozone using the above-mentioned trapping object for removing above-mentioned carbon black micro mist and devoting above-mentioned reactor again.

Description

Carbon black method for oxidation
Technical field
The present invention relates to carbon black method for oxidation.
Background technology
Carbon black is used as hydrophobicity originally, on multiple use, is used with other material mixings, it is therefore necessary to which modification is got married It is aqueous to use.For example, when will be modified to hydrophilic carbon black suitable for purposes such as ink, paint, can be improved in aqueous solution Dispersibility.
Have it is a kind of in order to by it is carbon black modified at hydrophily and surface introduce functional group method.This method includes wet type Oxidizing treatment.In wet oxidation facture, for example, using salpeter solution oxidized black, thus functional group is introduced to surface.
Invention content
The technical problem to be solved in the present invention
The example of the present invention provides the carbon black method for oxidation that can reduce production cost.
Technical solution
In the example of the present invention, carbon black method for oxidation is provided, including:In ozone generator, generated using oxygen smelly Oxygen, the step of to obtain the mixed gas of oxygen and ozone;To after the reactor supply carbon black equipped with input port and outlet, to Above-mentioned input port puts into above-mentioned mixed gas, so that above-mentioned mixed gas is in contact with the carbon black in above-mentioned reactor, to above-mentioned Carbon black carries out the step of oxidation processes;The gas that above-mentioned outlet by trapping device from the reactions above is discharged includes oxygen to obtain The step of with the trapping object of carbon black micro mist;Above-mentioned trapping object is filtered by using filter to remove above-mentioned carbon black micro mist The step of;And it regenerates ozone using the above-mentioned trapping object for removing above-mentioned carbon black micro mist and devotes above-mentioned reactor again The step of.
The trapping object for removing above-mentioned carbon black micro mist can be devoted above-mentioned ozone generator to regenerate ozone again, and The above-mentioned ozone regenerated is devoted into above-mentioned reactor again.
Advantageous effect
The efficiency of carbon black can be improved in above-mentioned carbon black method for oxidation, also, smelly to generate by re-using oxygen Oxygen, therefore usage amount can be reduced, so as to effectively reduce production cost.
, can be by the way that unreacted ozone gas be discharged also, according to above-mentioned carbon black method for oxidation, or keep its discharge rate minimum Change, to obtain the effect of environmental protection.
Description of the drawings
Fig. 1 is the process flow chart for the carbon black method for oxidation for schematically showing an example of the invention.
Specific implementation mode
Hereinafter, the example that the present invention will be described in detail.But this for illustrating, the present invention is not limited thereto, the present invention by Invention above-mentioned is claimed range and is defined.
In the example of the present invention, carbon black method for oxidation is provided, including:In ozone generator, generated using oxygen smelly Oxygen, the step of to obtain the mixed gas of oxygen and ozone;To after the reactor supply carbon black equipped with input port and outlet, to Above-mentioned input, which is made a slip of the tongue, puts into above-mentioned mixed gas, so that above-mentioned mixed gas is in contact with the carbon black in above-mentioned reactor, to upper State the step of carbon black carries out oxidation processes;Gas by the above-mentioned outlet discharge for trapping device from the reactions above included The step of trapping object of oxygen and carbon black micro mist;Above-mentioned trapping object is filtered by using filter micro- to remove above-mentioned carbon black The step of powder;And it regenerates ozone using the above-mentioned trapping object for removing above-mentioned carbon black micro mist and devotes above-mentioned reaction again The step of device.
In above-mentioned carbon black method for oxidation, oxidation processes are carried out by making carbon black be reacted with ozone.
Carbon black is used as hydrophobicity originally, on multiple use, is used with other material mixings, it is therefore necessary to which modification is got married It is aqueous to use.For example, when will be modified to hydrophilic carbon black suitable for purposes such as ink, paint, can be improved in aqueous solution Dispersibility.
In above-mentioned carbon black method for oxidation, in order to assign hydrophily to carbon black, carbon black is set to be reacted with ozone, in carbon black Surface introduce hydroxyl, the functional group containing oxygen atom such as carboxyl, thus by carbon black modified at hydrophily.That is, ozone is used as oxidation Agent carries out oxidation processes to carbon black, is thus modified to hydrophily.
Fig. 1 is the process flow chart for the carbon black method for oxidation for schematically showing an example of the invention.
First, in above-mentioned carbon black method for oxidation, the ozone as oxidant is generated in ozone generator.
In Fig. 1, it if from oxygen supply device to ozone generator for oxygen supply, in ozone generator, is generated using oxygen smelly Oxygen, the ozone generated are fed into reactor with the state of the mixed gas mixed with oxygen.
In above-mentioned ozone generator, for example, using air or oxygen as primary raw material, plasma discharge, such as high pressure can be passed through Arc discharge, to generate ozone.After compressor compresses air, oxygen is only separately separated to utilize oxygen.
As another example, ozone can also be generated by voltolisings such as such as corona discharges.Passing through plasma discharge In the case of generating ozone, for example, pressing from both sides between the electrodes by such as glass or ceramics dielectric and being blown into air or oxygen, if to electricity Pole applies high pressure (6~15kv), then in discharge space, by reacting generation ozone as follows.
O2+e--->O+O+e-
O2+e--->O2*+e-
O+O2+M-->O3(M is carbon black to+M.)
O2*+O2-->O3+O
In above-mentioned ozone generator, if generating ozone, the mixed gas for the state that ozone is mixed with oxygen is obtained.
In above-mentioned mixed gas, oxygen puts into reactor as carrier gas together with ozone.
Before putting into above-mentioned mixed gas to above-mentioned reactor, supply carbon black in advance, at this point, so that carbon black occupy it is above-mentioned The mode of 1/2 volume below of the total volume of reactor inner space supplies carbon black.As described above, so that carbon black occupy it is above-mentioned The mode of 1/2 volume below of reactor total volume supplies carbon black to fill reactor, so as to equably treated carbon black.
When putting into above-mentioned mixed gas, the carbon black because of caused by the flow velocity of gas is flown upward in order to prevent, is adjusted State the input speed of mixed gas.
Also, the concentration of above-mentioned mixed gas can be adjusted according to the bulk density of the carbon black in reactor and throw per hour The volume entered.It specifically, can be with 15g/m3To 200g/m3Concentration put into above-mentioned mixed gas, can be according to the size of reactor To adjust input speed.It, can be with 0.5L/ minutes to 5L/ minutes speed to above-mentioned for example, on the basis of the reactor of 2.5L Reactor puts into above-mentioned mixed gas.It, can be with 5L/ minutes to 50L/ minutes on the basis of the reactor of 70L as another example Speed put into above-mentioned mixed gas to above-mentioned reactor.It can be above-mentioned mixed by being put into the inflow velocity in above-mentioned numberical range Gas is closed to improve the oxidation efficiency of carbon black.
Also, above-mentioned input speed can be made to increase according to the angular speed rotated with reactor size.For example, Above-mentioned input speed can be made to increase with the increase of reactor, so that the angular speed rpm of reactor rotation is equal.
As described in Figure 1, above-mentioned reactor is equipped with input port and outlet, and above-mentioned mixed gas is put into from above-mentioned input port.
If injecting above-mentioned mixed gas into reactor, and it is injected in advance in above-mentioned reactor in a batch manner Carbon black is in contact.
Ozone in above-mentioned gaseous mixture is reacted with the carbon black in above-mentioned reactor and is modified to carbon blacksurface, so that charcoal It is black be modified to hydrophily after, be discharged by hydrogen reduction and by above-mentioned outlet.In other words, in above-mentioned reactor, carbon black with Ozone reaction to which carbon black is aoxidized, thus generates and is modified to hydrophilic carbon black.
The exposure of above-mentioned carbon black and ozone and improve modification efficiency in order to further increase, can make above-mentioned reactor into Row rotation.
Then, the gas of the above-mentioned outlet discharge of device from the reactions above is trapped, and it is gaseous oxidation to be re-used Agent, so as to reduce the usage amount of oxygen.
The gas of the above-mentioned outlet discharge of device is arranged as carrier gas, the from the reactions above above-mentioned outlet of device from the reactions above Go out included in the oxygen of mixed gas reacted with carbon black after the oxygen that is generated by ozone, therefore above-mentioned carrier gas includes mainly oxygen.Also, By it is remaining not with carbon black reaction micro ozone be discharged together with oxygen, from above-mentioned outlet be discharged gas In can include simultaneously ozone and oxygen, also, carbon black micro mist is discharged with together with the gas that above-mentioned outlet is discharged.
Therefore, the trapping object obtained by trapping the gas being discharged from above-mentioned outlet includes oxygen and carbon black micro mist, is gone back It may include ozone.In above-mentioned trapping object, it is gaseous oxidizing agent that the residue for removing carbon black micro mist, which is re-used,.
Above-mentioned trapping object is filtered using filter to remove carbon black micro mist, specifically, carries out dust filtering (dust filtration)。
The trapping object that carbon black micro mist is removed by dust filtering includes mainly oxygen, using in the trapping object for removing above-mentioned carbon black micro mist Oxygen generate ozone, and the ozone regenerated is devoted into above-mentioned reactor again.
During oxygen in the trapping object using the above-mentioned carbon black micro mist of removal generates the method for ozone, for example, being given birth to using ozone It grows up to be a useful person, or as another example, the method irradiated by additional ultraviolet light (UV) can be used.
It in the former case, will be in removal in order to regenerate ozone using the trapping object for removing above-mentioned carbon black micro mist The trapping object for stating carbon black micro mist devotes above-mentioned ozone generator to regenerate ozone again, can be above-mentioned smelly by what is regenerated Oxygen devotes above-mentioned reactor again.
In the latter case, ozone is generated to the trapping object irradiation ultraviolet light (UV) for removing above-mentioned carbon black micro mist, it can The above-mentioned ozone regenerated is devoted into above-mentioned reactor again.Specifically, using the ultraviolet light of 240nm or less wavelength Light.If to high-energy of the oxygen irradiation with 240nm wavelength below, that is, the ultraviolet more than combination energy between oxygen, then oxygen Between double bond be broken off, thus generate free oxygen (free oxygen), the molecule under high energy excited state can pass through reception Oxygen forms O3The unstable ozone gas of form.
In Fig. 1, supplied together to above-mentioned ozone generator remove the trapping object of above-mentioned carbon black micro mist with to above-mentioned ozone The oxygen of generator input.
In Fig. 1, the trapping object of above-mentioned carbon black micro mist is removed along the pipeline conveying indicated by A.The conveying indicated by A Line is connected with the oxygen portable cord put into from oxygen supply device to ozone generator, to remove the trapping object edge of above-mentioned carbon black micro mist The pipeline indicated by A can mix with the oxygen supplied from oxygen supply device.
In the carbon black method for oxidation of another example, in order to remove above-mentioned carbon black micro mist to above-mentioned ozone generator input Trapping object and during being conveyed, ultraviolet light is irradiated to the trapping object for removing above-mentioned carbon black micro mist, to above-mentioned trapping object In oxygen can generate ozone by ultraviolet light.That is, in Fig. 1, it can be above-mentioned to the removal conveyed along the pipeline indicated by A The trapping object irradiation ultraviolet light of carbon black micro mist generates ozone, at this point, continue to convey generated ozone, as described above, with from The oxygen pipeline that oxygen supply device is put into ozone generator is connected, so as to be mixed with the oxygen supplied from oxygen supply device.
In Fig. 1, the trapping object along the transported above-mentioned carbon black micro mist of removal of the pipeline indicated by A can pass through delivery pipe Road is conveyed.Above-mentioned conveyance conduit can be designed to include the first pipe and the second pipe double pipe structure, on above-mentioned second pipe surrounds State the peripheral surface of the first pipe.
Above-mentioned second pipe can be equipped with ultraviolet light source, and above-mentioned ultraviolet light source is for the removal to the inside via the first pipe The trapping object of above-mentioned carbon black micro mist irradiates ultraviolet.Ultraviolet light can be irradiated to the oxygen in the trapping object for removing above-mentioned carbon black micro mist To generate ozone.For example, as above-mentioned ultraviolet light source, using ultraviolet LED (UV LED).Above-mentioned ultraviolet light Light source can irradiate the light of 240nm or less wavelength.
It is available to make the transparent material that ultraviolet light passes through as the material of above-mentioned first pipe.
The efficiency of carbon black can be improved in above-mentioned carbon black method for oxidation, also, smelly to generate by re-using oxygen Oxygen, therefore the usage amount of oxygen can be reduced, so as to effectively reduce production cost.
, can be by the way that unreacted ozone gas be discharged according to above-mentioned carbon black method for oxidation, or its discharge rate is made to minimize, come Obtain environment protecting.
On the other hand, as described above, above-mentioned carbon black method for oxidation is simple, therefore even if without using complicated and expensive machinery Equipment can also obtain efficient effect.
Type by the above-mentioned available carbon black of carbon black method for oxidation is unrestricted, be applicable to as conductive carbon black, A variety of black wood charcoals such as the carbon black as ink or painting color imparting agent.
Hydrophilic carbon black can be obtained by above-mentioned carbon black method for oxidation, therefore can prepare and be applicable to effectively serve as oil The carbon black of ink or painting color imparting agent.
Hereinafter, illustrating specific embodiments of the present invention.But embodiment described below is only used for particular instantiation or explanation The present invention, the present invention is not limited thereto.
Embodiment
Embodiment 1
Prepare the reactor of the 2.5L equipped with input port and outlet.
Ozone generator is connected with the input port of above-mentioned reactor.
It is additionally provided with the unit for the gas that the outlet for trapping device from the reactions above is discharged.
The unit for being used to trap the gas being discharged from above-mentioned outlet is connected with dirt catcher by connection unit, with Make from being given birth to above-mentioned ozone by above-mentioned dirt catcher for trapping the gas that the unit for the gas being discharged from above-mentioned outlet traps It grows up to be a useful person conveying.
The hydrocarbon black powder of 50g is put into above-mentioned reactor.
The ozone generated by injecting oxygen to above-mentioned ozone generator is devoted with the mixed gas that oxygen mixes State the input port of reactor.
By above-mentioned mixed gas with 84g/m3Concentration and 1L/ minutes speed devote above-mentioned reactor.
Trapping object is obtained by trapping the gas being discharged from above-mentioned outlet, above-mentioned trapping object is made to pass through dirt catcher, from After above-mentioned trapping object removal carbon black micro mist, the trapping object for removing carbon black micro mist is devoted into above-mentioned ozone generator again.
The carbon black for obtaining being aoxidized from reactor.
Adjusting reaction time, so that the pH of the carbon black aoxidized by above-mentioned ozone is 3, the reaction time used is 2 hours.
The consumption for obtaining the oxygen used in the above-mentioned carbon black that pH is 3 is 20L.
Comparative example 1
It is same as Example 1, the hydrocarbon black powder of 50g is put into the reactor of 2.5L, by being noted to above-mentioned ozone generator The ozone for entering oxygen to generate devotes the input port of above-mentioned reactor with the mixed gas that oxygen mixes.It is different from embodiment 1 , the gas of the outlet discharge of device from the reactions above is not trapped, and directly the carbon black aoxidized is obtained from reactor.
Adjusting reaction time, so that the pH of the carbon black aoxidized by above-mentioned ozone is 3, the reaction time used is 2 hours.
The consumption for obtaining the oxygen used in the above-mentioned carbon black that pH is 3 is 60L.
In embodiment 1, can confirm as re-using is from the oxygen in the gas that the outlet of reactor is discharged, compared with Example 1 is compared, and the usage amount of oxygen is remarkably decreased.
More than, the preferred embodiment of the present invention is described in detail, but range not office is claimed in the invention of the present invention It is limited to this, those skilled in the art that the basic conception of the present invention defined in range is claimed using invention above-mentioned are made Range is claimed in the invention that the various modifications and modification gone out also belong to the present invention.

Claims (8)

1. a kind of carbon black method for oxidation, which is characterized in that including:
In ozone generator, ozone is generated using oxygen, the step of to obtain the mixed gas of oxygen and ozone;
To after the reactor supply carbon black equipped with input port and outlet, above-mentioned mixed gas is put into above-mentioned input port, is made The step of stating mixed gas to be in contact with the carbon black in above-mentioned reactor, oxidation processes carried out to above-mentioned carbon black;
Gas by trapping the above-mentioned outlet discharge of device from the reactions above obtains including the trapping object of oxygen and carbon black micro mist The step of;
The step of above-mentioned trapping object is filtered to remove above-mentioned carbon black micro mist by using filter;And
The step of ozone being regenerated using the above-mentioned trapping object for removing above-mentioned carbon black micro mist and devoting above-mentioned reactor again.
2. carbon black method for oxidation according to claim 1, which is characterized in that above-mentioned trapping object also includes ozone.
3. carbon black method for oxidation according to claim 1, which is characterized in that the trapping object weight of above-mentioned carbon black micro mist will be removed Above-mentioned ozone generator is newly devoted to regenerate ozone, and the above-mentioned ozone regenerated is devoted into above-mentioned reaction again Device.
4. carbon black method for oxidation according to claim 1, which is characterized in that shone to the trapping object for removing above-mentioned carbon black micro mist Ultraviolet light is penetrated to regenerate ozone, and the above-mentioned ozone regenerated is devoted into above-mentioned reactor again.
5. carbon black method for oxidation according to claim 1, which is characterized in that in above-mentioned ozone generator, by it is equal from Electron discharge simultaneously generates ozone using oxygen.
6. carbon black method for oxidation according to claim 1, which is characterized in that smelly to increase by making above-mentioned reactor rotate The exposure of oxygen and carbon black.
7. carbon black method for oxidation according to claim 1, which is characterized in that with 15g/m3To 200g/m3Concentration to above-mentioned Reactor puts into above-mentioned mixed gas.
8. carbon black method for oxidation according to claim 1, which is characterized in that the oxygen for being included in above-mentioned mixed gas is from sky The oxygen of separation is compressed in gas.
CN201810059141.9A 2017-01-23 2018-01-22 Carbon black oxidation process Active CN108342100B (en)

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KR10-2017-0010337 2017-01-23
KR1020170010337A KR20180087492A (en) 2017-01-23 2017-01-23 Method of oxidation of carbon black

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CN108342100B CN108342100B (en) 2020-03-17

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112679998A (en) * 2021-01-11 2021-04-20 北京化工大学 Preparation facilities of high pigment carbon black
CN112724711A (en) * 2021-01-11 2021-04-30 北京化工大学 Preparation method of high-pigment carbon black
US11653646B2 (en) 2019-04-01 2023-05-23 Vulpes Agricultural Corp. Bifunctional plant promoter and preparation thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100588792B1 (en) * 1998-05-29 2006-06-13 데구사 아게 Oxidatively aftertreated carbon black
CN201842796U (en) * 2010-10-22 2011-05-25 安徽省勇锋化工有限责任公司 Carbon black ozone-oxidizing device
CN102585565A (en) * 2012-03-19 2012-07-18 苏州宝化炭黑有限公司 Method and device for manufacturing carbon black pigment

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100588792B1 (en) * 1998-05-29 2006-06-13 데구사 아게 Oxidatively aftertreated carbon black
CN201842796U (en) * 2010-10-22 2011-05-25 安徽省勇锋化工有限责任公司 Carbon black ozone-oxidizing device
CN102585565A (en) * 2012-03-19 2012-07-18 苏州宝化炭黑有限公司 Method and device for manufacturing carbon black pigment

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11653646B2 (en) 2019-04-01 2023-05-23 Vulpes Agricultural Corp. Bifunctional plant promoter and preparation thereof
CN112679998A (en) * 2021-01-11 2021-04-20 北京化工大学 Preparation facilities of high pigment carbon black
CN112724711A (en) * 2021-01-11 2021-04-30 北京化工大学 Preparation method of high-pigment carbon black

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CN108342100B (en) 2020-03-17

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