CN101104761A - Method for preparing nano carbon black color paste adapted for neutral ink and preparation device thereof - Google Patents
Method for preparing nano carbon black color paste adapted for neutral ink and preparation device thereof Download PDFInfo
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- CN101104761A CN101104761A CN 200710070333 CN200710070333A CN101104761A CN 101104761 A CN101104761 A CN 101104761A CN 200710070333 CN200710070333 CN 200710070333 CN 200710070333 A CN200710070333 A CN 200710070333A CN 101104761 A CN101104761 A CN 101104761A
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Abstract
The invention discloses a preparation method of a nano carbon black color paste with carbon black in high oxidation efficiency, carbon black particles in good self-dispersity and good color stability which is suitable for neutral ink, and a preparation device. The steps of the preparation method are as follow: a. adding pure water, aided dispersant, defoaming agent into a reactor to be mixed with carbon black uniformly; b. inputting ozone into the reactor, the ozone generates micro bubbles with diameter of about 100 micrometer through a super micro bubble diffuser, so that the ozone micro bubbles contact with carbon particles fully to react for 4 to 5 hours; c. degassing the above-mentioned production and adding the aided dispersant to prepare the color paste. The preparation device comprises a reactor, an ozone generator, a super micro bubble ceramic diffuser, a material stirring circulation mechanism, and a tail gas absorption mechanism. The super micro bubble ceramic diffuser is arranged at the bottom of the reactor; the ozone outlet of the ozone generator is communicated with the air inlet of the super micro bubble ceramic diffuser through a pipe.
Description
Technical field
The present invention relates to a kind of nano carbon black color paste preparation method and preparation facilities thereof that is applicable to Neutral writing ink.
Background technology
Carbon black is the fines that produces through incomplete combustion with carbon raw material (being mainly oil).Outward appearance is the particulate or the meal of ater.
Carbon black has following characteristics when being used for gel ink pen with the manufacturing of ink as tinting material:
1. carbon black is best black pigment.
2. carbon black almost is the most cheap pigment.
3. carbon black is tinting strength and the strongest pigment of opacifying power.
4. sooty colourity is neutral on the visual perception.
5. carbon black has the good characteristics of weather resistance, is the most stable pigment, heat-resisting, chemicals-resistant, fast light.
6. the depth of carbon black color, the fineness of particle, the size of proportion, all different and variant with raw materials used and manufacture method.
As a kind of pigment, carbon black is widely used in ink and mill base is made the field.Continuous development along with social scientific and technological level; particularly along with the raising of environmental protection requirement; in mill base, use a lot of solvents in use to be restricted, therefore in ink and mill base manufacturing field, make aqueous color paste and progressively replace the main selection that the solvent-borne type mill base becomes people.Carbon black stably is dispersed in the water, needs to improve the sooty hydrophilicity, therefore carbon black is carried out modification becomes people's research with the needs that adapt to aqueous systems stability a hot subject.
Liquid phase oxidation is the oxidizing methods for surface modification of color that colour carbon black uses the earliest, and available nitric acid, potassium permanganate, sodium chlorate, aqueous sodium hypochlorite solution and bromine aqueous solution etc. carry out the surface oxidation modification to carbon black.With nitric acid is the liquid phase oxidation of representative, though carboxyl functional group is increased, significantly improve the dispersiveness of carbon black in water, but in the suitability for industrialized production of reality, handle because the carbon black after low, the Cheng Mugao of oxidation efficiency, complex technical process, the especially oxidation needs the water secondary to clean, cause serious environmental pollution, thereby this method oneself is eliminated in developed country, China is also progressively eliminating this method.
Catalytic oxidation is to utilize catalyzer carbon black to be carried out the method for catalyzed oxidation.Reported use TiCl abroad
4, VOCl
3, CrOCl
4Deng metal catalyst carbon black is carried out the catalytic gas phase oxidation experiment, the result shows, utilize the catalyst oxidation carbon black can improve carbon blacksurface oxygen-containing functional group content, especially be good with Cr, its optimal reaction temperature is about 250 ℃, when oxidizing temperature was high again, the oxygen-containing functional group of carbon blacksurface will decompose, and generated CO and CO
2, cause oxygen-containing functional group content to descend.Catalyst oxidation sooty research at present also is in laboratory level, and key factor is not work out low price, temperature of reaction low (under the room temperature), oxidation efficiency height, is convenient to high-effect, the low consumed catalyzer of commercial exploitation.
Plasma surface oxidation modification technology is a new technology that grows up the eighties, has obtained at present using comparatively widely in material surface modifying, as improving adhesiveproperties, hydrophilicity and the oleophylic performance etc. of material.And modal to the oxidation modification of carbon powder surface be that carbon black is carried out the low-temperature plasma oxidation, its main process is that polar group is introduced carbon blacksurface, makes its surface polarityization, as with high-frequency corona discharge, makes with O
2It is main Cement Composite Treated by Plasma carbon black.It is acid that carbon black after this handles shows, and dispersed good in water, and the dispersiveness of the carbon black of non-modified in water is not good, easily produces sedimentation.Plasma body commonly used has air, oxygen gas plasma, NO low-temperature plasma etc.Carbon black plasma oxidation method also is in the experimental study stage at present, and its industrialized technical difficult points is how to cut down the consumption of energy, and makes carbon black problem such as even oxidation and realization serialization production in reactor.
Vapour phase oxidation process is the method that world today's colour carbon black surface oxidation modified industry production is generally adopted.Gaseous oxidation is often used oxidizing gas such as air, oxygen, oxynitrides and ozone etc. that carbon black is carried out the surface oxidation modification and is handled.With gases such as air, oxygen is that oxygenant carries out the product that the gaseous oxidation carbon black obtains, its surface oxygen functional group content is relatively low, major cause is that oxidizing reaction generally will carried out more than 400 ℃, and the part oxygen-containing functional group that is under this temperature is own unstable, decomposes to generate CO and CO
2Therefore, be that oxygenant comes the method hexyl wood of oxygenated black to stop using with gases such as air, oxygen.Equally, be oxygenant with the oxynitrides, because defectives such as source of the gas restriction, cost height and environmental pollution also seldom adopt.
Ozone is one of the strongest known oxygenant, is only second to fluorine, can the most organism of oxidation, inorganics.The strong and weak contrast of ozone and other oxidizing substance oxidisability is as follows: fluorine＞hydroxide radical＞ozone＞hydrogen peroxide＞MnO4＞dioxide peroxide＞hypochlorous acid＞chlorine＞oxygen, the ozone stable extreme difference, can be decomposed into oxygen voluntarily at normal temperatures, the transformation period of the following ozone of 1% concentration in air (normal temperature and pressure) is about half hour, rising with temperature, decomposition rate is accelerated, and can transfer oxygen immediately to when temperature reaches 270 ℃ of high temperature.With ozone is oxygenant; gas source is convenient, oxidation efficiency is high, reaction conditions is gentle (under the room temperature), low cost and other advantages because of having; for the world today generally uses, do not have residuals to exist soon owing to it decomposes, so ozonation technology help environment protection.Calendar year 2001, Lu of chemical industry metallurgical institute of Chinese Academy of Sciences cdear, people such as Wang Zhaolin, Li Hongzhong carry out the applied research of ozone in ultra-fine carbon black surface modification, carried out in fluidized-bed, utilizing ozone under different condition, carbon black to be carried out the experiment of surface modification, all be better than non-oxide carbon black in many aspects through the character of the oxygenated black of ozonize.But also there is certain defective in the fluidization of oxidizing carbon black through ozone, and the oxidizing carbon black through ozone fluidization is the gas-solid two phase reaction, and ozone utilization rate is lower, and the sooty oxidation efficiency is low.
Summary of the invention
Technical problem to be solved by this invention provides the nano carbon black color paste preparation method and the preparation facilities thereof that are applicable to Neutral writing ink that a kind of carbon black oxidation efficiency height, carbon black pellet are good from dispersing property, stability of pigment paste can be good.
The invention provides a kind of nano carbon black color paste preparation method who is applicable to Neutral writing ink, comprise the following steps:
A. add pure water, dispersion aids, defoamer and mix in reactor, slowly add carbon black under the high-speed stirring, adjusting system pH with the pH regulator agent is 7～9, and making beating is more than 1 hour;
B. in reactor, feed ozone, ozone generates about 100 microns micro-bubble by the ultramicro air bubble scatterer, progressively rise by reactor bottom, the abundant contact reacts of ozone micro-bubble and carbon black pellet in uphill process, in the reaction process material is stirred fully, reacted 4～5 hours;
C, above-mentioned product is outgased, add dispersion aids, and adjust in pH to 7～9 scopes, stir and make product, finally make required mill base fully from dispersion with the pH regulator agent.
Can also also comprise in the technique scheme and remove the tail gas step, after ozone tail gas rose to the top by reactor bottom, absorbing mechanism absorbed by tail gas.
In the technique scheme, the ozone bubbles that is produced by the ultramicro air bubble ceramic diffusers has minimum diameter and great surface-area, the transfer rate of ozone in whole mixed liquid system is very high, its reactivity worth is strengthened greatly, in sooty ozone oxidation process, not only carbon black coacervate surface is oxidized, and carbon black coacervate inside is also progressively oxidized simultaneously, the result of oxidation makes the depolymerization gradually of carbon black coacervate, forms less from the disperse black carbon particle.
Become the good stable dispersion with nanoscale scope for making from disperse black carbon, what only use preparation is the purpose that does not reach stably dispersing from disperse black carbon, also need add certain dispersion aids, and its effect is to assist to reach stably dispersing from disperse black carbon.Add dispersion aids and also have the effect that reduces surface energy, can make pigment particles is that medium is fully wetting, help from the disperse black carbon depolymerization for the particle diameter range scale be 150 nanometers with interior particle, and reach self-dispersed state.The present invention recommends to use is that fatty alcohol-polyoxyethylene ether or polyacrylic ester are as the dispersion aids from the disperse black carbon mill base.
The use of defoamer is to eliminate the micro-bubble that is produced in the ozone oxidation process, and defoamer can wettingly be penetrated in the micro-bubble thin layer that is produced, and reduces its surface tension, destroys the stability of thin layer, reaches the purpose of froth breaking.The defoamer that the present invention recommends mainly comprises three major types: phosphoric acid ester defoamer, mineral oil defoaming agent and silicone based defoamer.
The pH regulator agent is used for the potential of hydrogen of the hierarchy of control, is beneficial to the stable of system.The present invention recommends the weakly alkaline material to regulate the pH value, as ammoniacal liquor, monoethanolamine, diethanolamine, trolamine, yellow soda ash etc.
The present invention also provides a kind of nano carbon black color paste preparation facilities that is applicable to Neutral writing ink, comprise reactor, ozonizer, ultramicro air bubble ceramic diffusers, material agitation cycle mechanism, tail gas absorbing mechanism, the ultramicro air bubble ceramic diffusers is arranged on the bottom of reactor, the ozone outlet of ozonizer is connected by the inlet mouth of pipeline with the ultramicro air bubble ceramic diffusers, be provided with material agitation cycle mechanism in the reactor, the top of reactor is provided with exhaust port, and exhaust port is connected with tail gas absorbing mechanism by pipeline.
Reactor wherein: be the oxidizing carbon black through ozone reaction zone, reaction zone is a cylindrical region, helps the installation of ozone ultramicro air bubble scatterer and the adding of material;
Ozonizer: by high voltage pulse discharge generation ozone, raw materials used gas is pure oxygen, and the ozone of generation is one of the strongest known oxygenant, and the ozone that produces by ozone generating-device accounts for 5～8% of gas gross, can carry out sufficient oxidation to carbon black;
Ultramicro air bubble ceramic diffusers: can produce diameter and be the bubble about 100 microns, it is long-pending that the generation of microbubble has greatly increased reacted surface, improved the transfer rate of ozone, in less space, has higher efficient, reaction times is short, pottery has better chemical stability simultaneously, be not subjected to the influence of ozone oxidation, so the ultramicro air bubble ceramic diffusers has important effect to oxidizing carbon black through ozone;
Material agitation cycle mechanism: be conventional whipping appts, material is circulated fully, what help reacting effectively carries out;
Tail gas absorbing mechanism: ozone concn reaches 0.01～0.02ppm and can smell in the air; concentration reaches 1ppm has certain influence to HUMAN HEALTH when above; therefore utilize chemical substance that the ozone of discharging is absorbed, absorb the back emptying, be beneficial to HUMAN HEALTH and environment protection.
The invention has the beneficial effects as follows: ozone oxidation reaction carries out in gas-liquid-solid three-phase among the present invention, the utilization ratio of ozone is higher, utilize the ultramicro air bubble method simultaneously, can obviously improve the mass-transfer efficiency of ozone in liquid, thereby improve the sooty oxidation efficiency, prepare can be in aqueous systems self-dispersed oxygenated black product, thereby form nano level from the disperse black carbon particle; Add dispersion aids simultaneously and assist to reach stably dispersing, thereby greatly improved carbon black pellet from dispersing property from disperse black carbon; Add the pH regulator agent in addition, be used for the potential of hydrogen of the hierarchy of control, more help the stable of system, thereby improved the stability of mill base greatly.
Below in conjunction with the drawings and specific embodiments the present invention is described in further detail.
Description of drawings
Fig. 1 is the overall structure synoptic diagram that the present invention is applicable to the nano carbon black color paste preparation facilities of Neutral writing ink.
Embodiment
As shown in Figure 1, the present invention is applicable to a kind of embodiment of the nano carbon black color paste preparation facilities of Neutral writing ink, comprise reactor 2, ozonizer 5, ultramicro air bubble ceramic diffusers 3, material agitation cycle mechanism 1, tail gas absorbing mechanism 6, ultramicro air bubble ceramic diffusers 3 is arranged on the bottom of reactor 2, the ozone outlet of ozonizer 5 is connected by the inlet mouth of pipeline 4 with ultramicro air bubble ceramic diffusers 3, be provided with material agitation cycle mechanism 1 in the reactor 2, the top of reactor 2 is provided with exhaust port 8, and exhaust port 8 is connected with tail gas absorbing mechanism 6 by pipeline 7.
Further specify a kind of nano carbon black color paste preparation method who is applicable to Neutral writing ink of the present invention below by several concrete examples.
Example 1-6 concrete steps:
By following steps carbon black is carried out ozone oxidation, make it reach self-dispersed state.
1. in reactor, add pure water, dispersion aids fatty alcohol-polyoxyethylene ether or modified polyacrylate, the phosphoric acid ester defoamer mixes, and slowly adds carbon black under the high-speed stirring, adjusting system pH with trolamine is 8.5, pulls an oar 1 hour;
2. feed ozone in reactor, ozone generates about 100 microns micro-bubble by the ultramicro air bubble scatterer, is progressively risen the abundant contact reacts of ozone micro-bubble and carbon black pellet in uphill process by reactor bottom;
3, material is stirred material fully by basket whipping appts in reaction process, and what be beneficial to react fully carries out;
4, reaction is 5 hours, measures volatile matter of carbon black every 1 hour, determines reaction end;
5, after the ozone micro-bubble rose to the top by the bottom, system absorbed by exhaust emissions;
6, after the product that above-mentioned steps is obtained outgased 1 hour, add dispersion aids fatty alcohol-polyoxyethylene ether or modified polyacrylate, and adjust in pH to the 7.5-8.5 scope, stirred 1 hour with trolamine, make product fully from disperseing, final required mill base.
Various component concentrations see Table one among the example 1-6, and wherein raw material carbon black Degussa SB-6, DegussaSB-4, Degussa PrintexU are German goldschmidt chemical corporation product.
Table one: the various component concentrations of example 1-6 (gram)
| Component | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 |
| Degussa SB-6 | 300 | 300 | ||||
| Degussa SB-4 | 300 | 300 | ||||
| Degussa PrintexU | 300 | 300 | ||||
| Fatty alcohol-polyoxyethylene ether (adding for the first time) | 17 | 17 | 17 | |||
| Fatty alcohol-polyoxyethylene ether (adding for the second time) | 17 | 17 | 17 | |||
| Modified polyacrylate (adding for the first time) | 20 | 20 | 20 | |||
| Modified polyacrylate (adding for the second time) | 20 | 20 | 20 | |||
| The phosphoric acid ester defoamer | 20 | 20 | 20 | 20 | 20 | 20 |
| |
3 | 3 | 3 | 3 | 3 | 3 |
| Water | 1000 | 1000 | 1000 | 1000 | 1000 | 1000 |
Interpretation of result:
Volatile matter to product in the reaction process is measured, the result as shown in Table 2, when reaction is carried out 4～5 hours, the volatile matter of product is basicly stable, reach reaction end, as can be seen from Table II, reach about 20, illustrate that the carbon black oxidation is very abundant by volatile matter of carbon black in the carbon black color slurry of preparation method's preparation of the present invention.
Table two: the variation of volatile matter of carbon black in the ozone oxidation process
| 0 hour | 1 |
2 |
3 hours | 4 |
5 hours | |
| Example one | 4.6 | 7.8 | 11.9 | 16.1 | 19.2 | 19.6 |
| Example two | 4.6 | 8.1 | 12.6 | 15.0 | 20.2 | 21.1 |
| Example three | 5.1 | 9.3 | 12.3 | 16.8 | 21.8 | 22.0 |
| Example four | 5.1 | 8.8 | 11.2 | 15.6 | 19.0 | 19.6 |
| Example five | 4.2 | 6.6 | 9.5 | 12.0 | 14.8 | 15.4 |
| Example six | 4.2 | 6.8 | 9.8 | 11.9 | 15.2 | 15.8 |
The TURBSCAN dispersion stabilization analyser that adopts French formulaction company carries out stability test to the mill base of preparation, the result as shown in Table 3, from the data of table three as can be seen, adopt method provided by the invention, make from the disperse black carbon tinting material by the ozone oxidation modified carbon black, and make and have nanoscale mill base product, be fit to Neutral writing ink and use, wherein the example three products have more outstanding dispersing property and stability.
Table three: the particle diameter and the stability test of nano modification carbon black color paste product
| Median size (nm) | The beds of precipitation | Clear layer | Stability | |
| Example one | 130 | On a small quantity | Have | 0.12 |
| Example two | 125 | Have | Have | 0.09 |
| Example three | 98 | Do not have | Do not have | 0.07 |
| Example four | 114 | Do not have | Have | 0.13 |
| Example five | 150 | Do not have | Have | 0.14 |
| Example six | 148 | Do not have | Do not have | 0.17 |
Claims (6)
1. a nano carbon black color paste preparation method who is applicable to Neutral writing ink is characterized in that comprising the following steps:
A. add pure water, dispersion aids, defoamer and mix in reactor, slowly add carbon black under the high-speed stirring, adjusting system pH with the pH regulator agent is 7～9, and making beating is more than 1 hour;
B. in reactor, feed ozone, ozone generates about 100 microns micro-bubble by the ultramicro air bubble scatterer, progressively rise by reactor bottom, the abundant contact reacts of ozone micro-bubble and carbon black pellet in uphill process, in the reaction process material is stirred fully, reacted 4～5 hours;
C, above-mentioned product is outgased, add dispersion aids, and adjust in pH to 7～9 scopes, stir and make product, finally get required mill base fully from disperseing with the pH regulator agent.
2. according to the described nano carbon black color paste preparation method who is applicable to Neutral writing ink of claim 1, it is characterized in that: also comprise and remove the tail gas step, after ozone tail gas rose to the top by reactor bottom, absorbing mechanism absorbed by tail gas.
3. according to claim 1 or the 2 described nano carbon black color paste preparation methods that are applicable to Neutral writing ink, it is characterized in that: described dispersion aids is fatty alcohol-polyoxyethylene ether or polyacrylic ester.
4. according to claim 1 or the 2 described nano carbon black color paste preparation methods that are applicable to Neutral writing ink, it is characterized in that: described defoamer is phosphoric acid ester defoamer, mineral oil defoaming agent and silicone based defoamer.
5. according to claim 1 or the 2 described nano carbon black color paste preparation methods that are applicable to Neutral writing ink, it is characterized in that: described pH regulator agent is ammoniacal liquor, monoethanolamine, diethanolamine, trolamine, yellow soda ash.
6. nano carbon black color paste preparation facilities that is applicable to Neutral writing ink, it is characterized in that: comprise reactor (2), ozonizer (5), ultramicro air bubble ceramic diffusers (3), material agitation cycle mechanism (1), tail gas absorbing mechanism (6), ultramicro air bubble ceramic diffusers (3) is arranged on the bottom of reactor (2), the ozone outlet of ozonizer (5) is connected by the inlet mouth of pipeline (4) with ultramicro air bubble ceramic diffusers (3), be provided with material agitation cycle mechanism (1) in the reactor (2), the top of reactor (2) is provided with exhaust port (8), and exhaust port (8) is connected with tail gas absorbing mechanism (6) by pipeline (7).
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101423207B (en) * | 2008-11-17 | 2011-03-16 | 袁翔云 | Synthetic process of lithium hexafluorophosphate |
| CN101531836B (en) * | 2009-04-13 | 2012-10-31 | 杭州中富彩化工新材料有限公司 | Environment-friendly type aqueous color paste for leather and coating as well as manufacturing method thereof |
| CN105026501A (en) * | 2013-03-05 | 2015-11-04 | 卡博特公司 | Aqueous pigment dispersions |
| CN105507077A (en) * | 2015-09-17 | 2016-04-20 | 浙江纳美新材料股份有限公司 | Fruit bag paper special-purpose aqueous black color paste and preparation method thereof |
| CN106660823A (en) * | 2014-08-01 | 2017-05-10 | 国立研究开发法人产业技术综合研究所 | Water including permanganate ions, and method for producing same |
| CN108641412A (en) * | 2018-06-11 | 2018-10-12 | 四川迈克兰诺气泡科技有限公司 | A kind of carbon black modified technique and device |
| CN112480719A (en) * | 2020-11-17 | 2021-03-12 | 唐山黑猫炭黑有限责任公司 | Nano carbon black with metallic luster and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101423207B (en) * | 2008-11-17 | 2011-03-16 | 袁翔云 | Synthetic process of lithium hexafluorophosphate |
| CN101531836B (en) * | 2009-04-13 | 2012-10-31 | 杭州中富彩化工新材料有限公司 | Environment-friendly type aqueous color paste for leather and coating as well as manufacturing method thereof |
| CN105026501A (en) * | 2013-03-05 | 2015-11-04 | 卡博特公司 | Aqueous pigment dispersions |
| CN106660823A (en) * | 2014-08-01 | 2017-05-10 | 国立研究开发法人产业技术综合研究所 | Water including permanganate ions, and method for producing same |
| CN106660823B (en) * | 2014-08-01 | 2019-05-31 | 国立研究开发法人产业技术综合研究所 | Water and its manufacturing method containing high manganese ion |
| CN105507077A (en) * | 2015-09-17 | 2016-04-20 | 浙江纳美新材料股份有限公司 | Fruit bag paper special-purpose aqueous black color paste and preparation method thereof |
| CN108641412A (en) * | 2018-06-11 | 2018-10-12 | 四川迈克兰诺气泡科技有限公司 | A kind of carbon black modified technique and device |
| CN112480719A (en) * | 2020-11-17 | 2021-03-12 | 唐山黑猫炭黑有限责任公司 | Nano carbon black with metallic luster and preparation method thereof |
| CN112480719B (en) * | 2020-11-17 | 2021-12-28 | 唐山黑猫炭黑有限责任公司 | Nano carbon black with metallic luster and preparation method thereof |
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