CN104151877A - Method for modifying ordinary carbon black into pigment carbon black - Google Patents
Method for modifying ordinary carbon black into pigment carbon black Download PDFInfo
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- CN104151877A CN104151877A CN201410388487.5A CN201410388487A CN104151877A CN 104151877 A CN104151877 A CN 104151877A CN 201410388487 A CN201410388487 A CN 201410388487A CN 104151877 A CN104151877 A CN 104151877A
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- carbon black
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Abstract
The invention discloses a method for modifying ordinary carbon black into pigment carbon black. The method comprises the following steps: 1) levigating and drying the ordinary carbon black; 2) preparing a sulfuric acid solution with a concentration of 2 to 18mol/L; 3) adding the dried carbon black into the sulfuric acid solution, and performing water bath reaction for 2 to 10 h under the condition of 50 to 65 DEG C to modify the ordinary carbon black by using a thermostatic water bath kettle; 4) performing suction filtration on the modified carbon black, washing the carbon black to neutral by using distilled water, and drying the carbon black in a constant temperature drying oven to obtain the modified pigment carbon black. According to the method, the ordinary carbon black is used as a raw material to prepare the pigment carbon black, the preparation process is simple, and a requirement on equipment, the preparation temperature, the energy consumption and the production cost are low; low-cost rubber reinforcement carbon black can be used to replace high-cost pigment carbon black for surface acidification modification, and great economic values are brought.
Description
Technical field
The present invention relates to ordinary carbon black modification, specifically refer to that a kind of ordinary carbon black is modified as the method for colour carbon black, belongs to colour black technical field.
Background technology
Carbon black is a kind of important industrial raw materials, is mainly used in rubber industry (account for carbon black loading 90%), particularly tire production (account for carbon black loading 69%).The advantages such as carbon black is painted, weather-proof owing to itself having, reinforcement and conduction, and be widely used as strengthening agent, weighting agent, tinting material and the conducting medium etc. of macromolecular material, particularly carbon black has stronger chemical stability, and therefore, it is also a kind of desirable black pigment simultaneously.Because carbon black pellet is little, it is large that particle has specific surface area, and surface free energy high, so produce extremely strong aggregation force between carbon black particle, easily forms Cluster group, causes dispersiveness poor, limited its application in water-based system.Research shows: ordinary carbon black can reach the basic demand of colour carbon black after treatment, can be used for the industrial tinting pigments such as printing-ink, coating, paint.
Colour carbon black is generally divided into four kinds of high-carbon black pigment, middle colour carbon black, ordinary carbon black pigment and low colour carbon blacks according to colour strength (or blackness) and size of particles.The traditional production method of colour carbon black mainly contains oven process, lamp black method, drum process and channel process.In addition, liquid-phase oxidation contacts fully with carbon black, and oxidation effectiveness is better, can improve carbon black in the dispersiveness of water-soluble system, is the focus that people study always.The deficiency of existing production method is that required equipment is complicated, and production efficiency is low, energy consumption is large, production cost is high.
The paper " Characterization of surface oxidation carbon and their influence on dynamic adsorption " that NV beck etc. is published on Carbon periodical adopts the oxygenated blacks such as nitric acid, ammonia thiosulfate and hydrogen peroxide, and the oxygen level of introducing mostly is 2.1% most.Although it is high that the method is introduced oxygen level, need equipment complicated, reaction conditions and subsequent disposal are complicated, and cost is higher.
Summary of the invention
For prior art above shortcomings, the object of this invention is to provide a kind of method that ordinary carbon black is modified as colour carbon black, present method technique is simple, and equipment requirements is low, and energy consumption is low, and production cost is low.
Technical scheme of the present invention is achieved in that
Ordinary carbon black is modified as a method for colour carbon black, it is characterized in that, step is as follows,
1) after ordinary carbon black is levigate, put into thermostatic drying chamber and carry out drying treatment;
2) measure the vitriol oil and the distilled water of certain volume, being mixed with concentration is 2-18 mol/L sulphuric acid soln;
3) by the 1st) the dried carbon black of step adds the 2nd) in the sulphuric acid soln of step configuration, use thermostat water bath to bathe reaction 2-10h at 50-65 ℃ of Water Under, by ordinary carbon black modification;
4) by the 3rd) the modified carbon black suction filtration that obtains of step and through distilled water wash to neutral, put into thermostatic drying chamber dry, obtain the colour carbon black after modification.
Preferred reaction conditions is that sulphuric acid soln concentration is 10mol/L, water-bath 8h, 60 ℃ of bath temperatures.
Compared to existing technology, the present invention has the following advantages:
The present invention is usingd ordinary carbon black as raw material, carries out acidification reaction with sulfuric acid, prepares colour carbon black, and technique is simple, and equipment requirements is low, and preparation temperature is low, energy consumption is low, and production cost is low.It is acidified modified that the used for rubber reinforcement carbon black that present method available rates is cheap carries out surface, replaces the high colour carbon black of price, has huge economic worth.
Accompanying drawing explanation
The carbon black natural subsidence comparison diagram of Fig. 1-different sulfuric acid concentrations.
Carbon black N330 sreen analysis figure after Fig. 2-former state and modification.
Fig. 3-carbon black modified front and back FT-IR figure.
Fig. 4-carbon black modified front and back XRD figure.
Fig. 5-carbon black modified front and back thermal weight loss design sketch.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
The present invention mainly solves the high problem of existing colour carbon black price, carries out surface acidified modified with cheap used for rubber reinforcement carbon black, replaces the high colour carbon black of price, has huge economic worth.The present invention, by carbon black and certain density sulfuric acid water-bath, prepares the modified carbon black suitable with ordinary carbon black pigment performance.
Ordinary carbon black of the present invention is modified as the method for colour carbon black, and its concrete preparation process is as follows:
1) take certain mass ordinary carbon black (N330), after ball mill is levigate, put into thermostatic drying chamber, at 80 ℃, be dried 12 hours;
2) measure the vitriol oil and the distilled water of certain volume, being mixed with concentration is 2-18 mol/L sulphuric acid soln;
3) by the 1st) dried carbon black adds in enough sulphuric acid solns of configuration in step, uses thermostat water bath to bathe reaction 2-10h at 50-65 ℃ of Water Under, by ordinary carbon black modification;
4) by the 3rd) modified carbon black that obtains of step with circulating water type vacuum pump suction filtration and through distilled water wash to neutral, put into thermostatic drying chamber dry, obtain the colour carbon black after modification.
Change sulfuric acid concentration, reaction times, temperature of reaction can obtain different embodiment.
Embodiment 1: 65 ℃ of sulfuric acid concentration 2mol/L, reaction times 7h, temperature of reaction.
Embodiment 2: 60 ℃ of sulfuric acid concentration 6mol/L, reaction times 6h, temperature of reaction.
Embodiment 3: 65 ℃ of sulfuric acid concentration 10mol/L, reaction times 5h, temperature of reaction.
Embodiment 4: 55 ℃ of sulfuric acid concentration 14mol/L, reaction times 2h, temperature of reaction.
Embodiment 5: 60 ℃ of sulfuric acid concentration 18mol/L, reaction times 4h, temperature of reaction.
Embodiment 6: 60 ℃ of sulfuric acid concentration 10mol/L, reaction times 8h, temperature of reaction.
Embodiment 7: 54 ℃ of sulfuric acid concentration 12mol/L, reaction times 5h, temperature of reaction.
The present invention utilizes natural sedimentation to observe dispersiveness and the laser particle size analyzer of modification front and back carbon black in the aqueous solution and measures its size.Adopt Fourier infrared spectrograph (FT-IR), X-ray diffraction analysis instrument (XRD), Thermal Synthetic Analysis (TGA), scanning electronic microscope energy spectrum analysis (SEM-EDS) to carry out analysis and characterization.
natural sedimentation
Natural subsidence experiment is to detect carbon black one of dispersed conventional means in water, can observe intuitively the dispersion effect of modification front and back carbon black by natural subsidence.N330 carbon black is carried out acidified modified with different concns sulfuric acid, study different sulfuric acid concentrations to dispersed impact.Take different carbon blacks before and after 0.01g modification, put into respectively 6 beakers of number consecutively, add after the ultrasonic concussion of 50ml distilled water half hour standing observation settling velocity.
The carbon black oxidation of the different sulfuric acid concentrations of table 1
| 1# | 2# | 3# | 4# | 5# | 6# |
| Former state | 2mol/L | 6mol/L | 10mol/L | 14mol/L | 18mol/L |
As shown in Fig. 1 (a), every kind of carbon black is all dispersed in water.After second day, 6# starts sedimentation; After the 3rd day, 1# sample starts sedimentation, and 6# becomes clarification; The tenth day, 2#, 3# carbon black sample also started sedimentation, and 1# becomes clarification; After the 16 day, as shown in Fig. 1 (b), 5# style starts sedimentation, and 4# is substantially still muddy shape.Result shows: through concentration, be that the carbon black dispersion of 10mol/L sulfuric acid oxidation is best.
the acid base titration of surface function group of carbon black
According to GB GB/T601-2002 configuration, obtain the hydrochloric acid standard solution that concentration is 0.046698mol/L; The Na that compound concentration is 0.05mol/L respectively
2cO
3(PT), NaOH(GR), NaHCO
3(GR) alkaline solution; Carbon black (after modification, carbon black divides again different sulfuric acid concentrations and time modification) 0.5g before and after modification is added respectively in tri-kinds of alkaline solutions that prepare of 15ml, after ultrasonic dispersion 20min in 100 ℃ of reacting by heating 90min, react complete after suction filtration gained filtrate with hydrochloric acid standard solution, carry out titrimetry.
The acid oxygen-containing functional group of carbon blacksurface mainly contains carboxyl, lactones base, phenolic hydroxyl group etc.The variation of surface function group of carbon black content has larger impact to the dispersiveness of carbon black, therefore, quantitatively judges the Changing Pattern of the oxygen-containing functional group of carbon blacksurface by acid base titration, the dispersed impact of research on carbon black.Calculation formula is as follows:
A=（C
bV
b-C
aV
a）/m
a?；
In formula: C
bfor the volumetric molar concentration (mol/L) of reaction with alkaline solution; V
bvolume (mL) for alkaline solution; C
afor sour volumetric molar concentration (mol/L) for titration; V
afor sour consumption volume (mL) for titration; M
aquality (g) for carbon black sample.A is carboxyl-content; P is carboxyl, lactone group sum; T is total acid content.
(1) different sulfuric acid concentration modified carbon black acidic oxygenous group on surface content is as shown in table 2:
The content (mmol/g) of table 2 different concns carbon blacksurface oxy radical
| Sulfuric acid concentration/(mol/L) | Carboxyl | Lactones base | Phenolic hydroxyl group | Total acid content |
| Former state N330 | 0.1857 | 0.0171 | 0.0200 | 0.2228 |
| 2 | 0.1781 | 0.0212 | 0.0312 | 0.2305 |
| 6 | 0.1828 | 0.0223 | 0.0550 | 0.2601 |
| 10 | 0.1921 | 0.0611 | 0.0153 | 0.2685 |
| 14 | 0.1828 | 0.0237 | 0.0327 | 0.2391 |
| 18 | 0.1613 | 0.0253 | 0.0365 | 0.2251 |
As can be seen from Table 2, when concentration reaches 10mol/L, it is maximum that the total amount of oxygen-containing functional group reaches, and when continuing to increase the concentration of sulfuric acid, oxygen-containing functional group total amount reduces gradually.The Changing Pattern of carboxyl and lactones base and the Changing Pattern of total acid content are roughly the same, and the content of lactone group is far longer than other concentration when sulphuric acid soln concentration is 10mol/L.And the content of phenolic hydroxyl group reaches maximum when sulphuric acid soln concentration is 6mol/L, minimum during 10mol/L, after this increase content of phenolic hydroxyl groups with sulfuric acid concentration has certain increase, and reason may be under this sulfuric acid concentration, and phenolic hydroxyl group has certain coming off.Result shows: the carbon blacksurface after oxide treatment has been introduced the oxygen acid group with good hydrophilic performance, and the introducing of these groups has improved carbon black dispersion stabilization in the aqueous solution.
(2) content of the surperficial oxy radical of differential responses time oxygenated black is as shown in table 3:
The content (mmol/g) of table 3 differential responses time carbon blacksurface oxy radical
| Oxidization time/h | Carboxyl | Lactones base | Phenolic hydroxyl group | Total acid content |
| - | 0.1857 | 0.0171 | 0.0200 | 0.2228 |
| 2 | 0.1925 | 0.0079 | 0.0107 | 0.2111 |
| 4 | 0.2058 | 0.0054 | 0.0093 | 0.2205 |
| 6 | 0.1921 | 0.0611 | 0.0153 | 0.2685 |
| 8 | 0.2005 | 0.0405 | 0.0298 | 0.2708 |
| 10 | 0.2058 | 0.0333 | 0.0253 | 0.2644 |
As can be seen from Table 3, increase along with the reaction times, the surface oxygen functional group total amount of carbon black increases gradually, when the water-bath time, be 6h, the total acid content of carbon blacksurface starts to tend to be steady, reaction 8h, carbon blacksurface oxygen-containing functional group total amount reaches maximum value, while showing that the reaction times is 8h, the oxidizing reaction of carbon blacksurface is sufficient reacting, and the dispersiveness of carbon black in water is best.
laser particle analyzer interpretation of result
In order further to inquire into sulfuric acid concentration to dispersed impact, the particle size distribution figure of former state and the sample (embodiment 6) after concentration is 10mol/L sulfuric acid 8h modification is compared, as shown in Figure 2: wherein, (a) represent the particle size distribution figure of carbon black N330 former state, (b) representative is by the particle size distribution figure of 10mol/L sulfuric acid carbon black after 8h modification.Former state N330 carbon black is compared with carbon black after modification, the size-grade distribution approximate range of former state is at 0.25 μ m-94 μ m, carbon black size-grade distribution approximate range after the modification of 10mol/L sulfuric acid acidation is 0.2 μ m-68 μ m, and the carbon black granularity after modification obviously reduces, and has improved the dispersing property in water.
infrared spectroscopy interpretation of result (FT-IR)
Fig. 3 is carbon black modified front and back FT-IR figure.By the infrared spectrum of carbon black (embodiment 6, the curve of figure middle and lower part) after contrast carbon black former state (curve of figure middle and upper part) and oxidation, can find: its absorption peak mainly concentrates on 3437cm
-1, 2368cm
-1, 1638cm
-1, 1049cm
-1and 670cm
-1near.Wherein, 3437cm
-1strong absorption peak be considered to that the stretching vibration of carbon blacksurface hydroxyl causes; 2368cm
-1absorption peak is due to the stretching vibration peak of O-H in carbon blacksurface; 1638cm
-1absorption peak is due to the stretching vibration peak of C=O in carbon blacksurface carboxyl; 1049cm
-1it near absorption peak, is the vibration peak of carbon blacksurface ester group.And at 3437cm
-1after place's modification, the absorption peak of carbon black is obviously large than carbon black former state peak area, and from an aspect has proved oxidation, carbon blacksurface has been introduced the oxygen acid groups such as hydroxyl, carboxyl.
x-ray diffraction interpretation of result (XRD)
Because sulfuric acid has oxidisability, when oxygenated black, the quality of carbon black has a certain amount of loss, although oxidation can promote the oxy radical content of carbon blacksurface, strong oxidizing property may be destroyed the structure of carbon black inside, thereby affects the character of carbon black.In order to study the destructiveness of oxidation to graphite crystal layer, carbon black has been carried out to X-ray diffraction analysis, as shown in Figure 4 (before oxidation curve upper, after oxidation curve under):
Contrast is oxidized front and back peak position, peak is strong and peak width, and after oxide treatment, carbon black rises a little 25 ° of peak positions, and does not substantially have change at the peak height of 45 ° of peak positions, and peak width is faint to be reduced, and illustrates that oxidation does not damage substantially to the microlitic structure of carbon black inside.
thermogravimetric interpretation of result (TG)
Composition in carbon black system after oxidation modification and performance are not identical, the carbon black before and after oxidation is carried out to heat and analyze, and can, according to the carbon black of the oxidation front and back difference of decomposition temperature at high temperature, relatively be oxidized the impact on carbon black.Fig. 5 be carbon black modified front and back thermogravimetic analysis (TGA) comparison diagram (oxidation before curve upper, oxidation after curve under).
Known by contrasting: total weightlessness of N330 former state is less than the carbon black after oxidation modification.Carbon black after modification (embodiment 6) for the first time larger weightless temperature 50 ℃ of left and right, than N330 former state for the first time larger weightless temperature shifted to an earlier date 10 ℃ of left and right; Obvious wide than before carbon black modified of weightless temperature range simultaneously; Within the scope of diagram, the quality change of former state is-4.62%, and after modification, carbon black mass is changed to-7.20%, and after oxidation, the weightless temperature of carbon black obviously shifts to an earlier date, and rate of weight loss also improves greatly, illustrates that being oxidized rear carbon blacksurface has introduced oxygen-containing functional group really.
sem energy spectrum analysis (SEM-EDS)
The carbon black modified front and back of table 4 are elementary composition
Table 4 is scanning electron microscope gamma-spectrometric data, and correlation data is known: the carbon content after oxidation obviously reduces, and mass percent reduces to 82.07% by 87.83%; And Sauerstoffatom quality percentage composition is increased to 17.88% by 8.61%, after oxidation, carbon blacksurface oxygen-containing functional group obviously increases as can be seen here.
the comparison of carbon black and ordinary carbon black pigment after modification
After embodiment 6 modifications, the contrast of the significant parameter of the ordinary carbon black C611 of carbon black and domestic certain manufacturer production is as shown in table 5.After modification, its tinctorial strength of carbon black is compared slightly almost with C611 with DBP absorption value, but its blackness and ordinary carbon black pigment C611 are very approaching, comprehensively it seems, modified carbon black can be used as ordinary carbon black pigment and uses, and from now on modified carbon black is applied to in water-borne coatings, will have larger meaning.
The significant parameter contrast of table 5 modified carbon black and colour carbon black
| Significant parameter | Carbon black before modification | Carbon black after modification | C611 ordinary carbon black pigment |
| Blackness (reflectivity) | 55 | 47 | 46 |
| Tinctorial strength/(%) | 97 | 99 | 113 |
| DBP absorption value/(ml/g) | 1.03 | 1.10 | 0.72 |
By above-mentioned experiment, can find out, after using sulfuric acid to ordinary carbon black N330 acidification, through FT-IR, XRD, thermogravimetric analysis, the analysis modes such as sem energy spectrum analysis show: acidifying makes to have increased the oxy radicals such as carboxyl, hydroxyl on carbon blacksurface, and these hydrophilic radicals have increased the dispersion stabilization of carbon black in the aqueous solution.
When particle size carbon black is 140 orders, sulfuric acid concentration is 10mol/L, and the reaction times is while being 8h, carbon black dispersion optimal stability, and the particle size carbon black making is less, and the increase of surperficial oxy radical amount is the most obvious, substantially reaches the requirement of ordinary carbon black pigment.
Through the carbon black of sulfuric acid oxidation, its performance and ordinary carbon black pigment are very approaching, can be used as ordinary carbon black pigment and use.
The present invention adopts fairly simple processing unit and technique, successfully ordinary carbon black is modified as to colour carbon black.Compare with existing technique, have that method is simple, temperature of reaction is low, low power consumption and other advantages.Ordinary carbon black N330 is modified as ordinary carbon black pigment, is a kind of new expansion to pigment production of carbon black thinking, is developing new product variety simultaneously, and the development of new products, provides new means.Colour carbon black has wide market outlook, and the market price of ordinary carbon black pigment is 1.6 ten thousand yuan/t left and right, and the market price of N330 carbon black is 0.8 ten thousand yuan/t left and right; Sulfuric acid modified rear carbon black is 1.2 ~ 1.3 ten thousand yuan/t in the price that affects that takes into full account the factors such as sulfuric acid, current consumption, water, and modified carbon black will have great economic worth.
The above embodiment of the present invention is to be only explanation example of the present invention, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make on the basis of the above description other multi-form variation and changes.Here cannot give all embodiments exhaustive.Every still row in protection scope of the present invention of apparent variation that technical scheme of the present invention amplifies out or change that belong to.
Claims (4)
1. ordinary carbon black is modified as a method for colour carbon black, it is characterized in that, step is as follows,
1) after ordinary carbon black is levigate, put into thermostatic drying chamber and carry out drying treatment;
2) measure the vitriol oil and the distilled water of certain volume, being mixed with concentration is 2-18 mol/L sulphuric acid soln;
3) by the 1st) the dried carbon black of step adds the 2nd) in the sulphuric acid soln of step configuration, use thermostat water bath to bathe reaction 2-10h at 50-65 ℃ of Water Under, by ordinary carbon black modification;
4) by the 3rd) the modified carbon black suction filtration that obtains of step and through distilled water wash to neutral, put into thermostatic drying chamber dry, obtain the colour carbon black after modification.
2. ordinary carbon black according to claim 1 is modified as the method for colour carbon black, it is characterized in that: preferred reaction conditions is that sulphuric acid soln concentration is 10mol/L, water-bath 8h, 60 ℃ of bath temperatures.
3. ordinary carbon black according to claim 1 is modified as the method for colour carbon black, it is characterized in that: preferred reaction conditions is that sulphuric acid soln concentration is 65 ℃ of 10mol/L, reaction times 5h, temperature of reaction.
4. ordinary carbon black according to claim 1 is modified as the method for colour carbon black, it is characterized in that: preferred reaction conditions is that sulphuric acid soln concentration is 54 ℃ of 12mol/L, reaction times 5h, temperature of reaction.
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| CN107022112A (en) * | 2017-05-11 | 2017-08-08 | 四川理工学院 | A kind of method of carbon blacksurface graphite alkylene |
| CN107312364A (en) * | 2017-07-04 | 2017-11-03 | 济南大学 | A kind of preparation method of cladded type magnetic black pigment |
| CN107629489A (en) * | 2017-08-14 | 2018-01-26 | 合肥市田源精铸有限公司 | A kind of production method of modified carbon black |
| CN109942215A (en) * | 2019-02-26 | 2019-06-28 | 中昊黑元化工研究设计院有限公司 | A kind of preparation method of cement constructional material special carbon black |
| CN111138694A (en) * | 2019-12-13 | 2020-05-12 | 江苏省农业科学院 | Biochar acrylate material with photo-thermal effect and preparation method thereof |
| CN113337143A (en) * | 2021-05-31 | 2021-09-03 | 安徽德瑞新材料科技有限公司 | Processing technology of special carbon black for high-pigment automobile finish |
| CN113429809A (en) * | 2021-05-31 | 2021-09-24 | 安徽德瑞新材料科技有限公司 | Processing technology of carbon black for ultrablue phase color matching |
| CN114031959A (en) * | 2021-11-29 | 2022-02-11 | 安徽工业大学 | Regulation and control method of carbon black structure, activated carbon black solid and application of activated carbon black solid to catalyst carrier |
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| CN107022112A (en) * | 2017-05-11 | 2017-08-08 | 四川理工学院 | A kind of method of carbon blacksurface graphite alkylene |
| CN107312364A (en) * | 2017-07-04 | 2017-11-03 | 济南大学 | A kind of preparation method of cladded type magnetic black pigment |
| CN107629489A (en) * | 2017-08-14 | 2018-01-26 | 合肥市田源精铸有限公司 | A kind of production method of modified carbon black |
| CN109942215A (en) * | 2019-02-26 | 2019-06-28 | 中昊黑元化工研究设计院有限公司 | A kind of preparation method of cement constructional material special carbon black |
| CN111138694A (en) * | 2019-12-13 | 2020-05-12 | 江苏省农业科学院 | Biochar acrylate material with photo-thermal effect and preparation method thereof |
| CN111138694B (en) * | 2019-12-13 | 2022-10-18 | 江苏省农业科学院 | Biochar acrylate material with photo-thermal effect and preparation method thereof |
| CN113337143A (en) * | 2021-05-31 | 2021-09-03 | 安徽德瑞新材料科技有限公司 | Processing technology of special carbon black for high-pigment automobile finish |
| CN113429809A (en) * | 2021-05-31 | 2021-09-24 | 安徽德瑞新材料科技有限公司 | Processing technology of carbon black for ultrablue phase color matching |
| CN114031959A (en) * | 2021-11-29 | 2022-02-11 | 安徽工业大学 | Regulation and control method of carbon black structure, activated carbon black solid and application of activated carbon black solid to catalyst carrier |
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Application publication date: 20141119 |