CN114958038A - Preparation method of water-soluble carbon black - Google Patents

Preparation method of water-soluble carbon black Download PDF

Info

Publication number
CN114958038A
CN114958038A CN202210721108.4A CN202210721108A CN114958038A CN 114958038 A CN114958038 A CN 114958038A CN 202210721108 A CN202210721108 A CN 202210721108A CN 114958038 A CN114958038 A CN 114958038A
Authority
CN
China
Prior art keywords
carbon black
water
stirring
reaction
solution
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202210721108.4A
Other languages
Chinese (zh)
Inventor
虞立平
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Anhui Delui New Materials Technology Co ltd
Original Assignee
Anhui Delui New Materials Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Anhui Delui New Materials Technology Co ltd filed Critical Anhui Delui New Materials Technology Co ltd
Priority to CN202210721108.4A priority Critical patent/CN114958038A/en
Publication of CN114958038A publication Critical patent/CN114958038A/en
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44—Carbon
    • C09C1/48—Carbon black
    • C09C1/56—Treatment of carbon black ; Purification
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/12—Treatment with organosilicon compounds

Abstract

The invention discloses a preparation method of water-soluble carbon black, which comprises the following steps: s1, soaking the carbon black in 1-5 wt% nitric acid solution, and stirring at 80-90 ℃ for reaction to obtain oxidized carbon black; s2, adding the oxidized carbon black into 0.5-5 wt% of strong base solution, and stirring for reaction at 45-55 ℃ to obtain neutralized carbon black; s3, adding the tannic acid and the N-2-aminoethyl) -3-aminopropyltriethoxysilane into a Tris-HCl buffer solution, and uniformly mixing to obtain a mixed solution; and S4, soaking the neutralized carbon black in the mixed solution obtained in the step S3, and stirring at room temperature to form a hydrophilic layer on the surface of the carbon black to obtain the water-soluble carbon black. According to the invention, the carbon black is synergistically modified by nitric acid oxidation and coprecipitation surface modification of tannic acid and N-2-aminoethyl) -3-aminopropyltriethoxysilane, so that the carbon black has excellent water solubility and can be stably dispersed in water. The preparation method disclosed by the invention has the characteristics of simplicity, high efficiency, environmental friendliness and the like, and is suitable for popularization.

Description

Preparation method of water-soluble carbon black
Technical Field
The invention belongs to the field of carbon black material preparation, and particularly relates to a preparation method of water-soluble carbon black.
Background
Carbon black has been widely used in the fields of rubber, pigment, paint, ink, printing and dyeing because of its excellent weather resistance, chemical stability, coloring property, and conductivity. Since carbon black contains carbon as a main component and has a small number of surface oxygen-containing functional groups (-OH, -COOH, etc.), it is difficult to stably disperse in water at high concentration and only dissolves in organic solvents such as benzene, xylene, etc., and the use of these solvents not only pollutes the environment but also harms human health. In recent years, with the idea of green environmental protection, water instead of an organic solvent has been attracting more and more attention as a dispersion medium. Therefore, the development of an environment-friendly water-soluble carbon black product using water as a solvent is the key point of the current development of carbon black products.
At present, methods for improving the water solubility of carbon black mainly comprise: the method is simple in operation and easy in condition control, but the dispersion system can generate a phenomenon of inverse coarseness along with the increase of time; the oxidation modification method adopts suitable oxidizing substances (gas phase oxidant: air, oxygen, ozone and nitrogen oxide compound, liquid phase oxidant: HNO 3 And H 2 O 2 ) The carbon black is subjected to chemical reaction with the carbon black, and oxygen-containing functional groups (-OH, -COOH and the like) on the surface of the carbon black are added to improve the water solubility of the carbon black, but the oxidation degree of the carbon black obtained by the method is low, and the carbon black cannot be stably dispersed in water; the graft modification method is to graft a polymer on the surface of carbon black through a chemical bond, and a certain steric hindrance repulsion is provided due to the long chain of the polymer, but the method relates to complex polymerization reaction, has strict requirements, and has small improvement on the grafting rate. The coating modification method is a method of coating a polymer with a hydrophilic group on the surface of carbon black by a phase separation method, a surface polymerization method or the like, so that the affinity of the carbon black and water molecules is increased, and the dispersion stability of carbon black particles in water is improved.
In recent years, a surface modification method for realizing water-soluble (hydrophilic) modification of a hydrophobic material by utilizing the remarkable adhesion efficiency of natural polyphenol to various substrates has been attracting much attention, but no report has been made on water-soluble modification of carbon black by this method.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a preparation method of water-soluble carbon black modified by a liquid-phase oxidation method and surface modification, so as to solve the problems that the water-soluble carbon black prepared by the existing method is easy to agglomerate, poor in dispersibility, easy to precipitate and the like in the use process.
In order to achieve the purpose, the invention adopts the following technical scheme.
A preparation method of water-soluble carbon black comprises the following steps:
s1, soaking the carbon black in 1-5 wt% nitric acid solution, and stirring at 80-90 ℃ for reaction to obtain oxidized carbon black;
s2, adding the obtained oxidized carbon black into 0.5-5 wt% of strong base solution, and stirring for reaction at 45-55 ℃ to obtain neutralized carbon black;
s3, adding the tannic acid and the N-2-aminoethyl) -3-aminopropyltriethoxysilane into a Tris-HCl buffer solution, and uniformly mixing to obtain a mixed solution;
and S4, soaking the neutralized carbon black in the mixed solution obtained in the step S3, and stirring at room temperature to form a hydrophilic layer on the surface of the carbon black so as to obtain the water-soluble carbon black.
Preferably, in the step S1, the stirring speed is 30-40 rpm, the stirring reaction time is 1-10 hours, solid-liquid separation is performed after the reaction is finished, deionized water is washed until no oxidant exists, and then drying is performed at 150-180 ℃ for 9-12 hours.
Preferably, in step S2, the stirring speed is 30-40 rpm, the stirring reaction time is 0.5-2 hours, after the reaction is finished, solid-liquid separation is performed, deionized water is used for washing, and then drying is performed at 150-180 ℃ for 9-12 hours.
Preferably, in step S3, the concentration of tannic acid in the mixed solution is 0.5 to 2 g/L; the mass ratio of the tannic acid to the N-2-aminoethyl) -3-aminopropyltriethoxysilane is 1-3: 1, the concentration of the neutralized carbon black is 0.8-2.0 g/L.
Preferably, in the step S4, the stirring speed is 100 to 160rpm, and the stirring time is 3 to 15 hours.
Preferably, the carbon black is furnace carbon black, the average particle size is 55-80 nm, the pH is 7-9, and the DBP absorption is 85-100 cm 3 100g, and the nitrogen adsorption specific surface area is 90-150 m 2 /g。
The invention also aims to provide the water-soluble carbon black prepared by the preparation method.
Preferably, the particle size of the water-soluble carbon black is in the range of 5 to 50 μm.
Preferably, in step S1, the mass ratio of nitric acid to carbon black is (1 to 3): 1, the solid-liquid separation is centrifugal separation or filtration separation, and more preferably filtration separation;
preferably, the concentration of the carbon black dispersion liquid is 30-200 g/L; preferably 50 to 100 g/L.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention combines the liquid phase oxidation method and the surface modification method to modify the carbon black, and the prepared modified carbon black can be stably dispersed in water and can be stored for at least 180 days without sedimentation. Specifically, the method comprises the steps of firstly, enabling the edges of graphite microcrystals on the surface layer of carbon black and the defects between conglomerates to react under the action of strong oxidizing acid (1-5 wt% of dilute nitric acid) to generate oxygen-containing functional groups (-COOH, -OH and the like), increasing the oxygen-containing functional groups on the surface layer of the oxidized carbon black, improving wettability and well dispersing the carbon black in water; and then the tannin and the N- (2-aminoethyl) -3-aminopropyltriethoxysilane (which is a bisaminosilane coupling agent) are combined to be coprecipitated on the surface of the carbon black to form a hydrophilic coating containing abundant hydroxyl and amino, so that the solubility of the carbon black in water is further enhanced. The Zeta potential value of the water-soluble carbon black solution prepared by the invention is obtained by a Zeta potential test and is as high as-52.8 mV, which shows that the carbon black which is subjected to nitric acid oxidation and surface modification synergistic modification by tannic acid and N-2-aminoethyl) -3-aminopropyltriethoxysilane coprecipitation can be stably dispersed in water.
(2) The preparation method disclosed by the invention has the characteristics of simplicity, high efficiency, environmental friendliness and the like, is suitable for popularization, and provides a new idea for the surface functional modification of the carbon black.
Detailed Description
In the following description, for purposes of explanation and not limitation, specific details are set forth, such as particular system structures, techniques, etc. in order to provide a thorough understanding of the embodiments of the invention. It will be apparent, however, to one skilled in the art that the present invention may be practiced in other embodiments that depart from these specific details.
Example 1
A preparation method of water-soluble carbon black comprises the following steps:
s1, 50g of commercial furnace black (average particle diameter of 55-65 nm, pH 8, DBP absorption 100 cm) 3 100g, nitrogen adsorption specific surface area of 120m 2 /g) soaking in 3L of 5 wt% nitric acid solution, stirring at a stirring speed of 30rpm to fully disperse carbon black in the nitric acid solution, then stirring at 85 ℃ for reaction for 4 hours, filtering after the reaction is finished, washing with deionized water, performing suction filtration until no oxidant exists in the filtrate, and drying at 150 ℃ for 10 hours to obtain oxidized carbon black;
s2, adding the obtained oxidized carbon black into 25mL of 2 wt% sodium hydroxide solution, stirring at a stirring speed of 40rpm to fully disperse the oxidized carbon black, then stirring at 50 ℃ for reaction for 1h, filtering after the reaction is finished, washing with deionized water until the pH value of the filtrate is kept unchanged, and drying at 160 ℃ for 10h to obtain neutralized carbon black;
s3, dissolving 60mg of tannic acid and 50mg of N-2-aminoethyl) -3-aminopropyltriethoxysilane in 50 ml of Tris-HCl buffer solution (pH is 8.3), then soaking the neutralized carbon black in the mixed system, stirring at the stirring speed of 120rpm for 10 hours at normal temperature to ensure that the tannic acid and the N-2-aminoethyl) -3-aminopropyltriethoxysilane are coprecipitated on the surface of the carbon black to form a hydrophilic layer, taking out, repeatedly washing with distilled water until the washing solution is colorless, and drying to obtain the modified carbon black H-CB 1.
Example 2
A preparation method of water-soluble carbon black comprises the following steps:
s1, 80g of commercial furnace black (average particle diameter of 55-65 nm, pH 8, DBP absorption of 100 cm) 3 100g, nitrogen adsorption specific surface area of 120m 2 /g) soaking the carbon black in 5L of 3 wt% nitric acid solution, stirring at the stirring speed of 35rpm to fully disperse the carbon black in the nitric acid solution, then stirring and reacting for 8 hours at 90 ℃, filtering after the reaction is finished, washing with deionized water, performing suction filtration until no oxidant exists in the filtrate, and drying for 12 hours at 150 ℃ to obtain oxidized carbon black;
s2, adding the obtained oxidized carbon black into 35mL of 5 wt% sodium hydroxide solution, stirring at a stirring speed of 40rpm to fully disperse the oxidized carbon black, then stirring at 55 ℃ for reaction for 1h, after the reaction is finished, filtering, washing with deionized water until the pH value of the filtrate is kept unchanged, and drying at 180 ℃ for 9h to obtain neutralized carbon black;
s3, dissolving 75mg of tannic acid and 25mg of N-2-aminoethyl) -3-aminopropyltriethoxysilane in 50 ml of Tris-HCl buffer solution (pH is 8.3), then soaking the neutralized carbon black in the mixed system, stirring at the stirring speed of 120rpm for 8 hours at normal temperature to ensure that the tannic acid and the N-2-aminoethyl) -3-aminopropyltriethoxysilane are coprecipitated on the surface of the carbon black to form a hydrophilic layer, taking out, repeatedly washing with distilled water until the washing solution is colorless, and drying to obtain the modified carbon black H-CB 2.
Example 3
A preparation method of water-soluble carbon black comprises the following steps:
s1, 100g of commercially available furnace carbon black (average particle diameter of 55 to 65nm, pH 8, DBP absorption of 100 cm) 3 100g, nitrogen adsorption specific surface area of 120m 2 /g) soaking the carbon black in 5L of 5 wt% nitric acid solution, stirring at a stirring speed of 30rpm to fully disperse the carbon black in the nitric acid solution, then stirring and reacting for 1h at 80 ℃, filtering after the reaction is finished, washing with deionized water, performing suction filtration until no oxidant exists in the filtrate, and drying for 10h at 165 ℃ to obtain oxidized carbon black;
s2, adding the obtained oxidized carbon black into 25mL of 5 wt% sodium hydroxide solution, stirring at a stirring speed of 35rpm to fully disperse the oxidized carbon black, then stirring at 45 ℃ for reaction for 2 hours, after the reaction is finished, filtering, washing with deionized water until the pH value of the filtrate is kept unchanged, and drying at 180 ℃ for 9 hours to obtain neutralized carbon black;
s3, dissolving 50mg of tannic acid and 50mg of N-2-aminoethyl) -3-aminopropyltriethoxysilane in 100 ml of Tris-HCl buffer solution (pH is 8.3), then soaking the neutralized carbon black in the mixed system, stirring at the stirring speed of 160rpm for 15 hours at normal temperature to ensure that the tannic acid and the N-2-aminoethyl) -3-aminopropyltriethoxysilane are coprecipitated on the surface of the carbon black to form a hydrophilic layer, taking out, repeatedly washing with distilled water until the washing solution is colorless, and drying to obtain the modified carbon black H-CB 3.
Example 4
A preparation method of water-soluble carbon black comprises the following steps:
s1, 50g of commercial furnace black (average particle diameter of 55-65 nm, pH 8, DBP absorption 100 cm) 3 100g, nitrogen adsorption specific surface area of 120m 2 /g) soaking the carbon black in 5L of 1 wt% nitric acid solution, stirring at a stirring speed of 30rpm to fully disperse the carbon black in the nitric acid solution, then stirring and reacting for 10 hours at 85 ℃, filtering after the reaction is finished, washing with deionized water, performing suction filtration until no oxidant exists in filtrate, and drying for 10 hours at 160 ℃ to obtain oxidized carbon black;
s2, adding the obtained oxidized carbon black into 25mL of 5 wt% sodium hydroxide solution, stirring at a stirring speed of 35rpm to fully disperse the oxidized carbon black, then stirring at 50 ℃ to react for 0.5h, after the reaction is finished, filtering, washing with deionized water until the pH value of the filtrate is kept unchanged, and drying at 150 ℃ for 12h to obtain neutralized carbon black;
s3, dissolving 100mg of tannic acid and 50mg of N-2-aminoethyl) -3-aminopropyltriethoxysilane in 50 ml of Tris-HCl buffer solution (pH is 8.3), then soaking the neutralized carbon black in the mixed system, stirring at the stirring speed of 160rpm for 3 hours at normal temperature to ensure that the tannic acid and the N-2-aminoethyl) -3-aminopropyltriethoxysilane are coprecipitated on the surface of the carbon black to form a hydrophilic layer, taking out, repeatedly washing with distilled water until the washing solution is colorless, and drying to obtain the modified carbon black H-CB 4.
Comparative example 1
Only the oxidized carbon black O-CB prepared in example 1 was used.
Comparative example 2
The commercially available carbon black was subjected to surface modification treatment using only tannic acid and N-2-aminoethyl) -3-aminopropyltriethoxysilane in example 1 to obtain surface-modified carbon black S-CB.
And (3) performance characterization:
(1) dispersion stability test in aqueous solution
The settling time in different carbon black slurries can reflect the dispersion stability of the carbon black particles under the same conditions.
Specifically, each of the modified carbon blacks prepared in examples 1 to 4 and comparative examples 1 to 2 and the unmodified commercially available carbon black was prepared as a 0.06% carbon black slurry using deionized water as a dispersion liquid, and then the carbon black slurry was placed in the same environment, and the sedimentation of the carbon black was recorded at intervals of time to evaluate the dispersion stability of the carbon black slurry, and the obtained carbon black slurry was subjected to a drying treatment, and the water solubility of the unmodified and modified carbon blacks was evaluated by the drying time, and the results are shown in table 1.
TABLE 1 static sedimentation evaluation of Dispersion stability of carbon Black slurries at various times
Figure BDA0003709635960000081
As is clear from the results of Table 1 above, the unmodified carbon black was completely precipitated on the bottom of the bottle on day 3 of the test, and the dilute nitric acid oxidation-modified carbon black and the surface modification-modified carbon black were completely precipitated on the bottom of the bottle on days 35 and 60, respectively, whereas the nitric acid liquid phase oxidation and surface modification synergistically modified carbon blacks prepared in examples 1 to 4 of the present invention stably maintained a uniform dispersion in water on day 180. The above results further show that the coating formed by co-precipitating tannic acid rich in amino and hydroxyl groups and N-2-aminoethyl) -3-aminopropyltriethoxysilane successfully covers the surface of carbon black, and as N- (2-aminoethyl) -3-aminopropyltriethoxysilane is dispersed in water and ethoxy is hydrolyzed to form 3 hydroxyl groups, the hydroxyl groups are easily dissolved in water, the amino groups are strongly polar groups, the two amino groups have higher polarity and the solution surface tension is lower, so that the hydroxyl groups can be more easily spread on the surface of carbon black, and the solubility of the oxidized carbon black in water is further enhanced by interfacial co-deposition with tannic acid with more catechol groups on the surface of the carbon black material; the results of drying times further demonstrate the success of examples 1-4 in synergistically modifying carbon blacks.
(2) Zeta potential test
The Zeta potential, which is approximately indicative of the potential of the electrostatic charge carried by a material on its surface in a liquid (often in an aqueous solution), can be used as an indicator of the stability of the system. In general, the higher the Zeta potential, the better the system stability.
Specifically, the modified carbon blacks prepared in examples 1-4 and comparative examples 1-2 and the unmodified commercially available carbon black were dispersed in water to form an aqueous dispersion of the carbon black, which was subjected to the Zeta potential test, the Zeta potential test results of which are shown in Table 2 below.
TABLE 2 Zeta potential test results
CB O-CB S-CB H-CB1 H-CB2 H-CB3 H-CB4
Zeta potential(mV) 22.8 -12.6 -30.9 -52.8 -52.5 51.5 51.9
From the results of Table 2, it is understood that the value of the Zeta potential when the unmodified commercially available carbon black was dispersed in water was 22.8mV, which indicates that the dispersibility of the unmodified commercially available carbon black in water was extremely poor, and that the value of the potential of the modified carbon black solution changed from a positive value to a negative value, which indicates that the dispersion stability of the carbon black in water was greatly improved. The potential values of the carbon black solution subjected to (dilute) nitric acid oxidation modification and surface modification by tannic acid and N-2-aminoethyl) -3-aminopropyltriethoxysilane coprecipitation are-12.6 mV and-30.9 mV respectively, which shows that the carbon black modified by the single method tends to be stable in water. This is because the carbon surface oxidized by nitric acid under certain conditions has increased oxygen-containing functional groups (-COOH, -OH) so that its dispersibility in water is greatly improved; a layer of coating is formed on the surface of the oxidized carbon black through coprecipitation of tannic acid and N-2-aminoethyl) -3-aminopropyltriethoxysilane, after N- (2-aminoethyl) -3-aminopropyltriethoxysilane is dispersed in water, ethoxy is hydrolyzed to form 3 hydroxyl groups which are easily dissolved in water, the amino groups are strong polar groups, the two amino groups have higher polarity and lower solution surface tension, so that the amino groups can be more easily spread on the surface of the carbon black, and the tannic acid with more catechol groups and the tannic acid generate interfacial codeposition on the surface of the carbon black to form a water-soluble layer, so that the dispersibility of the carbon black in water is enhanced; after nitric acid oxidation and co-modification of tannin and N-2-aminoethyl) -3-aminopropyltriethoxysilane coprecipitation surface modification, the Zeta potential value is as high as-52.8 mV, which is obviously increased compared with the potential value modified by a single method, which shows that the carbon black is very stably dispersed in water, and the two modification methods play a role in synergistic modification and produce unexpected technical effects.
The present invention is not limited to the above-described embodiments, and those skilled in the art will be able to make various modifications without creative efforts from the above-described conception, and fall within the scope of the present invention.

Claims (8)

1. A preparation method of water-soluble carbon black is characterized by comprising the following steps:
s1, soaking the carbon black in 1-5 wt% nitric acid solution, and stirring at 80-90 ℃ for reaction to obtain oxidized carbon black;
s2, adding the obtained oxidized carbon black into 0.5-5 wt% of strong base solution, and stirring for reaction at 45-55 ℃ to obtain neutralized carbon black;
s3, adding tannic acid and N-2-aminoethyl) -3-aminopropyltriethoxysilane to a Tris-HCl buffer solution with the pH of 8.2-8.8 to obtain a mixed solution;
and S4, soaking the neutralized carbon black in the mixed solution obtained in the step S3, and stirring at room temperature to form a hydrophilic layer on the surface of the carbon black to obtain the water-soluble carbon black.
2. The preparation method according to claim 1, wherein in step S1, the stirring speed is 30-40 rpm, the stirring reaction time is 1-10 hours, solid-liquid separation is performed after the reaction is finished, deionized water is used for washing until no oxidant exists, and then drying is performed at 150-180 ℃ for 9-12 hours.
3. The preparation method according to claim 1, wherein in step S2, the stirring speed is 30-40 rpm, the stirring reaction time is 0.5-2 h, after the reaction is finished, solid-liquid separation is performed, deionized water is used for washing, and then drying is performed at 150-180 ℃ for 9-12 h.
4. The method according to claim 1, wherein in step S3, the concentration of tannic acid in the mixed solution is 0.5 to 2 g/L; the mass ratio of the tannic acid to the N-2-aminoethyl) -3-aminopropyltriethoxysilane is 1-3: 1, the concentration of the neutralized carbon black is 0.8-2.0 g/L.
5. The method according to claim 1, wherein in the step S4, the stirring speed is 100-160 rpm, and the stirring time is 3-15 hours.
6. The method according to claim 1, wherein the carbon black is a furnace carbon black having an average particle diameter of 55 to 80nm, a pH of 7 to 9, and a DBP absorption of 85 to 100cm 3 100g, and the nitrogen adsorption specific surface area is 90-150 m 2 /g。
7. A water-soluble carbon black obtained by the production method as described in any one of claims 1 to 6.
8. The water-soluble carbon black according to claim 7, wherein the particle diameter of the water-soluble carbon black is in the range of 5 to 50 μm.
CN202210721108.4A 2022-06-23 2022-06-23 Preparation method of water-soluble carbon black Pending CN114958038A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210721108.4A CN114958038A (en) 2022-06-23 2022-06-23 Preparation method of water-soluble carbon black

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210721108.4A CN114958038A (en) 2022-06-23 2022-06-23 Preparation method of water-soluble carbon black

Publications (1)

Publication Number Publication Date
CN114958038A true CN114958038A (en) 2022-08-30

Family

ID=82966286

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210721108.4A Pending CN114958038A (en) 2022-06-23 2022-06-23 Preparation method of water-soluble carbon black

Country Status (1)

Country Link
CN (1) CN114958038A (en)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB862018A (en) * 1957-01-16 1961-03-01 Etude Des Ind Du Petrole Au Po Water-dispersible carbon black and production thereof
JP2008195837A (en) * 2007-02-14 2008-08-28 Daito Kasei Kogyo Kk Surface treated carbon black and its manufacturing method, water dispersion formed by dispersing same, and cosmetic, ink and coating containing the dispersion
CN106634059A (en) * 2016-12-16 2017-05-10 江南大学 Preparation method of aqueous self-dispersing nanometer carbon black
CN111117301A (en) * 2020-01-08 2020-05-08 郑州久源化工有限公司 Preparation method and application of modified carbon black
CN113307523A (en) * 2021-06-01 2021-08-27 安徽德瑞新材料科技有限公司 Method for preparing water-soluble carbon black, water-soluble carbon black and application thereof
CN114016288A (en) * 2021-12-07 2022-02-08 中国第一汽车股份有限公司 Fiber cord dipping solution and preparation method and application thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB862018A (en) * 1957-01-16 1961-03-01 Etude Des Ind Du Petrole Au Po Water-dispersible carbon black and production thereof
JP2008195837A (en) * 2007-02-14 2008-08-28 Daito Kasei Kogyo Kk Surface treated carbon black and its manufacturing method, water dispersion formed by dispersing same, and cosmetic, ink and coating containing the dispersion
CN106634059A (en) * 2016-12-16 2017-05-10 江南大学 Preparation method of aqueous self-dispersing nanometer carbon black
CN111117301A (en) * 2020-01-08 2020-05-08 郑州久源化工有限公司 Preparation method and application of modified carbon black
CN113307523A (en) * 2021-06-01 2021-08-27 安徽德瑞新材料科技有限公司 Method for preparing water-soluble carbon black, water-soluble carbon black and application thereof
CN114016288A (en) * 2021-12-07 2022-02-08 中国第一汽车股份有限公司 Fiber cord dipping solution and preparation method and application thereof

Similar Documents

Publication Publication Date Title
CN111171607B (en) Method for preparing hydrophilic carbon black, hydrophilic carbon black and application thereof
CN107383405B (en) Composite proton exchange membrane and preparation method thereof
CN108165069B (en) High-content aqueous graphene dispersion liquid and preparation method thereof
CN111410855A (en) Preparation method of high-surface-activity/high-hydrophilicity dispersion type carbon black
CN112940282A (en) Composite modified graphene modified waterborne polyurethane emulsion and preparation method thereof
CN112121774A (en) Preparation method of hydrophilic graphene film
CN114958038A (en) Preparation method of water-soluble carbon black
CN108584934B (en) Sulfonic group functionalized graphene dispersion system and preparation method thereof
CN110591413B (en) Preparation method of photodegradation-resistant, dust-free and easy-to-disperse organic pigment solid color paste
CN113502089B (en) Color paste for ink of water-based pen
CN111359458A (en) Molybdenum disulfide oxide modified flat nanofiltration membrane as well as preparation method and application thereof
CN111334096B (en) Preparation method and product of graphene oxide coated modified carbon black
CN115646196A (en) Amphiphilic graft polymer hydrophilic modified polymer ultrafiltration membrane and preparation method thereof
Mohammadi et al. Effect of concentration of surfactant and additive on morphology of polyaniline nanocomposites prepared in aqueous solution
CN114574001B (en) Method for preparing hydrophilic carbon black through biomimetic modification of phenolic amine and hydrophilic carbon black
CN112547028B (en) Preparation method and application of rosin-based magnetic porous microspheres for adsorbing cationic dye
CN113307523A (en) Method for preparing water-soluble carbon black, water-soluble carbon black and application thereof
CN110452568B (en) Anticorrosive paint, preparation method thereof and anticorrosive coating
CN113666345B (en) Preparation method and application of graphite oxide phase carbon nitride
CN110698582A (en) Dispersing agent, organic color paste containing dispersing agent and preparation method
CN115569632B (en) Magnetic activated carbon fiber adsorbent and preparation method thereof
CN114574006B (en) Preparation method of superfine special carbon black
CN117659771A (en) High-solid-content nano water-based color paste and preparation method thereof
CN109880404B (en) Blue electrophoretic particle for electronic ink display and preparation method thereof
CN117487098A (en) Preparation method and application of modified water-based self-dispersion carbon black

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
CB02 Change of applicant information

Address after: 242000 West District (Shijie Town) of Guangde Economic Development Zone, Xuancheng City, Anhui Province

Applicant after: Anhui Delui New Materials Technology Co.,Ltd.

Address before: Wanneng Road, Chengxi Industrial Park, Jingchuan Town, Jing County, Xuancheng City, Anhui Province, 242000

Applicant before: Anhui Delui New Materials Technology Co.,Ltd.

CB02 Change of applicant information