CN112210233B - Preparation method of conductive carbon black - Google Patents
Preparation method of conductive carbon black Download PDFInfo
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Abstract
The invention relates to a preparation method of conductive carbon black, which mainly solves the problem that an effective regeneration method of byproduct carbon black of acetylene preparation from natural gas is lacked. The preparation method of the conductive carbon black comprises the following steps: a) acid treatment: treating the raw material carbon black with an acid solution to obtain a conductive carbon black intermediate product I; (b) alkali treatment: treating the conductive carbon black intermediate product I with an alkali solution, and treating the conductive carbon black intermediate product II; (c) loading salt: mixing the conductive carbon black intermediate product II with a salt-containing aqueous solution to obtain a conductive carbon black intermediate product III; (d) and (3) calcining: the technical scheme of calcining the conductive carbon black intermediate product III to obtain the conductive carbon black finished product better solves the problem and can be used in the recycling production of the byproduct carbon black in the process of preparing acetylene from natural gas in an industrial device.
Description
Technical Field
The invention relates to a preparation method of conductive carbon black, in particular to a preparation method of conductive carbon black prepared from a byproduct carbon black produced in acetylene preparation from natural gas.
Background
The carbon black as a byproduct of acetylene preparation from natural gas refers to that in the process of preparing acetylene by partial oxidation of natural gas, because the reaction is carried out at an extremely high temperature, unsaturated hydrocarbons (such as acetylene) generated in part of the reaction process can undergo deep cracking reaction to generate carbon black, and the generated amount is about 50kg/t of acetylene, although the retention time is short. The main reaction process is that the raw materials of natural gas and oxygen are respectively heated to a certain temperature in a gas preheater and then mixed to enter a reaction furnace. One part of natural gas is burnt to provide heat energy for reaction, and the other part of natural gas is subjected to cracking reaction at about 1500 ℃ to produce acetylene. Acetylene is easily decomposed into carbon black and hydrogen at high temperature, so the optimum reaction time at high temperature is only a few thousandths of a second, and the reaction is terminated by water spray quenching. Although the reaction time is extremely short, carbon black is produced.
At present, two main treatment modes of the generated carbon black are provided, firstly, the carbon black is mixed into a coal boiler for combustion, and the combustion process is unstable and the using amount is limited due to low heat value and large water content of the carbon black; secondly, the carbon black is buried, so that the carbon black treatment cost is increased and the environmental damage is large. The purpose of exploring the utilization way of the byproduct carbon black is to convert the byproduct carbon black into a carbon black product with wide application, widen the application of the byproduct carbon black, make the best use of the product and realize the maximization of the benefit of the process for preparing acetylene from natural gas.
The Wangping et al in article "structural analysis and utilization discussion of by-product carbon black from acetylene preparation by natural gas" think that the valuable recycling ways of by-product carbon black from acetylene preparation by natural gas are mainly the following four ways: (1) the modified carbon black is used for asphalt modification, (2) modified pigment carbon black preparation, (3) modified conductive carbon black preparation, and (4) modified activated carbon preparation; however, since the by-product carbon black has a complicated structure and components, a reasonable recovery method cannot be proposed.
Disclosure of Invention
The invention aims to solve the technical problem that an effective regeneration method of a byproduct carbon black produced in acetylene preparation from natural gas is lacked in the prior art, and provides a preparation method of conductive carbon black based on the byproduct carbon black produced in acetylene preparation from natural gas.
In order to solve the technical problems, the technical scheme of the invention is as follows:
the preparation method of the conductive carbon black comprises the following steps:
(a) acid treatment: treating the raw material carbon black with an acid solution to obtain a conductive carbon black intermediate product I;
(b) alkali treatment: treating the conductive carbon black intermediate product I with an alkali solution, and treating the conductive carbon black intermediate product II;
(c) loading salt: mixing the conductive carbon black intermediate product II with a salt-containing aqueous solution to obtain a conductive carbon black intermediate product III;
(d) and (3) calcining: and calcining the conductive carbon black intermediate product III to obtain a conductive carbon black finished product.
In the technical scheme, the concentration of the acid solution is preferably 0.5-7.0 mol/L, and an acid water solution is preferably selected.
In the above technical scheme, the concentration of the acid solution is, for example, but not limited to, 0.6mol/L, 0.7mol/L, 0.8mol/L, 1.0mol/L, 1.5mol/L, 2.0mol/L, 2.5mol/L, 3.0mol/L, 3.5mol/L, 4.0mol/L, 4.5mol/L, 5.0mol/L, 5.5mol/L, 6.0mol/L, 6.5mol/L, and the like.
In the above technical scheme, the acid treatment temperature is preferably 60 to 90 ℃, for example, but not limited to, 65 ℃, 70 ℃, 75 ℃, 80 ℃, 85 ℃ and the like.
In the technical scheme, the acid treatment time is preferably 24-48 h, such as but not limited to 26h, 28h, 30h, 32h, 34h, 36h, 38h, 40h, 42h, 44h, 46h and the like.
In the above technical solution, the ratio of the gram number of the raw material carbon black to the milliliter number of the acid solution may be preferably 1 (0.5 to 2.5), for example but not limited to 1:0.6, 1:0.8, 1:1, 1:1.2, 1:1.4, 1:1.6, 1:1.8, 1:2, 1:2.2, 1:2.4, and the like.
In the above technical solution, the acid solution preferably includes at least one selected from the group consisting of hydrochloric acid, nitric acid, and perchloric acid.
In the above technical solution, the acid includes a first acid and a second acid, the first acid is at least one selected from nitric acid and perchloric acid, and the second acid is hydrochloric acid. We have found that there is an interactive, synergistic effect between the first acid and the second acid in reducing the resistivity of the conductive carbon black. In this case, the ratio of the first acid to the second acid is not particularly limited, and any comparable mutual accelerating effect can be obtained. For example, but not limited to, the molar ratio of the first acid to the second acid can be 1 to 10, and more specific non-limiting values within this range can be, for example, 1.5, 2, 2.5, 3, 3.5, 4, 4.5, 5, 5.5, 6, 6.5, 7, 7.5, 8, 8.5, 9, 9.5, and so forth.
In the above technical solution, the concentration of the alkali solution is preferably 8 to 14mol/L, for example, but not limited to, 8.5mol/L, 9mol/L, 9.5mol/L, 10mol/L, 10.5mol/L, 11mol/L, 11.5mol/L, 12mol/L, 12.5mol/L, 13mol/L, 13.5mol/L, and the like.
In the above technical scheme, the alkali treatment temperature is preferably 20 to 40 ℃, for example, but not limited to, 25 ℃, 30 ℃, 35 ℃ and the like.
In the technical scheme, the alkali treatment time is preferably 12-24 h, such as but not limited to 14h, 16h, 18h, 20h, 22h and the like.
In the above technical scheme, the ratio of the gram number of the conductive carbon black intermediate product I to the milliliter number of the alkali solution can be preferably 1: 0.5-5; such as, but not limited to, 1:0.6, 1:0.8, 1:1, 1:1.2, 1:1.4, 1:1.6, 1:1.8, 1:2, 1:2.2, 1:2.4, 1:3, 1:4, and the like.
In the above technical solution, the alkali preferably includes an alkali metal hydroxide, and more preferably includes one of the group consisting of sodium hydroxide and potassium hydroxide.
In the technical scheme, the salt concentration in the salt-containing aqueous solution is preferably 0.3-2.0 mol/L, and the salt preferably comprises one of ferric nitrate, ferrous nitrate and aluminum nitrate.
In the above technical scheme, the ratio of the grams of the conductive carbon black intermediate product II to the milliliters of the saline solution may be 1:0.5 to 10, for example, but not limited to, 1:0.6, 1:0.8, 1:1, 1:1.2, 1:1.4, 1:1.6, 1:1.8, 1:2, 1:2.2, 1:2.4, 1:3, 1:4, 1:5, 1:6, 1:7, 1:8, 1:9, and the like.
In the above technical solution, the calcination atmosphere is preferably carbon dioxide.
In the above technical scheme, the calcination temperature is preferably 800 to 1300 ℃, such as but not limited to 900 ℃, 950 ℃, 1000 ℃, 1050 ℃, 1100 ℃, 1150 ℃, 1200 ℃, 1250 ℃ and the like.
In the above technical solution, the calcination time is preferably 1 to 5 hours, such as but not limited to 1.5 hours, 2 hours, 2.5 hours, 3 hours, 3.5 hours, 4 hours, 4.5 hours, and the like.
The sodium hydroxide alkali solution is adopted for treatment, so that the conductive groups in the conductive carbon black can be improved, and the conductive performance of the conductive carbon black can be improved; the shape of the pore structure can be optimized by adopting the carbon dioxide atmosphere for calcination, and the conductivity of the carbon dioxide can be enhanced.
The second part of the carbon black of the national standard GB/T3780.2-2003 is adopted: the DBP oil absorption value of the conductive carbon black is measured by the experimental method specified in the determination of dibutyl phthalate absorption value; the national standard GB/T3781.9-2006 acetylene black part 9 is adopted: measurement of resistivity the resistivity of the conductive carbon black was measured by the method specified in "measurement of resistivity". The larger the oil absorption value and the smaller the resistivity, the better the conductivity.
Experimental results show that compared with the original byproduct carbon black DBP oil absorption value, the preparation method of the conductive carbon black provided by the invention has the advantages that the DBP oil absorption value is greatly improved, the resistivity is obviously reduced, and a better technical effect is achieved.
Detailed Description
[ example 1 ]
(1) Preparation of conductive carbon black
A step (a): adding the byproduct carbon black with the drying mass of 1000g into an acid solution with the volume of 1000ml, wherein the concentration of hydrochloric acid in the acid solution is 1.5mol/L, and standing at the temperature of 60 ℃ for 40 h; filtering, washing with deionized water until the eluate is neutral, and drying to obtain conductive carbon black intermediate product I;
a step (b): taking the conductive carbon black intermediate product I with the mass of 800g, adding 800ml of alkali solution, standing for 20h at the temperature of 20 ℃, filtering, washing with deionized water until the eluate is neutral, and drying to obtain a conductive carbon black intermediate product II;
step (c): adding 800g of the conductive carbon black intermediate product II into 800ml of aqueous solution containing salts, wherein the salts are ferric nitrate, the concentration of the ferric nitrate is 0.3mol/L, standing for 10h, filtering and drying to obtain a conductive carbon black intermediate product III;
step (d): and calcining the conductive carbon black intermediate product III for 2 hours at the temperature of 900 ℃ in a carbon dioxide atmosphere to obtain a conductive carbon black finished product.
(2) Product analysis characterization
The resistivity of the conductive carbon black is measured by a resistivity meter, and the DBP oil absorption value of the conductive carbon black is measured by a dimethyl phthalate (DBP) adsorption method.
For convenience of comparison, the conditions for preparing the conductive carbon black and the data on the physical properties of the conductive carbon black are shown in tables 1 and 2, respectively.
[ example 2 ]
(1) Preparation of conductive carbon black
Step (a): adding the byproduct carbon black with the drying mass of 1000g into an acid solution with the volume of 1000ml, wherein the concentration of nitric acid in the acid solution is 7.0mol/L, and standing at the temperature of 90 ℃ for 40 h; filtering, washing with deionized water until the eluate is neutral, and drying to obtain conductive carbon black intermediate product I;
step (b): taking 800g of conductive carbon black intermediate product I, adding 800ml of alkali solution, standing for 20h at the temperature of 40 ℃ with the concentration of potassium hydroxide in the alkali solution being 14mol/L, filtering, washing with deionized water until eluate is neutral, and drying to obtain conductive carbon black intermediate product II;
step (c): adding 800g of the conductive carbon black intermediate product II into 800ml of aqueous solution containing salts, wherein the salts are ferric nitrate, the concentration of the ferric nitrate is 2.0mol/L, standing for 10h, filtering and drying to obtain a conductive carbon black intermediate product III;
step (d): and calcining the conductive carbon black intermediate product III for 2 hours at the temperature of 1200 ℃ in a carbon dioxide atmosphere to obtain a conductive carbon black finished product.
For convenience of comparison, the conditions for preparing the conductive carbon black and the data on the physical properties of the conductive carbon black are shown in tables 1 and 2, respectively.
[ example 3 ]
(1) Preparation of conductive carbon black
Step (a): adding 1000g of dried by-product carbon black into 1000ml of acid solution, wherein the concentration of perchloric acid in the acid solution is 4.2mol/L, and standing at the temperature of 80 ℃ for 40 hours; filtering, washing with deionized water until the eluate is neutral, and drying to obtain a conductive carbon black intermediate product I;
step (b): taking 800g of conductive carbon black intermediate product I, adding 800ml of alkali solution, standing for 20h at the temperature of 30 ℃ with the concentration of sodium hydroxide of 11mol/L in the alkali solution, filtering, washing with deionized water until eluate is neutral, and drying to obtain a conductive carbon black intermediate product II;
step (c): adding 800g of the conductive carbon black intermediate product II into 800ml of aqueous solution containing salts, wherein the salts are ferric nitrate, the concentration of the ferric nitrate is 1.2mol/L, standing for 10h, filtering and drying to obtain a conductive carbon black intermediate product III;
step (d): and calcining the conductive carbon black intermediate product III for 2 hours at 1050 ℃ in a carbon dioxide atmosphere to obtain a conductive carbon black finished product.
For convenience of comparison, the conditions for preparing the conductive carbon black and the data on the physical properties of the conductive carbon black are shown in tables 1 and 2, respectively.
[ example 4 ]
(1) Preparation of conductive carbon black
Step (a): adding 1000g of dried by-product carbon black into 1000ml of acid solution, wherein the concentration of hydrochloric acid in the acid solution is 0.84mol/L, the concentration of nitric acid in the acid solution is 3.36mol/L, and standing at the temperature of 80 ℃ for 40 hours; filtering, washing with deionized water until the eluate is neutral, and drying to obtain conductive carbon black intermediate product I;
a step (b): taking 800g of conductive carbon black intermediate product I, adding 800ml of alkali solution, standing for 20h at the temperature of 30 ℃, filtering, washing with deionized water until eluate is neutral, and drying to obtain conductive carbon black intermediate product II;
step (c): adding 800g of the conductive carbon black intermediate product II into 800ml of aqueous solution containing salts, wherein the salts are 1.2mol/L of ferric nitrate, standing for 10h, filtering and drying to obtain a conductive carbon black intermediate product III;
step (d): and calcining the conductive carbon black intermediate product III for 2 hours at 1050 ℃ in a carbon dioxide atmosphere to obtain a conductive carbon black finished product.
For convenience of comparison, the conditions for preparing the conductive carbon black and the data on the physical properties of the conductive carbon black are shown in tables 1 and 2, respectively.
[ example 5 ] A method for producing a polycarbonate
(1) Preparation of conductive carbon black
Step (a): adding the byproduct carbon black with the drying mass of 1000g into an acid solution with the volume of 1000ml, wherein the concentration of hydrochloric acid in the acid solution is 0.6mol/L, the concentration of perchloric acid in the acid solution is 3.6mol/L, and standing at the temperature of 80 ℃ for 40 h; filtering, washing with deionized water until the eluate is neutral, and drying to obtain conductive carbon black intermediate product I;
a step (b): taking 800g of conductive carbon black intermediate product I, adding 800ml of alkali solution, standing for 20h at the temperature of 30 ℃ with the concentration of sodium hydroxide of 11mol/L in the alkali solution, filtering, washing with deionized water until eluate is neutral, and drying to obtain a conductive carbon black intermediate product II;
step (c): adding 800g of the conductive carbon black intermediate product II into 800ml of aqueous solution containing salts, wherein the salts are ferric nitrate, the concentration of the ferric nitrate is 1.2mol/L, standing for 10h, filtering and drying to obtain a conductive carbon black intermediate product III;
a step (d): and calcining the conductive carbon black intermediate product III for 2 hours at 1050 ℃ in a carbon dioxide atmosphere to obtain a conductive carbon black finished product.
For convenience of comparison, the conditions for preparing the conductive carbon black and the data on the physical properties of the conductive carbon black are shown in tables 1 and 2, respectively.
[ example 6 ]
(1) Preparation of conductive carbon black
Step (a): adding the byproduct carbon black with the drying mass of 1000g into an acid solution with the volume of 1000ml, wherein the concentration of hydrochloric acid in the acid solution is 4.2mol/L, and standing at the temperature of 80 ℃ for 40 h; filtering, washing with deionized water until the eluate is neutral, and drying to obtain conductive carbon black intermediate product I;
a step (b): taking 800g of conductive carbon black intermediate product I, adding 800ml of alkali solution, standing for 20h at the temperature of 30 ℃ with the concentration of sodium hydroxide of 11mol/L in the alkali solution, filtering, washing with deionized water until eluate is neutral, and drying to obtain a conductive carbon black intermediate product II;
step (c): adding 800g of the conductive carbon black intermediate product II into 800ml of aqueous solution containing salts, wherein the salts are ferric nitrate, the concentration of the ferric nitrate is 1.2mol/L, standing for 10h, filtering and drying to obtain a conductive carbon black intermediate product III;
step (d): and calcining the conductive carbon black intermediate product III for 2 hours at 1050 ℃ in a carbon dioxide atmosphere to obtain a conductive carbon black finished product.
For comparison, the conditions for preparing the conductive carbon black and the physical property data of the conductive carbon black are shown in tables 1 and 2, respectively.
[ example 7 ]
(1) Preparation of conductive carbon black
Step (a): adding the byproduct carbon black with the drying mass of 1000g into an acid solution with the volume of 1000ml, wherein the concentration of nitric acid in the acid solution is 4.2mol/L, and standing at the temperature of 80 ℃ for 40 h; filtering, washing with deionized water until the eluate is neutral, and drying to obtain conductive carbon black intermediate product I;
step (b): taking the conductive carbon black intermediate product I with the mass of 800g, adding 800ml of alkali solution, standing for 20h at the temperature of 30 ℃ with the concentration of sodium hydroxide being 11mol/L, filtering, washing with deionized water until the eluate is neutral, and drying to obtain a conductive carbon black intermediate product II;
step (c): adding 800g of the conductive carbon black intermediate product II into 800ml of aqueous solution containing salts, wherein the salts are ferric nitrate, the concentration of the ferric nitrate is 1.2mol/L, standing for 10h, filtering and drying to obtain a conductive carbon black intermediate product III;
step (d): and calcining the conductive carbon black intermediate product III for 2 hours at 1050 ℃ in a carbon dioxide atmosphere to obtain a conductive carbon black finished product.
For convenience of comparison, the conditions for preparing the conductive carbon black and the data on the physical properties of the conductive carbon black are shown in tables 1 and 2, respectively.
[ COMPARATIVE EXAMPLE 1 ]
The resistivity of the conductive carbon black is measured by a resistivity meter without any treatment of the byproduct carbon black, and the DBP oil absorption value of the conductive carbon black is measured by a dimethyl phthalate (DBP) adsorption method.
For convenience of comparison, the conditions for preparing the conductive carbon black and the data on the physical properties of the conductive carbon black are shown in tables 1 and 2, respectively.
TABLE 1
TABLE 2
| DBP oil absorption number (ml/100g) | Resistivity (k omega. cm) | |
| Example 1 | 240 | 0.44 |
| Example 2 | 290 | 0.39 |
| Example 3 | 300 | 0.37 |
| Example 4 | 302 | 0.30 |
| Example 5 | 321 | 0.32 |
| Example 6 | 301 | 0.36 |
| Example 7 | 299 | 0.38 |
| Comparative example 1 | 52 | 0.93 |
Claims (10)
1. The preparation method of the conductive carbon black comprises the following steps:
(a) acid treatment: treating the raw material carbon black with an acid solution to obtain a conductive carbon black intermediate product I;
(b) alkali treatment: treating the conductive carbon black intermediate product I with an alkali solution, and treating the conductive carbon black intermediate product II;
(c) loading salt: mixing the conductive carbon black intermediate product II with a salt-containing aqueous solution to obtain a conductive carbon black intermediate product III;
(d) and (3) calcining: calcining the conductive carbon black intermediate product III to obtain a conductive carbon black finished product; wherein the raw material carbon black is a byproduct carbon black of a process for preparing acetylene based on natural gas;
the acid includes a first acid selected from at least one of nitric acid and perchloric acid, and a second acid that is hydrochloric acid;
the base comprises sodium hydroxide or potassium hydroxide;
the salt comprises ferric nitrate, ferrous nitrate or aluminum nitrate.
2. The method according to claim 1, wherein the concentration of the acid solution is 0.5 to 7.0mol/L, and the acid treatment temperature is 60 to 90 ℃.
3. The method according to claim 1, wherein the acid treatment time is 24 to 48 hours.
4. The process according to claim 1, wherein the ratio of the gram amount of the carbon black as the raw material to the milliliter amount of the acid solution is 1 (0.5 to 2.5).
5. The method according to claim 1, wherein the concentration of the alkali solution is 8 to 14 mol/L.
6. The method according to claim 1, wherein the alkali treatment temperature is 20 to 40 ℃.
7. The process according to claim 1, wherein the alkali treatment time is 12 to 24 hours.
8. The process according to claim 1, wherein the ratio of the gram quantity of the conductive carbon black intermediate I to the milliliter quantity of the alkali solution is 1 (0.5 to 5).
9. The method according to claim 1, wherein the salt concentration in the saline solution is 0.3 to 2.0mol/L, and the ratio of the gram quantity of the conductive carbon black intermediate II to the milliliter quantity of the saline solution is 1 (0.5 to 10).
10. The method according to claim 1, wherein the calcination atmosphere is carbon dioxide, the calcination temperature is 800 to 1300 ℃, and the calcination time is 1 to 5 hours.
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