Modified pigment carbon black as well as preparation method and application thereof
By acidifying, dispersing, and modifying carbon black, the problem of poor storage stability was solved, and modified pigment carbon black that is not prone to coarsening, agglomeration, and stratification was prepared. When applied to soft PVC plastic color paste, it improved the coloring power and stability of the color paste.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-05-20
- Publication Date
- 2026-04-10
AI Technical Summary
Existing carbon black production methods produce products with poor storage stability, and they are prone to coarsening, agglomeration, and stratification during use.
Modified pigment carbon black is prepared by acidifying carbon black, mixing it with washed kaolin, dispersing it, and then mixing it with polydimethylsiloxane for modification.
Modified pigment carbon black does not exhibit coarsening, agglomeration, or stratification during use, thus improving storage stability and tinting strength, and enhancing abrasion resistance, hydrophobicity, and flexibility.
Smart Images
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Abstract
Description
Technical Field
[0001] This invention belongs to the field of plastic materials technology, specifically relating to a modified pigment carbon black, its preparation method, and its application. Background Technology
[0002] Carbon black is produced by the incomplete combustion or pyrolysis of hydrocarbons in the gas phase under strictly controlled process conditions. Its main component is elemental carbon, with small amounts of oxygen, hydrogen, and sulfur. It is a black powdery substance widely used in the flexible PVC plastics industry due to its excellent physical and chemical properties. As a colorant, conductive agent, and ultraviolet absorber in flexible PVC plastics, carbon black's applications mainly include enhancing the strength of plastics, improving their weather resistance, and increasing their electrical conductivity and antistatic properties. Currently, carbon black is produced using three methods: furnace method, tank method, and thermal cracking method. Among these, the oil furnace method is the most efficient and economical. However, carbon black produced by all three methods suffers from poor storage stability and is prone to coarsening, agglomeration, and stratification during use. Summary of the Invention
[0003] The purpose of this invention is to provide a modified pigment carbon black, its preparation method and application. The modified pigment carbon black prepared by this invention has excellent storage stability and does not exhibit coarsening, agglomeration or stratification during use.
[0004] To achieve the objectives of this invention, the following technical solutions are provided:
[0005] A method for preparing modified pigment carbon black includes the following steps:
[0006] Carbon black is acidified to obtain acidified carbon black;
[0007] The acidified carbon black and washed kaolin are mixed and dispersed to obtain dispersed carbon black;
[0008] The dispersed carbon black and polydimethylsiloxane are mixed and modified to obtain the modified pigment carbon black.
[0009] Preferably, the carbon black has a particle size of 800-1000 mesh and a tinting strength >130.
[0010] Preferably, the acid used in the acidification includes nitric acid and / or sulfuric acid.
[0011] Preferably, the concentration of the acid is 68-98 wt%; the mass ratio of the carbon black to the acid is 1:5-10%.
[0012] Preferably, the pH value of the acidified carbon black is 3 to 5.
[0013] Preferably, the polydimethylsiloxane has a viscosity of 500–1000 cps at 25°C.
[0014] Preferably, the mass ratio of the acidified carbon black, washed kaolin, and polydimethylsiloxane is 80-85:3-5:10-15.
[0015] Preferably, the dispersion treatment is ball milling dispersion; the dispersion speed is 1000-1500 r / min, the temperature is 60-80℃, and the time is 30-40 min.
[0016] The present invention also provides a modified pigment carbon black prepared by the preparation method described above, comprising dispersed carbon black and polydimethylsiloxane attached to the dispersed carbon black.
[0017] The present invention also provides the application of the modified pigment carbon black described in the above technical solution in color paste.
[0018] This invention provides a method for preparing modified pigment carbon black, comprising the following steps: acidifying carbon black to obtain acidified carbon black; mixing the acidified carbon black with water-washed kaolin and dispersing it to obtain dispersed carbon black; and mixing the dispersed carbon black with polydimethylsiloxane and modifying it to obtain the modified pigment carbon black. In this invention, acidification enhances the surface activity of the carbon black, improving the stability of the modified carbon black; water-washed kaolin improves the dispersibility of the carbon black, preventing coarsening, agglomeration, and stratification; and polydimethylsiloxane, as a brightening agent, coats and modifies the carbon black, improving its blackness and enhancing its abrasion resistance, hydrophobicity, and flexibility. Detailed Implementation
[0019] This invention provides a method for preparing modified pigment carbon black, comprising the following steps:
[0020] Carbon black is acidified to obtain acidified carbon black;
[0021] The acidified carbon black and washed kaolin are mixed and dispersed to obtain dispersed carbon black;
[0022] The dispersed carbon black and polydimethylsiloxane are mixed and modified to obtain the modified pigment carbon black.
[0023] In this invention, unless otherwise specified, all raw materials used in the preparation are preferably commercially available products well known to those skilled in the art.
[0024] This invention involves acidifying carbon black to obtain acidified carbon black. In this invention, the carbon black is preferably high-color high-carbon black; the high-color carbon black is preferably furnace black; the particle size of the carbon black is preferably 800-1000 mesh, more preferably 800-900 mesh; the tinting strength of the carbon black is preferably >130; and the pH value of the carbon black is preferably 7-10, more preferably 8-9.
[0025] In this invention, the acid used for acidification preferably includes nitric acid and / or sulfuric acid, more preferably nitric acid. In this invention, the concentration of the acid is preferably 68–98 wt%, more preferably 68–80 wt%. In this invention, the mass ratio of carbon black to acid is preferably 1:5–10%, more preferably 1:6–9%. In this invention, the pH value of the acidified carbon black is preferably 3–5, more preferably 4.
[0026] The present invention does not have any particular limitation on the acidification method, and any acidification method known to those skilled in the art can be used.
[0027] In this invention, the carbon black is preferably pulverized before acidification. The pulverization is preferably carried out in a circulating tubular air jet mill; the pulverization pressure is preferably 0.7–0.85 MPa, more preferably 0.8 MPa.
[0028] After obtaining acidified carbon black, the present invention mixes the acidified carbon black with water-washed kaolin and performs a dispersion treatment to obtain dispersed carbon black. In the present invention, the dispersion treatment is preferably ball milling. In the present invention, the dispersion speed is preferably 1000–1500 r / min, more preferably 1000–1300 r / min; the temperature is preferably 60–80℃, more preferably 60–70℃; and the time is preferably 30–40 min, more preferably 30–35 min. In the present invention, the grinding media of the ball mill is preferably alumina beads.
[0029] After obtaining dispersed carbon black, the present invention mixes the dispersed carbon black and polydimethylsiloxane and performs a modification treatment to obtain the modified pigment carbon black. In the present invention, the viscosity of the polydimethylsiloxane at 25°C is preferably 500–1000 cps, more preferably 600–800 cps. In the present invention, the mass ratio of the acidified carbon black, washed kaolin, and polydimethylsiloxane is preferably 80–85:3–5:10–15, more preferably 81–84:4–5:12–14. The conditions for the modification treatment in the present invention are not particularly limited, and methods well known to those skilled in the art can be used.
[0030] In this invention, the modified product is preferably pulverized after the modification treatment to obtain the modified pigment carbon black. In this invention, the pulverization is preferably performed using an air jet mill. In this invention, the particle size of the modified pigment carbon black is preferably 1000-1200 mesh, more preferably 1100-1200 mesh.
[0031] The present invention also provides a modified pigment carbon black prepared by the preparation method described above, comprising dispersed carbon black and polydimethylsiloxane attached to the dispersed carbon black.
[0032] In this invention, acidification enhances the surface activity of carbon black and improves the stability of modified carbon black; water-washed kaolin can improve the dispersibility of carbon black and prevent coarsening, agglomeration and stratification; polydimethylsiloxane, as a brightener, coats and modifies carbon black, which can improve the blackness of carbon black and enhance its wear resistance, hydrophobicity and flexibility.
[0033] The present invention also provides the application of the modified pigment carbon black described in the above technical solution in color paste.
[0034] In this invention, it is preferable to disperse dioctyl terephthalate (DOTP), fatty alcohol polyoxyethylene ether phosphate, and modified pigment carbon black to obtain a color paste.
[0035] In this invention, the preferred mass ratio of DOTP, fatty alcohol polyoxyethylene ether phosphate, and modified pigment carbon black is 55–75:20–35:5–10, more preferably 55–65:25–35:6–8. In this invention, the dispersion is preferably carried out in a ball mill; the preferred dispersion rate is 800–1000 r / min, more preferably 90–1000 r / min; the preferred dispersion time is 30–40 min, more preferably 35–40 min. In this invention, the dispersion is further preferably followed by grinding; the grinding is preferably carried out in a bead mill.
[0036] The modified pigment carbon black provided by this invention can be used in color pastes at a content of up to 35%. At the same time, it does not coarsen, agglomerate, or separate during use, thus improving the coloring power and storage stability of the color paste.
[0037] To further illustrate the present invention, the modified pigment carbon black, its preparation method, and its application provided by the present invention are described in detail below with reference to the embodiments, but these should not be construed as limiting the scope of protection of the present invention.
[0038] Example 1
[0039] High-pigment furnace black (ZY-900) (800 mesh particle size) is mixed with nitric acid (68 wt%) at 7.5 wt% of the carbon black mass, and acidified to obtain acidified carbon black;
[0040] By mass fraction, 83.3% acidified carbon black and 4.2% washed kaolin were placed in a ball mill with alumina beads as the grinding media and dispersed at 1000 r / min and 60℃ for 30 min. Then, the mixture was transported by a blower through a pipeline to a modified mixer and mixed with 12.5% polydimethylsiloxane. After pulverization, modified pigment carbon black was obtained.
[0041] Comparative Example 1
[0042] By mass fraction, 83.3% commercially available channel black and 4.2% calcined washed kaolin were placed in a ball mill with alumina beads as the grinding medium and dispersed at 1000 r / min and 60℃ for 30 min. Then, the mixture was transported by a blower through a pipeline to a modified mixer and mixed with 12.5% polydimethylsiloxane. After pulverization, modified pigment carbon black was obtained.
[0043] Comparative Example 2
[0044] By mass fraction, 83.3% high-pigment furnace black (zy-900) and 4.2% calcined washed kaolin were placed in a ball mill with alumina beads as the grinding media and dispersed at 1000 r / min and 60℃ for 30 min. Then, the mixture was transported to a modified mixer by a blower and mixed with 12.5% polydimethylsiloxane. After pulverization, modified pigment carbon black was obtained.
[0045] Comparative Example 3
[0046] High-pigment furnace black (ZY-900) is mixed with nitric acid (68 wt%) at 7.5 wt% of the carbon black mass, and acidified to obtain acidified carbon black.
[0047] By mass fraction, 83.3% of acidified carbon black was placed in a ball mill with alumina beads as the grinding medium and dispersed at 1000 r / min and 60℃ for 30 min. Then, it was transported by a blower through a pipeline to a modified mixer and mixed with 16.7% polydimethylsiloxane. After pulverization, modified pigment carbon black was obtained.
[0048] Comparative Example 4
[0049] High-pigment furnace black (ZY-900) is mixed with nitric acid (68 wt%) at 7.5 wt% of the carbon black mass, and acidified to obtain acidified carbon black.
[0050] Modified pigment carbon black was obtained by placing 95.8% acidified carbon black and 4.2% calcium carbonate in a ball mill with alumina beads as the grinding medium, dispersing them at 1000 r / min and 60℃ for 30 min, and then pulverizing them.
[0051] Comparative Example 5
[0052] Commercially available channel black.
[0053] Comparative Example 6
[0054] Commercially available high-pigment furnace black (ZY-900).
[0055] Comparative Example 7
[0056] The acidification furnace carbon black was prepared according to the technical solution described in Example 1.
[0057] Test Example 1
[0058] The carbon black described in Example 1 and Comparative Examples 1-7 were tested according to the indicators listed in Table 1. The test results are shown in Table 1.
[0059] Table 1. Performance test results of the carbon black described in Example 1 and Comparative Examples 1-7
[0060]
[0061] As shown in Table 1, the iodine absorption value of the modified carbon black decreased, it exhibited better dispersibility, and its coloring strength was improved.
[0062] Test Example 2
[0063] By mass fraction, 57% DOTP and 8% fatty alcohol polyoxyethylene ether phosphate were mixed, and 35% of the carbon black described in Example 1 and Comparative Examples 1-7 were added respectively. The mixture was dispersed at 1000 r / min for 40 min, and then ground twice in a bead mill to obtain a color paste.
[0064] The above color paste was stored at 60℃ for 1 week, and the changes in the state of the color paste and the particle size of carbon black in the color paste were observed. The results are shown in Table 2.
[0065] Table 2. Test results of the color paste prepared from the carbon black described in Example 1 and Comparative Examples 1-7.
[0066]
[0067] As shown in Table 2, the modified carbon black produces soft PVC plastic pigments with good fineness and good storage stability.
[0068] Test Example 3
[0069] By mass fraction, 57% DOTP and 8% fatty alcohol polyoxyethylene ether phosphate were mixed, and 35% of the carbon black described in Example 1 and Comparative Examples 2-3, as well as commercially available black masterbatch, were added respectively. The mixture was dispersed at 1000 r / min for 40 min, and then ground twice in a bead mill to obtain a color paste. The color paste was then allowed to stand at 25°C for 24 h, and the blackness of the soft PVC plastic color paste and the particle size of the carbon black in the soft PVC plastic color paste were tested. The test results are shown in Table 3.
[0070] Table 3. Performance test results of flexible PVC plastics prepared from Examples 1, Comparative Examples 2-3, and commercially available black masterbatch.
[0071]
[0072] As shown in Table 3, the modified carbon black produces a better blackness in the production of soft PVC plastic color paste.
[0073] Although the above embodiments have provided a detailed description of the present invention, they are only some embodiments of the present invention, and not all embodiments. People can obtain other embodiments based on these embodiments without creative effort, and these embodiments all fall within the protection scope of the present invention.
Claims
1. A method for producing a modified pigment carbon black, characterized by, The method comprises the following steps: acidifying carbon black to obtain acidified carbon black; mixing the acidified carbon black and water-washed kaolin, and dispersing to obtain dispersed carbon black; mixing the dispersed carbon black and polydimethylsiloxane, and modifying to obtain the modified pigment carbon black.
2. The production method according to claim 1, characterized by, The particle size of the carbon black is 800-1000 mesh, and the tinting strength is >130.
3. The production method according to claim 1, characterized by, The acid used in the acidification comprises nitric acid and / or sulfuric acid.
4. The production method according to claim 3, characterized by, The concentration of the acid is 68-98wt%, and the mass ratio of the carbon black to the acid is 1:5-10%.
5. The preparation method according to claim 1, characterized in that, The pH value of the acidified carbon black is 3-5.
6. The method of claim 1, wherein, The viscosity of the polydimethylsiloxane at 25℃ is 500-1000cps.
7. The production method according to claim 1 or 6, characterized by, The mass ratio of the acidified carbon black, water-washed kaolin and polydimethylsiloxane is 80-85:3-5:10-15.
8. The method of claim 1, wherein, The dispersing is ball-milling, the rotating speed is 1000-1500r / min, the temperature is 60-80℃, and the time is 30-40min.
9. The modified carbon black prepared by the process according to any one of claims 1 to 8, characterized in that The product comprises dispersed carbon black and polydimethylsiloxane attached to the dispersed carbon black.
10. The use of the modified pigment carbon black of claim 9 in color paste.