A preparation process of highly dispersed carbon black

Abstract

The present invention relates to the technical field of carbon black, and in particular to a preparation process of highly dispersible carbon black, comprising the following contents: adding a first mixed amino acid solution to a carbon black powder with a particle size of 15-20 μm, heating, ultrasonically dispersing, and then adding a first mixed dispersant, adding a second mixed amino acid solution to the material obtained after microwave treatment and grinding treatment, heating, ultrasonically dispersing, and then adding a second mixed dispersant, continuing microwave treatment, grinding treatment, and drying to obtain a highly dispersible carbon black product. The carbon black powder is treated with the first mixed amino acid solution and the first mixed dispersant so that a first coating layer is formed on the surface of the carbon black powder, and then treated with the second mixed amino acid solution and the second mixed dispersant so that a second coating layer is formed on the surface of the carbon black powder; each carbon black particle contains a double coating layer, and the first coating layer and the second coating layer can hinder the collision and condensation between the carbon black particles, thereby greatly improving the dispersibility of the carbon black.

Description

Technical Field

[0001] The invention relates to the technical field of carbon black, and in particular to a preparation process of highly dispersed carbon black. Background Art

[0002] Carbon black is a commonly used inorganic black pigment. Carbon black with fine enough particle size and uniform dispersion has obvious advantages over other black pigments in terms of blackness and hiding rate. However, the electrostatic effect between carbon black particles and the strong aggregation between carbon black particles will lead to adsorption problems between particles and unstable storage performance. Over time, carbon black will flocculate, which will eventually affect the use of carbon black. Currently, oxidation treatment or surfactant treatment is used to improve the dispersibility of carbon black, but the dispersibility of carbon black is not ideal and its agglomeration problem in aqueous systems cannot be solved. Therefore, in view of the above problems, it is necessary to develop a preparation process for highly dispersible carbon black. Summary of the invention

[0003] The technical problem to be solved by the present invention is: in view of the deficiencies of the prior art, a preparation process of highly dispersed carbon black is provided, by which a highly dispersed carbon black product can be obtained.

[0004] In order to solve the above technical problems, the technical solution of the present invention is:

[0005] A preparation process of highly dispersible carbon black, the preparation process comprising the following steps:

[0006] (1) Take carbon black powder with a particle size of 15-20 μm, add the first mixed amino acid solution, heat, ultrasonically disperse, and collect the liquid for later use;

[0007] (2) taking the liquid material in step (1), adding the first mixed dispersant, subjecting to microwave treatment and grinding, and obtaining a material for later use;

[0008] (3) Take the material described in step (2), add the second mixed amino acid solution, heat and ultrasonically disperse, and the obtained liquid is set aside;

[0009] (4) Take the liquid prepared in step (3), add a second mixed dispersant, perform microwave treatment, grind, and dry to obtain a highly dispersed carbon black product.

[0010] As an improved technical solution, the carbon black powder in step (1) is mixed with the first mixed amino acid solution in a mass volume ratio of 1:2-3; the first mixed amino acid solution is mixed with hydroxyproline, histidine and purified water in a mass volume ratio of 1-3:1-2:6-8.

[0011] As an improved technical solution, in step (1), the temperature is heated to 60-70° C., the power of the ultrasonic dispersion is 550-650 W, and the dispersion time is 10-20 min.

[0012] As an improved technical solution, the feed liquid and the first mixed dispersant in step (2) are added in a mass ratio of 1:0.1-0.3; the first mixed dispersant includes hexadecyl monopotassium phosphate and sodium lignin sulfonate, and the hexadecyl monopotassium phosphate and sodium lignin sulfonate are mixed in a mass ratio of 1:1-2.

[0013] As an improved technical solution, the power of the microwave treatment in step (2) is 300-400W, and the temperature of the liquid after the microwave treatment for 5-12 minutes is 80-90°C.

[0014] As an improved technical solution, the grinding time in step (2) is 15-25 minutes.

[0015] As an improved technical solution, the material in step (3) is mixed with the second mixed amino acid solution at a mass volume ratio of 1:2.5-3.5; the second mixed amino acid solution is an aqueous solution of pyroglutamic acid and arginine, wherein the pyroglutamic acid and arginine are mixed with purified water at a mass volume ratio of 2-3:1-2:6-9.

[0016] As an improved technical solution, in step (3), the heating temperature is 92-98°C, the power of ultrasonic dispersion treatment is 450-550W, and the dispersion time is 20-30min.

[0017] As an improved technical solution, the feed liquid in step (4) is mixed with the second mixed dispersant in a mass ratio of 1:0.1-0.3; the second mixed dispersant is polar amide wax, fatty acid methyl ester polyoxyethylene ether and sodium dodecylbenzene sulfonate, and the polar amide wax, fatty acid methyl ester polyoxyethylene ether and sodium dodecylbenzene sulfonate are mixed in a mass ratio of 1-2:1:0.5-1.5.

[0018] As an improved technical solution, the power of the microwave treatment in step (4) is 500-600W, and the temperature of the liquid after 5-10 minutes of microwave treatment is 100-110°C.

[0019] As an improved technical solution, the grinding time in step (4) is 10-20 minutes.

[0020] After adopting the above technical solution, the beneficial effects of the present invention are:

[0021] The present invention adds a first mixed amino acid solution to a carbon black powder with a particle size of 15-20 μm, heats and ultrasonically disperses it, then adds a first mixed dispersant, adds a second mixed amino acid solution to the material obtained after microwave treatment and grinding treatment, heats and ultrasonically disperses it, then adds a second mixed dispersant, and continues microwave treatment, grinding treatment, and drying to obtain a highly dispersible carbon black product. The carbon black powder is treated with the first mixed amino acid solution and the first mixed dispersant so that a first coating layer is formed on the surface of the carbon black powder, and then treated with the second mixed amino acid solution and the second mixed dispersant so that a second coating layer is formed on the surface of the carbon black powder; each carbon black particle contains a double coating layer, and the first coating layer and the second coating layer can hinder the collision and condensation between the carbon black particles, avoid agglomeration, and greatly improve the dispersibility of the carbon black. DETAILED DESCRIPTION

[0022] In order to make the purpose, technical solution and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention. Example 1

[0023] A process for preparing highly dispersible carbon black comprises the following steps:

[0024] (1) Take 100 mg of carbon black powder with a particle size of 15 μm, add 200 ml of the first mixed amino acid solution (hydroxyproline, histidine and purified water are mixed in a mass volume ratio of 1:1:6, where the unit corresponding to w / v is mg / ml) at a mass volume ratio of 1:2, heat to 60°C, and ultrasonically disperse at a power of 550 W for 10 min. Collect 300 mg of the liquid for use;

[0025] (2) Take 300 mg of the liquid in step (1), add 30 mg of the first mixed dispersant (hexadecyl phosphate monopotassium salt and sodium lignin sulfonate mixed in a mass ratio of 1:0.1), microwave treat at a power of 300 W for 5 min, the temperature of the liquid is 80 ° C, and grind for 15 min to obtain 330 mg of material for standby use;

[0026] (3) Take 330 mg of the material in step (2), add 825 ml of the second mixed amino acid solution (pyroglutamic acid and arginine are mixed with purified water in a mass volume ratio of 2:1:6, where w / v corresponds to mg / ml) at a mass volume ratio of 1:2.5, heat to 92°C, and ultrasonically disperse at a power of 450 W for 20 min to obtain 1155 mg of the feed solution for use;

[0027] (4) Take 1155 mg of the liquid in step (3), add 115.5 mg of the second mixed dispersant (polar amide wax, fatty acid methyl ester polyoxyethylene ether and sodium dodecylbenzene sulfonate mixed in a mass ratio of 1:1:0.5) in a mass ratio of 1:0.1, microwave treat for 5 min at a power of 500 W, the material temperature is 100 ° C, grind for 10 min and then dry to obtain a highly dispersed carbon black product. Example 2

[0028] A process for preparing highly dispersible carbon black comprises the following steps:

[0029] (1) Take 100 mg of carbon black powder with a particle size of 18 μm, add 220 ml of the first mixed amino acid solution (hydroxyproline, histidine and purified water are mixed in a mass volume ratio of 1.5:1.2:6.5, where the unit corresponding to w / v is mg / ml) at a mass volume ratio of 1:2.2, heat to 62°C, and ultrasonically disperse (ultrasonic dispersion power is 580 w, dispersion time is 12 min), and collect 320 mg of the liquid for use;

[0030] (2) Take 320 mg of the liquid in step (1), add 48 mg of the first mixed dispersant (hexadecyl phosphate monopotassium salt and sodium lignin sulfonate mixed in a mass ratio of 1:0.15), microwave treat at a power of 320 W for 8 min, the temperature of the liquid is 82 ° C, and grind for 18 min to obtain 368 mg of material for standby use;

[0031] (3) Take 368 mg of the material in step (2), add 1030.4 ml of the second mixed amino acid solution (pyroglutamic acid and arginine are mixed with purified water in a mass volume ratio of 2.3:1.2:7, where the unit of w / v is mg / ml) at a mass volume ratio of 1:2.8, heat to 95°C, and disperse by ultrasound (ultrasonic dispersion treatment power is 480 W, dispersion time is 22 min), and obtain 1398.4 mg of the feed solution for use;

[0032] (4) Take 1398.4 mg of the liquid in step (3), add 209.76 mg of the second mixed dispersant (polar amide wax, fatty acid methyl ester polyoxyethylene ether and sodium dodecylbenzene sulfonate mixed in a mass ratio of 1.2:1:0.8) at a mass ratio of 1:0.15, microwave treat at a power of 520 W for 8 min, the material temperature is 102 ° C, grind for 12 min and dry to obtain a highly dispersed carbon black product. Example 3

[0033] A process for preparing highly dispersible carbon black comprises the following steps:

[0034] (1) Take 100 mg of carbon black powder with a particle size of 18 μm, add 250 ml of the first mixed amino acid solution (hydroxyproline, histidine and purified water are mixed in a mass volume ratio of 2:1.5:7, where the unit corresponding to w / v is mg / ml) at a mass volume ratio of 1:2.5, heat to 65°C, and ultrasonically disperse at a power of 600 W for 15 min. Collect 350 mg of the liquid for later use;

[0035] (2) Take 350 mg of the liquid in step (1), add 70 mg of the first mixed dispersant (hexadecyl phosphate monopotassium salt and sodium lignin sulfonate mixed in a mass ratio of 1:0.2), microwave treat for 10 min at a power of 350 W, the temperature of the liquid is 85 ° C, and grind for 20 min to obtain 420 mg of material for standby use;

[0036] (3) Take 420 mg of the material in step (2), add 1260 ml of the second mixed amino acid solution (pyroglutamic acid and arginine are mixed with purified water in a mass volume ratio of 2.5:1.5:8, where w / v corresponds to mg / ml) in a mass volume ratio of 1:3, heat to 95°C, and ultrasonically disperse at a power of 500 W for 25 min to obtain 1680 mg of the feed solution for use;

[0037] (4) Take 1680 mg of the liquid in step (3), add 336 mg of the second mixed dispersant (polar amide wax, fatty acid methyl ester polyoxyethylene ether and sodium dodecylbenzene sulfonate mixed in a mass ratio of 1.5:1:1) at a mass ratio of 1:0.2, microwave treat at a power of 550 W for 8 min, the material temperature is 105 ° C, grind for 15 min and then dry to obtain a highly dispersed carbon black product. Example 4

[0038] A process for preparing highly dispersible carbon black comprises the following steps:

[0039] (1) Take 100 mg of carbon black powder with a particle size of 20 μm, add 280 ml of the first mixed amino acid solution (hydroxyproline, histidine and purified water are mixed in a mass volume ratio of 2.5:1.8:8, where the unit corresponding to w / v is mg / ml) at a mass volume ratio of 1:2.8, heat to 68°C, and ultrasonically disperse at a power of 620 w for 18 min. Collect 380 mg of the liquid for use;

[0040] (2) Take 380 mg of the liquid in step (1), add 95 mg of the first mixed dispersant (hexadecyl phosphate monopotassium salt and sodium lignin sulfonate mixed in a mass ratio of 1:0.25), microwave treat at a power of 380 W for 10 min, the temperature of the liquid is 88 ° C, and grind for another 22 min to obtain 475 mg of the material for standby use;

[0041] (3) Take 475 mg of the material in step (2), add 1520 ml of the second mixed amino acid solution (pyroglutamic acid and arginine are mixed with purified water in a mass volume ratio of 2.8:1.8:9, where w / v corresponds to mg / ml) at a mass volume ratio of 1:3.2, heat to 98°C, and ultrasonically disperse at a power of 520 W for 28 min to obtain 1995 mg of the obtained liquid for use;

[0042] (4) Take 1995 mg of the liquid in step (3), add 498.75 mg of the second mixed dispersant (polar amide wax, fatty acid methyl ester polyoxyethylene ether and sodium dodecylbenzene sulfonate mixed in a mass ratio of 1.8:1:1.2) at a mass ratio of 1:0.25, microwave treat at a power of 580 W for 8 min, the material temperature is 108 ° C, grind for 18 min and then dry to obtain a highly dispersed carbon black product. Example 5

[0043] A process for preparing highly dispersible carbon black comprises the following steps:

[0044] (1) Take 100 mg of carbon black powder with a particle size of 20 μm, add 300 ml of the first mixed amino acid solution (hydroxyproline, histidine and purified water are mixed in a mass volume ratio of 3:2:8, where the unit corresponding to w / v is mg / ml) at a mass volume ratio of 1:3, heat to 70°C, and ultrasonically disperse at a power of 650 W for 20 min. Collect 400 mg of the liquid for use;

[0045] (2) Take 400 mg of the liquid in step (1), add 120 mg of the first mixed dispersant (hexadecyl phosphate monopotassium salt and sodium lignin sulfonate mixed in a mass ratio of 1:0.3), microwave treat for 12 min at a power of 400 W, the temperature of the liquid is 90 ° C, and grind for 25 min to obtain 520 mg of material for standby use;

[0046] (3) Take 520 mg of the material in step (2), add 1820 ml of the second mixed amino acid solution (pyroglutamic acid and arginine are mixed with purified water in a mass volume ratio of 3:2:9, where w / v corresponds to mg / ml) at a mass volume ratio of 1:3.5, heat to 98°C, and ultrasonically disperse at a power of 550 W for 30 min to obtain 2340 mg of the feed solution for use;

[0047] (4) Take 2340 mg of the liquid in step (3), add 702 mg of the second mixed dispersant (polar amide wax, fatty acid methyl ester polyoxyethylene ether and sodium dodecylbenzene sulfonate mixed in a mass ratio of 2:1:1.5) at a mass ratio of 1:0.3, microwave treat for 10 min at a power of 600 W, the material temperature is 110°C, grind for 20 min and then dry to obtain a highly dispersed carbon black product.

[0048] In order to better prove that the carbon black obtained by the process of the present invention has good dispersibility, 17 comparative examples are given with reference to Example 3. The carbon black prepared in Examples 1-5 and Comparative Examples 1-17 are placed in normal temperature water for 65 days. The dispersion effect of the carbon black is specifically shown in the following content:

[0049] Comparative Example 1

[0050] The difference from Example 3 is that glycine is used instead of histidine in the first mixed amino acid solution in step (1), and the rest of the operations are the same.

[0051] Comparative Example 2

[0052] The difference from Example 3 is that fatty acid polyoxyethylene ester is used in the first mixed dispersant in step (2) instead of hexadecyl phosphate monopotassium salt, and the rest of the operations are the same.

[0053] Comparative Example 3

[0054] The difference from Example 3 is that microwave treatment is not used in step (2). Instead, hot steam is used to heat the liquid to 95° C. The remaining operations are the same.

[0055] Comparative Example 4

[0056] The difference from Example 3 is that tyrosine is used instead of arginine in the second mixed amino acid solution in step (3), and the remaining operations are the same.

[0057] Comparative Example 5

[0058] The difference from Example 3 is that the second mixed dispersant in step (4) does not contain polar amide wax, and the remaining operations are the same.

[0059] Comparative Example 6

[0060] The difference from Example 3 is that the second mixed dispersant in step (4) does not contain fatty acid methyl ester polyoxyethylene ether, and the remaining operations are the same.

[0061] Comparative Example 7

[0062] The difference from Example 3 is that the second mixed dispersant in step (4) does not contain sodium dodecylbenzenesulfonate, and the remaining operations are the same.

[0063] Comparative Example 8

[0064] The difference from Example 3 is that microwave treatment is not used in step (4). Instead, hot steam is used to heat the liquid to 105° C. The remaining operations are the same.

[0065] Comparative Example 9

[0066] The difference from Example 3 is that in step (2), the temperature of the liquid after microwave treatment is controlled at 75°C, and the other operations are the same.

[0067] Comparative Example 10

[0068] The difference from Example 3 is that in step (2), the temperature of the liquid after microwave treatment is controlled at 95° C., and the remaining operations are the same.

[0069] Comparative Example 11

[0070] The difference from Example 3 is that in step (4), the temperature of the liquid after microwave treatment is controlled at 95°C, and the other operations are the same.

[0071] Comparative Example 12

[0072] The difference from Example 3 is that in step (4), the temperature of the liquid after microwave treatment is controlled at 115° C., and the remaining operations are the same.

[0073] Comparative Example 13

[0074] The difference from Example 3 is that the grinding time in step (2) is controlled at 30 min, and the other operations are the same.

[0075] Comparative Example 14

[0076] The difference from Example 3 is that the grinding time in step (4) is controlled at 25 min, and the other operations are the same.

[0077] Comparative Example 15

[0078] The difference from Example 3 is that in step (2), the first mixed dispersant is added at a mass ratio of 1:0.5, and the rest of the operations are the same.

[0079] Comparative Example 16

[0080] The difference from Example 3 is that in step (4), the second mixed dispersant is added at a mass ratio of 1:0.5, and the remaining operations are the same.

[0081] Comparative Example 17

[0082] The difference from Example 3 is that the particle size of the carbon black powder in step (1) is 12 μm, and the remaining operations are the same.

[0083]

[0084] It can be found from the data in Table 1 that, by adopting the preparation process of the present invention, the dispersibility of the carbon black prepared in Example 3 is better than that in Example 1, Example 2, Example 4, Example 5 and Comparative Examples 1-17.

[0085] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A process for preparing highly dispersible carbon black, characterized in that: The preparation process comprises the following steps: (1) taking carbon black powder with a particle size of 15-20 μm, adding the first mixed amino acid solution, heating, ultrasonically dispersing, and collecting the liquid for use; the carbon black powder and the first mixed amino acid solution are mixed in a mass volume ratio of 1:2-3; the first mixed amino acid solution is a mixture of hydroxyproline, histidine and purified water in a mass volume ratio of 1-3:1-2:6-8; (2) taking the feed liquid in step (1), adding a first mixed dispersant, microwave-treating, grinding, and setting the obtained material aside; the feed liquid and the first mixed dispersant are added in a mass ratio of 1:0.1-0.3; the first mixed dispersant comprises hexadecyl monopotassium phosphate and sodium lignin sulfonate, and the hexadecyl monopotassium phosphate and sodium lignin sulfonate are mixed in a mass ratio of 1:1-2; (3) Take the material in step (2), add the second mixed amino acid solution, heat, and ultrasonically disperse, and the obtained liquid is used for standby; the material and the second mixed amino acid solution are mixed at a mass volume ratio of 1:2.5-3.5; the second mixed amino acid solution is an aqueous solution of pyroglutamic acid and arginine, wherein the pyroglutamic acid and arginine are mixed with purified water at a mass volume ratio of 2-3:1-2:6-9; (4) Take the feed liquid in step (3), add a second mixed dispersant, microwave treat, grind, and dry to obtain a highly dispersible carbon black product; the feed liquid and the second mixed dispersant are mixed in a mass ratio of 1:0.1-0.3; the second mixed dispersant is polar amide wax, fatty acid methyl ester polyoxyethylene ether and sodium dodecylbenzene sulfonate, and the polar amide wax, fatty acid methyl ester polyoxyethylene ether and sodium dodecylbenzene sulfonate are mixed in a mass ratio of 1-2:1:0.5-1.

5.

2. The process for preparing a highly dispersible carbon black according to claim 1, characterized in that: In step (1), the mixture is heated to 60-70°C and ultrasonically dispersed at a power of 550-650W for 10-20min.

3. The process for preparing highly dispersible carbon black according to claim 1, characterized in that: In step (2), microwave treatment is performed at a power of 300-400 W for 5-12 min, and grinding is performed when the temperature of the feed liquid reaches 80-90° C.

4. The process for preparing highly dispersible carbon black according to claim 1, characterized in that: The grinding time in step (2) is 15-25 minutes.

5. The process for preparing highly dispersible carbon black according to claim 1, characterized in that: In step (3), the mixture is heated to 92-98°C and ultrasonically dispersed at a power of 450-550W for 20-30 minutes.

6. The process for preparing highly dispersible carbon black according to claim 1, characterized in that: In step (4), microwave treatment is performed at a power of 500-600 W for 5-10 min, and grinding is performed when the temperature of the feed liquid reaches 100-110° C.

7. The process for preparing highly dispersible carbon black according to claim 1, characterized in that: The grinding time in step (4) is 10-20 min.

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