CN119264705B - A preparation process of highly dispersed antibacterial carbon black - Google Patents
A preparation process of highly dispersed antibacterial carbon black Download PDFInfo
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Abstract
本发明涉及炭黑技术领域，尤其涉及一种高分散性抗菌炭黑的制备工艺，包括以下内容：将炭黑经过研磨处理后加入第一混合氨基酸溶液，加热、超声分散、干燥得到改性后的炭黑物料，然后再加入混合抗菌剂料液和表面活性剂，加热、超声处理，得到的料液中再键入壳聚糖溶液，经过超声处理，浓缩、干燥得到具有抗菌性能的炭黑；然后再将加入第二混合氨基酸溶液，经过加热、超声分散处理后，对炭黑进一步改性，然后再加入混合分散剂，加热、研磨、干燥，得到高分散性的抗菌炭黑。上述工艺设计合理，大大提高了炭黑的分散性和防霉效果。The present invention relates to the technical field of carbon black, and in particular to a preparation process of highly dispersible antibacterial carbon black, comprising the following contents: grinding carbon black and adding a first mixed amino acid solution, heating, ultrasonic dispersion, and drying to obtain a modified carbon black material, then adding a mixed antibacterial agent liquid and a surfactant, heating, ultrasonic treatment, and then typing a chitosan solution into the obtained liquid, ultrasonic treatment, concentrating, and drying to obtain carbon black with antibacterial properties; then adding a second mixed amino acid solution, heating, ultrasonic dispersion treatment, further modifying the carbon black, and then adding a mixed dispersant, heating, grinding, and drying to obtain highly dispersible antibacterial carbon black. The above process design is reasonable, which greatly improves the dispersibility and mildew-proof effect of carbon black.
Description
Technical Field
The invention relates to the technical field of carbon black, in particular to a preparation process of high-dispersity antibacterial carbon black.
Background
Carbon black is the product of incomplete combustion or cracking of hydrocarbons, the main component of which is carbon, and quasi-crystalline structures of nearly graphite, nearly spherical colloidal particles or aggregates of particles and particles fused together, can be observed with an electron microscope.
The fields of application of carbon black include rubber industry, ink and paint industry, plastics industry, electronics industry, braking materials, and other fields. Wherein carbon black is added in the paint industry to play roles in coloring, reinforcing, ultraviolet resistance and the like. However, the problems of adsorption between particles, unstable storage performance, flocculation of carbon black after a long time, granular feel, color fading, and color shading are caused by the electrostatic action between carbon black particles and strong aggregation among carbon black particles, other harmful bacteria such as mold are easy to grow in the paint under a humid environment, the growth of the harmful bacteria such as mold is inhibited by adding a mold inhibitor into the paint at present, and the performance of the paint is affected by the addition of the mold inhibitor although the problem of the harmful bacteria is solved to a certain extent, and the formed mold-resistant bacteria layer becomes a new pollution source. Therefore, in view of the above problems, it is necessary to develop a process for preparing highly dispersible antibacterial carbon black.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation process of high-dispersity antibacterial carbon black, and the preparation process can be used for obtaining the high-dispersity antibacterial carbon black.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a preparation process of high-dispersibility antibacterial carbon black, which comprises the following steps:
(1) Adding a first mixed amino acid solution into carbon black powder obtained by grinding a carbon black material, and heating and performing ultrasonic dispersion to obtain carbon black slurry for later use;
(2) Adding the carbon black slurry obtained in the step (1) into a mixed antibacterial agent solution and a surfactant, and heating and carrying out ultrasonic treatment on the mixture to collect feed liquid for later use;
(3) Taking the feed liquid in the step (2), adding chitosan solution, stirring and mixing, and performing ultrasonic treatment to obtain a material for later use;
(4) Taking the material in the step (3), adding a second mixed amino acid solution, and heating and ultrasonically dispersing the material liquid for later use;
(5) And (3) adding a mixed dispersing agent into the feed liquid obtained in the step (4), heating, grinding and drying to obtain the high-dispersivity antibacterial carbon black product.
As an improved technical scheme, in the step (1), the fineness of the carbon black powder is smaller than 12 mu m, the carbon black powder and the first mixed amino acid solution are mixed according to the mass-volume ratio of 1:3-4, and the first mixed amino acid solution is mixed according to the mass-volume ratio of 1-2:1-1.5:6-8 by aspartic acid, glutamic acid and purified water.
As an improved technical scheme, heating to 48-56 ℃ in the step (1), wherein the power of ultrasonic dispersion is 420-480w, and the dispersion time is 20-30min.
As an improved technical scheme, in the step (2), the carbon black slurry and the mixed antibacterial agent solution are mixed according to the mass ratio of 1:0.2-0.5, wherein the mixed antibacterial agent solution is prepared by mixing nano zinc, graphene oxide, 4, 5-dichloro-N-octyl-4-isothiazolin-3-one and ethanol according to the mass volume ratio of 1-3:0.5-1:1-2:10-15.
As an improved technical scheme, heating is carried out to 60-75 ℃ in the step (2), the power of ultrasonic treatment is 400-500w, and the treatment time is 30-40min.
As an improved technical scheme, the surfactant in the step (2) is formed by mixing sodium dodecyl benzene sulfonate and sodium lauroyl sarcosinate according to the mass ratio of 1:1, and the addition amount of the surfactant is 0.3-0.5% of the weight of the carbon black slurry.
As an improved technical scheme, the adding amount of the chitosan solution in the step (3) is 0.2-0.5% of the weight of the feed liquid, the concentration of the chitosan solution is 0.5-0.8% by weight, the chitosan solution is prepared from chitosan with the molecular weight of 10kD and acetic acid with the weight of 0.5-1% by weight, the power of ultrasonic treatment is 300-360w, and the treatment time is 10-20min.
As an improved technical scheme, the adding amount of the second mixed amino acid solution in the step (4) is 20-30% of the weight of the material, and the second mixed amino acid solution is an aqueous solution of aspartic acid and threonine, wherein the aspartic acid and threonine are mixed with purified water according to a mass-volume ratio of 1-2:1-1.5:5-8.
As an improved technical scheme, the ultrasonic dispersing treatment is carried out at the power of 480-560w and the dispersing time of 20-30min after heating to 45-55 ℃ in the step (4).
As an improved technical scheme, in the step (5), the feed liquid and the mixed dispersing agent are mixed according to the mass ratio of 1:0.2-0.5, the mixed dispersing agent comprises polyurethane dispersing agent HT-163 and polyurethane dispersing agent-F440, the polyurethane dispersing agent HT-163 and the polyurethane dispersing agent-F440 are mixed according to the mass ratio of 1-2:1, the heating temperature is 90-105 ℃, and the grinding time is 20-30min.
After the technical scheme is adopted, the invention has the beneficial effects that:
The invention comprises the steps of grinding carbon black, adding a first mixed amino acid solution, heating, ultrasonic dispersing and drying to obtain a modified carbon black material, adding a mixed antibacterial agent solution and a surfactant, heating, ultrasonic treating, typing a chitosan solution into the obtained feed liquid, ultrasonic treating, concentrating and drying to obtain carbon black with antibacterial property, adding a second mixed amino acid solution, heating, ultrasonic dispersing, further modifying the carbon black, adding a mixed dispersing agent, heating, grinding and drying to obtain the high-dispersity antibacterial carbon black. The process is reasonable in design, and the surface of the carbon black is modified, and the mixed antibacterial material liquid adsorption layer, the chitosan solution adsorption layer and the mixed dispersing agent adsorption layer are wrapped, so that agglomeration among carbon black particles is avoided, and the dispersibility and mildew-proof effect of the carbon black are greatly improved.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
A preparation process of high-dispersibility antibacterial carbon black comprises the following steps:
(1) Grinding carbon black materials to obtain 200mg of carbon black powder with the fineness of 10 mu m, adding 600ml of first mixed amino acid solution (aspartic acid, glutamic acid and purified water are mixed according to the mass-volume ratio of 1:1:6, wherein the corresponding units of w/v are mg/ml), heating to 48 ℃, and performing ultrasonic dispersion for 20min under the power of 420w to obtain 800mg of carbon black slurry for later use;
(2) Taking 800mg of carbon black slurry in the step (1), adding 2.4mg of mixed antibacterial agent solution (nano zinc, graphene oxide, 4, 5-dichloro-N-octyl-4-isothiazolin-3-one and ethanol are mixed according to the mass volume ratio of 1:0.5:1:10, wherein the corresponding unit of w/v is mg/ml), heating to 60 ℃ and performing ultrasonic treatment for 30min under the power of 400w, and adding 962.4mg of collected feed liquid for standby, wherein the weight of the surfactant (which is formed by mixing sodium dodecyl benzene sulfonate and sodium lauroyl sarcosine according to the mass ratio of 1:1) is 0.3% of the weight of the carbon black slurry;
(3) Taking 962.4mg of the feed liquid in the step (2), adding 1.9mg of chitosan solution (prepared from chitosan with the molecular weight of 10kD and acetic acid with the concentration of 0.5 wt%) with the weight of 0.2% of the feed liquid, stirring and mixing, and performing ultrasonic treatment for 10min under the power of 300w to obtain 964.3mg of the material for later use;
(4) Taking 964.3mg of the material in the step (3), adding 192.9mg of a second mixed amino acid solution (the mixture of aspartic acid and threonine and purified water according to the mass volume ratio of 1:1:5) accounting for 20% of the weight of the material, heating to 45 ℃, and performing ultrasonic dispersion for 20min under 480w power to obtain 1157.2mg of feed liquid for later use;
(5) And (3) taking 1157.2mg of the feed liquid in the step (4), adding a mixed dispersing agent (polyurethane dispersing agent HT-163 and polyurethane dispersing agent F440 are mixed according to the mass ratio of 1:1) according to the mass ratio of 1:0.2, heating to 90 ℃, grinding for 20min, and drying to obtain the high-dispersity antibacterial carbon black product.
Example 2
A preparation process of high-dispersibility antibacterial carbon black comprises the following steps:
(1) Grinding carbon black materials to obtain 200g of carbon black powder with fineness of 8 mu m, adding 640ml of first mixed amino acid solution (mixing aspartic acid, glutamic acid and purified water according to the mass-volume ratio of 1.2:1:6.5) according to the mass-volume ratio of 1:3.2, heating to 50 ℃, performing ultrasonic dispersion for 22min under 435w power, and drying to obtain 840mg of carbon black slurry for later use;
(2) Taking 840mg of carbon black slurry in the step (1), adding 252mg of mixed antibacterial agent solution (mixed by nano zinc, graphene oxide, 4, 5-dichloro-N-octyl-4-isothiazolin-3-one and ethanol according to the mass volume ratio of 1.5:0.8:1.2:11) according to the mass ratio of 1:0.3, adding surfactant (mixed by sodium dodecyl benzene sulfonate and sodium lauroyl sarcosine according to the mass ratio of 1:1) accounting for 0.35% of the weight of the carbon black slurry, heating to 65 ℃, and carrying out ultrasonic treatment for 32min under the power of 420w, wherein the collected feed liquid is 1094.94mg for standby;
(3) Taking 1094.94mg of the feed liquid in the step (2), adding 3.28mg of chitosan solution (prepared from chitosan with the molecular weight of 10kD and acetic acid with the concentration of 0.6wt% by weight of the feed liquid), stirring and mixing, and performing ultrasonic treatment for 12min under the power of 315w to obtain 1098.2mg of the material for later use;
(4) Taking 1098.2mg of the material in the step (3), adding 252.6mg of a second mixed amino acid solution (the mixture of aspartic acid and threonine and purified water according to the mass volume ratio of 1.2:1.3:6) accounting for 23% of the weight of the material, heating to 48 ℃, and performing ultrasonic dispersion for 22min at 500w to obtain 1350.8mg of material liquid for later use;
(5) And (3) taking 1350.8mg of the feed liquid in the step (4), adding a mixed dispersing agent (mixing polyurethane dispersing agent HT-163 and polyurethane dispersing agent F440 according to the mass ratio of 1.2:1) according to the mass ratio of 1:0.3, heating to 95 ℃, grinding for 23min, and drying to obtain the high-dispersity antibacterial carbon black product.
Example 3
A preparation process of high-dispersibility antibacterial carbon black comprises the following steps:
(1) Grinding carbon black materials to obtain 200g of carbon black powder with fineness of 5 mu m, adding 700ml of first mixed amino acid solution (mixing aspartic acid, glutamic acid and purified water according to the mass-volume ratio of 1.5:1.3:7) according to the mass-volume ratio of 1:3.5, heating to 52 ℃, performing ultrasonic dispersion for 25min under the power of 450w, and drying to obtain 900mg of carbon black slurry for later use;
(2) Taking 900mg of carbon black slurry in the step (1), adding 3.6mg of mixed antibacterial agent solution (mixed by nano zinc, graphene oxide, 4, 5-dichloro-N-octyl-4-isothiazolin-3-one and ethanol according to the mass volume ratio of 2:0.8:1.5:13) according to the mass ratio of 1:0.4, adding surfactant (mixed by sodium dodecyl benzene sulfonate and sodium lauroyl sarcosine according to the mass ratio of 1:1) accounting for 0.4% of the weight of the carbon black slurry, heating to 70 ℃, carrying out ultrasonic treatment for 35min under the power of 450w, and collecting 1263.6mg of feed liquid for standby;
(3) Taking 1263.6mg of the feed liquid in the step (2), adding 5.1mg of a chitosan solution (prepared from chitosan with a molecular weight of 10kD and acetic acid with a concentration of 0.8 wt%) with a weight of 0.4% and a concentration of 0.8wt% of the feed liquid, stirring and mixing, and performing ultrasonic treatment for 15min under a power of 330w to obtain 1268.7mg of the material for later use;
(4) Taking 1268.7mg of the material in the step (3), adding 317.2mg of a second mixed amino acid solution (the mixture of aspartic acid and threonine and purified water according to the mass volume ratio of 1.5:1.3:7) accounting for 25% of the weight of the material, heating to 50 ℃, and performing ultrasonic dispersion for 25min under 520w power to obtain 1585.9mg of material liquid for later use;
(5) And (3) taking 1585.9mg of the feed liquid in the step (4), adding a mixed dispersing agent (mixing polyurethane dispersing agent HT-163 and polyurethane dispersing agent F440 according to the mass ratio of 1.5:1) according to the mass ratio of 1:0.4, heating to 98 ℃, grinding for 25min, and drying to obtain the high-dispersity antibacterial carbon black product.
Example 4
A preparation process of high-dispersibility antibacterial carbon black comprises the following steps:
(1) Grinding carbon black materials to obtain 200g of carbon black powder with fineness of 5 mu m, adding 760ml of first mixed amino acid solution (mixing aspartic acid, glutamic acid and purified water according to the mass-volume ratio of 1.8:1.5:7.5) according to the mass-volume ratio of 1:3.8, heating to 54 ℃, and performing ultrasonic dispersion for 28min under 465w power to obtain 960mg of carbon black slurry for later use;
(2) Taking 960mg of carbon black slurry in the step (1), adding 384mg of mixed antibacterial agent solution (mixed by nano zinc, graphene oxide, 4, 5-dichloro-N-octyl-4-isothiazolin-3-ketone and ethanol according to the mass volume ratio of 2.5:1:1.8:15) according to the mass ratio of 1:0.4, adding 0.45% of surfactant (mixed by sodium dodecyl benzene sulfonate and sodium lauroyl sarcosine according to the mass ratio of 1:1) according to the weight ratio of 4.32mg of the carbon black slurry, heating to 72 ℃, carrying out ultrasonic treatment for 38min under 480w, and collecting 1348.3mg of feed liquid for standby;
(3) Taking 1348.3mg of the feed liquid in the step (2), adding 5.4mg of a chitosan solution (prepared from chitosan with a molecular weight of 10kD and acetic acid with a concentration of 0.6wt% by weight) with the weight of 0.4% of the feed liquid, stirring and mixing, and performing ultrasonic treatment for 18min under 345w power to obtain 1353.7mg of the material for later use;
(4) Taking 1353.7mg of the material in the step (3), adding 379mg of a second mixed amino acid solution (the mixture of aspartic acid and threonine and purified water according to the mass volume ratio of 1.8:1.3:8) accounting for 28% of the weight of the material, heating to 52 ℃, and performing ultrasonic dispersion for 28min under the power of 540w to obtain 1732.7mg of material liquid for later use;
(5) And (3) taking 1732.7mg of the feed liquid in the step (4), adding a mixed dispersing agent (mixing polyurethane dispersing agent HT-163 and polyurethane dispersing agent F440 according to the mass ratio of 1.8:1) according to the mass ratio of 1:0.4, heating to 102 ℃, grinding for 28min, and drying to obtain the high-dispersity antibacterial carbon black product.
Example 5
A preparation process of high-dispersibility antibacterial carbon black comprises the following steps:
(1) Grinding carbon black materials to obtain 200g of carbon black powder with fineness of 5 mu m, adding 800ml of first mixed amino acid solution (the mixture of aspartic acid, glutamic acid and purified water according to the mass-volume ratio of 2:1.5:8) according to the mass-volume ratio of 1:4, heating to 55 ℃, and performing ultrasonic dispersion for 30min under 480w power to obtain 1000mg of carbon black slurry for later use;
(2) Taking 1000mg of carbon black slurry in the step (1), adding 5mg of mixed antibacterial agent solution (mixed by nano zinc, graphene oxide, 4, 5-dichloro-N-octyl-4-isothiazolin-3-ketone and ethanol according to the mass volume ratio of 3:1:2:15) according to the mass ratio of 1:0.5, adding surfactant (mixed by sodium dodecyl benzene sulfonate and sodium lauroyl sarcosine according to the mass ratio of 1:1) accounting for 0.5% of the weight of the carbon black slurry, heating to 75 ℃, carrying out ultrasonic treatment for 40min under the power of 500w, and collecting 1505mg of feed liquid for standby;
(3) Taking 1505mg of the feed liquid in the step (2), adding 7.5mg of chitosan solution (prepared from chitosan with the molecular weight of 10kD and acetic acid with the concentration of 0.8wt% by weight of the feed liquid), stirring and mixing, and performing ultrasonic treatment for 20min under the power of 360w to obtain 1512.5mg of material for later use;
(4) Taking 1512.5mg of the material in the step (3), adding 453.8mg of a second mixed amino acid solution (the mixture of aspartic acid and threonine and purified water according to the mass volume ratio of 2:1.5:8) accounting for 30% of the weight of the material, heating to 55 ℃, and performing ultrasonic dispersion for 30min under 560w power to obtain 1966.3mg of feed liquid for later use;
(5) And (3) taking 1966.3mg of the feed liquid in the step (4), adding a mixed dispersing agent (polyurethane dispersing agent HT-163 and polyurethane dispersing agent F440 are mixed according to the mass ratio of 2:1) according to the mass ratio of 1:0.5, heating to 105 ℃, grinding for 30min, and drying to obtain the high-dispersity antibacterial carbon black product.
In order to better prove that the carbon black obtained by the process method has better dispersibility and antibacterial effect, 15 comparative examples are given by taking example 3 as a reference, and the specific details are as follows;
Performance testing
Investigation of the dispersing Effect:
the carbon blacks prepared in examples 1 to 5 and comparative examples 1 to 15 were placed in warm water for 60 days, and the dispersion effect of the carbon black was observed, and the details are shown in Table 1;
examination of antibacterial Properties:
The carbon black products prepared in examples 1 to 5 and comparative examples 1 to 15 were subjected to E.coli, staphylococcus aureus and Aspergillus niger tests, 0.5g of the prepared carbon black products were respectively selected and placed in a sterilizing test tube, a detection solution diluted to 0.0001% was added, after 5 minutes of ultrasonic waves, an equivalent bacterial solution with a concentration of 0.0008% was added, and the mixture was thoroughly mixed, the E.coli and Staphylococcus aureus tests were placed in a 37+ -1 ℃ medium for 24 hours, and the Aspergillus niger tests were placed in a 30+ -1 ℃ medium for 120 hours ("-" represents the increase of aseptic colonies and "+" represents the increase of bacterial colonies), and the details are shown in Table 1.
Comparative example 1
Unlike example 3, the carbon black powder was treated with nitric acid in step (1), and the rest was the same.
Comparative example 2
Unlike example 3, the temperature in step (1) was 45 ℃, and the rest was the same.
Comparative example 3
In contrast to example 3, L-serine was used instead of aspartic acid in step (1), and the rest was the same.
Comparative example 4
Unlike example 3, no surfactant was added in step (2), and the rest was the same.
Comparative example 5
Unlike example 3, the mixed antimicrobial solution in step (2) does not contain graphene oxide, and the rest of the operations are the same.
Comparative example 6
Unlike example 3, the mixed antimicrobial solution in step (2) does not contain 4, 5-dichloro-N-octyl-4-isothiazolin-3-one, and the rest is the same.
Comparative example 7
Unlike example 3, the surfactant in step (2) does not contain sodium lauroyl sarcosinate, and the rest of the procedure is the same.
Comparative example 8
Unlike example 3, the heating to 55 ℃ in step (2) was performed in the same manner.
Comparative example 9
Unlike example 3, step (3) was absent and the rest was the same.
Comparative example 10
Unlike example 3, tyrosine was substituted for aspartic acid in step (4), and the rest was the same.
Comparative example 11
Unlike example 3, step (4) was heated to 40 ℃, the remainder of the procedure being identical.
Comparative example 12
Unlike example 3, the chitosan solution was added in an amount of 1% by weight of the feed solution in step (3), and the rest was the same.
Comparative example 13
Unlike example 3, the mixed dispersant in step (5) does not contain polyurethane dispersant-F440, and the rest is the same.
Comparative example 14
Unlike example 3, the heating to 85 ℃ in step (5) was performed in the same manner as the rest.
Comparative example 15
Grinding the carbon black material to obtain carbon black powder with fineness of 5 μm, and performing no other treatment.
As can be seen from the data in Table 1, the carbon black products prepared in example 3 were significantly better in dispersibility than those prepared in example 1, example 2, example 4, example 5 and comparative examples 1-15 using the preparation process of the present invention. The carbon black product prepared in example 3 was also superior in antibacterial properties to comparative example 1, comparative examples 4 to 9, and comparative example 15.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
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| CN118772666A (en) * | 2024-06-13 | 2024-10-15 | 安徽黑猫新材料有限公司 | A kind of high dispersibility carbon black and preparation method thereof |
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