CN113956686B - Carbon black dispersion and preparation method and application thereof - Google Patents

Carbon black dispersion and preparation method and application thereof Download PDF

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CN113956686B
CN113956686B CN202111322381.1A CN202111322381A CN113956686B CN 113956686 B CN113956686 B CN 113956686B CN 202111322381 A CN202111322381 A CN 202111322381A CN 113956686 B CN113956686 B CN 113956686B
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carbon black
surfactant
parts
polyester
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CN113956686A (en
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杜长森
徐利伟
梁栋
陈爽
冯淑芹
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Suzhou Sunmun Technology Co ltd
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    • 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
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
    • C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
    • 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
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/04—Pigments
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters

Abstract

The invention discloses a carbon black dispersion and a preparation method thereof, wherein the carbon black dispersion comprises the following components in parts by mass: 10-40 parts of modified carbon black, 2-5 parts of surfactant A, 2-5 parts of surfactant B, 40-90 parts of liquid dispersion medium and 0-0.1 part of additive; wherein the modified carbon black is prepared by esterification reaction of a modified substance C and carbon black with hydroxyl on the surface. The invention also provides an application of the carbon black dispersoid in the coloring of the stock solution of the polyester fiber, which comprises the following specific steps: preheating the carbon black dispersion to 170-180 ℃, and adding the carbon black dispersion into the polyester oligomer after esterification and before polycondensation in the production process of the polyester fiber. The carbon black dispersoid has good compatibility with polyester, can be stably dispersed in the polyester, can improve the spinnability of the colored polyester fiber, and ensures that the polyester fiber has higher elongation at break and breaking strength, higher soaping color fastness and dry/wet rubbing fastness.

Description

Carbon black dispersion and preparation method and application thereof
Technical Field
The invention belongs to the technical field of fine chemical engineering, and particularly relates to a carbon black dispersion, a preparation method thereof and application of the carbon black dispersion in coloring of a polyester fiber stock solution.
Background
Chemical fiber is a fiber with textile properties, which is prepared by taking natural or artificially synthesized macromolecular compounds as raw materials and carrying out the working procedures of spinning solution preparation, spinning, post-treatment and the like, and is widely applied to various aspects of people's clothing and housing. Chemical fibers are classified into rayon and synthetic fibers according to the raw materials. According to the statistics of the chemical fiber industry association in China, the yield of chemical fibers in China in 2019 is 5827 ten thousand tons, the yield of synthetic fibers is 5279 ten thousand tons, the yield of polyester fibers in the synthetic fibers is 4781 ten thousand tons, and the polyester fibers account for 90 percent of the yield of the synthetic fibers.
When the polyester fiber is dyed by adopting a dye dyeing mode, because the molecular arrangement in the polyester fiber is linear straight chain, the crystallinity is high, the orientation is good, the intermolecular gap is small, polar functional groups such as hydroxyl, amino and the like are not arranged on a macromolecular chain, only ester groups with smaller polarity are arranged, the dye is not easy to permeate, and the dyeing property is poorer. Dye molecules can enter the fiber for dyeing only under the conditions of high temperature and high pressure. The traditional dyeing process adopting the dye has the problems of high equipment requirement, high energy consumption, large wastewater discharge amount and the like. The stock solution coloring is a process of directly spinning colored fibers by adding a coloring agent before fiber spinning; the stock solution coloring process omits the subsequent dyeing procedure, reduces the three wastes pollution and huge energy consumption generated by the processes of dyeing, cleaning and the like, is beneficial to promoting the energy conservation and emission reduction in the fiber production process, and has good development prospect.
The most common way of coloring the polyester fiber stock solution is to color the polyester fiber by using the color master batch, and compared with the color master batch, the method has the advantages of smaller particle size distribution of pigment particles in the fiber, higher tinting strength and the like by using the liquid colorant to color the polyester fiber stock solution. The preparation and application research of the liquid colorant for coloring the stock solution of the polyester fiber is one of the research hotspots for coloring the polyester fiber. The coloring of fiber stock solutions requires that the pigment be uniformly, stably and highly dispersed in a dispersion carrier, and that the pigment dispersion have good dispersibility, color strength, chemical and physical resistance, strong fastness and the like. If the pigment has poor dispersibility, the problems of blockage of spinneret orifices, broken ends, defects and the like are easy to occur in the spinning process, and the mechanical strength of the fiber is influenced; on the other hand, the mechanical and physical properties of the fiber can be affected by adding a large amount of pigment, so that in order to maintain the original excellent properties of the fiber, the less pigment is required to be added, the better the fiber is, the pigment is required to have higher coloring strength, and the color requirement can be met only by adding a small amount of pigment; in addition, the components of the pigment dispersion also need to meet the requirements of no chemical change in the polyester reaction stage and no change in physical properties at the polycondensation temperature; for colored polyester fibers, pigments are also required to have good light fastness, abrasion resistance, washing resistance and the like.
The prior art discloses various colorants for dope-coloring polyester fibers, such as a colorant for polyester fibers disclosed in U.S. Pat. No. US5106905, which disperses pigments/dyes in liquid aliphatic polyesters for direct use in dope-coloring polyester fibers; chinese patent publication No. CN103031755A discloses a glycol-based pigment dispersion for coloring a polyester dope and a preparation method thereof, wherein the glycol-based pigment dispersion is composed of a pigment, a wetting agent, a dispersing agent and ethylene glycol; chinese patent publication No. CN106978639A discloses a liquid colorant for coloring a polyester fiber dope, which is composed of a liquid dispersion medium, a colorant, a dispersant, and the like, wherein the liquid dispersion medium is a mixture of two types of substances of mineral oil and aliphatic polyester, and a preparation method thereof.
Polyester fibers can be classified into black, white and colored according to color; in recent years, the demand of black polyester fibers is increasing, and the black colorant for the polyester fibers is a key field of the industrial research on the stock solution coloring of the polyester fibers; for example, Chinese patent with publication number CN110903611A discloses a super-black large-melting-index high-dispersibility black master batch special for direct-spun fine denier yarns, which is composed of 25-30 parts of extra-black carbon black, 74-67 parts of polyester carrier and 1-3 parts of dispersing agent, wherein the dispersing agent is a composite aliphatic polar auxiliary agent with low melting point, strong permeability and good fluidity; chinese patent publication No. CN101338067A discloses a black polyester chip and a method for preparing the black polyester chip, wherein carbon black color paste is added before esterification or ester exchange reaction, wherein the carbon black color paste comprises carbon black, ethylene glycol, cosolvent (ethanol and/or water), and nonylphenol polyethylene glycol ether dispersant.
The carbon black mainly comprises carbon which forms irregular aromatic condensed rings and contains a small amount of components such as hydrogen, oxygen, sulfur and the like on the surface. Generally, the smaller the particle size of carbon black, the stronger the coloring power and the blackness; however, the smaller the particle diameter, the larger the specific surface area and the higher the surface energy, the more easily the carbon black powder is agglomerated, and the more difficult the dispersion is, and therefore, it is necessary to improve the dispersibility by surface modification of the carbon black. Chinese patent No. CN104499079B discloses a method for preparing black polyester fiber by dope dyeing, black slurry is obtained by adding black pigment carbon black into liquid dispersion medium, grinding fully, adding compound capable of chemically reacting with carbon black surface group, and grafting reaction under certain temperature and catalyst, wherein the liquid dispersion medium is water. U.S. Pat. No. 4,487,9335 discloses a liquid colorant of carbon black and a process for producing a polyester fiber, wherein carbon black is subjected to oxidation treatment with a peroxide, neutralization with an alkali, filtration drying, and kneading with a liquid dispersion medium (e.g., a liquid polyester) to obtain a liquid colorant which can be used for a polyester fiber.
Furthermore, in the prior art, the carbon black dispersion is generally added to the polyester oligomer directly before polycondensation after esterification without preheating during application; the temperature of the polyester oligomer is generally above 210 ℃, and due to large temperature difference, the phenomena of instant volatilization of ethylene glycol and agglomeration of carbon black particles are easy to occur when the carbon black dispersion is added, so that the phenomena of poor spinnability, low fiber tinting strength and the like of the prepared polyester occur in the spinning process, and the prepared colored polyester fiber has poor fastness to washing and rubbing.
Disclosure of Invention
In order to solve the above technical problems, the present invention aims to provide a carbon black dispersion, a method for producing the same, and use thereof; the carbon black dispersoid has good compatibility with polyester, can be stably dispersed in the polyester, can improve the spinnability of the colored polyester fiber, and ensures that the polyester fiber has higher elongation at break and breaking strength, higher soaping color fastness and dry/wet rubbing fastness.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
a carbon black dispersion comprises the following components in parts by mass: 10-40 parts of modified carbon black, 2-5 parts of surfactant A, 2-5 parts of surfactant B, 40-90 parts of liquid dispersion medium and 0-0.1 part of additive; wherein the modified carbon black is prepared by esterification reaction of a modified substance C and carbon black with hydroxyl on the surface.
Preferably, the surfactant A is modified lignin.
Furthermore, the modified lignin is prepared by modifying lignin by epichlorohydrin and diethanolamine. The specific preparation process can be as follows: dissolving lignin with 30% sodium hydroxide water solution, adding epichlorohydrin, and reacting at 76 deg.C for 3-4 h; and adding diethanolamine, and reacting at 145 ℃ for 8h under the protection of nitrogen to obtain the modified lignin. Benzene rings in the lignin and condensed rings of the carbon black can enable the lignin to be adsorbed on the surface of the carbon black through a conjugation effect; the modification of the lignin by the epichlorohydrin and the diethanolamine can improve the stability of the carbon black in the polyester.
Further, the surfactant B is a surfactant containing a phosphate ester structure; the surfactant B has a structure shown in a general formula (I):
Figure BDA0003345766590000051
wherein n is an integer between 6 and 30, and comprises 6 and 30; m1And M2Independently of one another are H or CH3；R1And R2Independently of one another, H, K, Na, NH4Or a quaternary ammonium salt.
Further, the surfactant B is at least one of 2,4, 6-tri (1-methyl-1-phenylethyl) phenol polyoxyethylene ether phosphate or 2,4, 6-tri (1-phenylethyl) phenol polyoxyethylene ether phosphate.
Further, the structure of the modifying substance C contains 1 carboxyl, 1 benzene ring and at least 1 hydroxyl.
Furthermore, the modifying substance C is at least one of p-hydroxybenzoic acid, o-hydroxybenzoic acid, m-hydroxybenzoic acid, 2, 3-dihydroxybenzoic acid, 3, 5-dihydroxybenzoic acid, 2, 6-dihydroxybenzoic acid, 3,4, 5-trihydroxybenzoic acid and 2,4, 6-trihydroxybenzoic acid.
Further, the liquid dispersion medium is ethylene glycol.
Among them, there are many methods for carbon black having hydroxyl groups on the surface thereof or for increasing the hydroxyl group content on the surface of carbon black, and for example, the method can be obtained by: adding carbon black into 65% nitric acid, reacting for 12h at 100 ℃, and washing with water to obtain oxidized carbon black; then adding the oxidized carbon black into thionyl chloride, reacting for 12 hours at 70 ℃, and removing the thionyl chloride by suction filtration to obtain carbon black subjected to acyl chlorination; adding carbon black subjected to acyl chlorination into ethylene glycol, reacting for 12h at 120 ℃, filtering, washing and drying to obtain the carbon black with hydroxyl on the surface.
The specific preparation method of the modified carbon black comprises the following steps: adding carbon black with hydroxyl on the surface and a modified substance C in a mass ratio of 1 (0.05-0.08), adding N, N-dimethylformamide accounting for 10-20% of the mass of the carbon black with hydroxyl on the surface, uniformly dispersing, and kneading for 30-60 min by using a kneading machine to obtain the modified carbon black. The carboxyl of the modified substance C and the hydroxyl on the surface of the carbon black are subjected to esterification reaction; the hydroxyl group of the modifying substance C and the carboxyl group of another molecule of the modifying substance C undergo an esterification reaction, and therefore, a plurality of benzoate bonds are formed on the surface of the carbon black. The modified carbon black has good compatibility with polyester, and can be stably dispersed in the polyester under the action of the surfactant A and the surfactant B.
The invention further provides a preparation method of the carbon black dispersoid, which comprises the following steps: dispersing a surfactant A and a surfactant B in a liquid dispersion medium, adding modified carbon black, selectively adding an additive according to a formula, fully mixing to obtain a carbon black pre-dispersion body, and then dispersing, grinding, filtering and defoaming to obtain the carbon black dispersion body.
According to actual needs, various functional additives such as a pH value regulator and an antibacterial agent can be selectively added into the carbon black dispersion, wherein the pH value regulator is mainly used for regulating the pH value of the carbon black pre-dispersion obtained after the modified carbon black is added to be 7-9, and the pH value regulator is preferably at least one of sodium hydroxide, potassium hydroxide and triethanolamine. Although glycol solvents have a certain bacteriostatic effect, in order to minimize the risk of mildew during long-term storage of the carbon black dispersion, common antibacterial agents such as 1, 2-benzisothiazolin-3-one can be optionally added during the preparation of the carbon black dispersion disclosed by the present invention.
The invention further provides an application of the carbon black dispersoid in the coloring of the stock solution of the polyester fiber, which comprises the following specific steps: preheating the carbon black dispersion to 170-180 ℃, and adding the carbon black dispersion into the polyester oligomer after esterification and before polycondensation in the production process of the polyester fiber.
The invention has the beneficial effects that:
(1) the surfactant A is modified lignin, and the benzene ring in the lignin and the condensed ring of the carbon black enable the lignin to be adsorbed on the surface of the carbon black through a conjugation effect, so that the lignin is not easy to desorb; the modified lignin obtained by modifying the lignin by epoxy chloropropane and diethanol amine is adsorbed on the surface of the carbon black, so that the stability of the carbon black in the polyester can be improved; in addition, the lignin is a natural surfactant, is cheap and easy to obtain, and can reduce the production cost;
(2) the dispersion stability of the carbon black in the carbon black dispersion and the dispersion stability of the carbon black in the polyester are further improved by compounding the surfactant A and the surfactant B.
(3) The modified substance C is grafted to the carbon black with hydroxyl on the surface through esterification reaction, so that the surface of the modified carbon black contains a benzoate structure; the benzoate structure is similar to that of polyester, and the compatibility of carbon black and polyester is improved.
(4) The melt direct spinning colored polyester fiber is generally prepared by directly spinning raw materials such as polybasic acid, polyhydric alcohol and the like after esterification and polycondensation reaction. The pigment dispersion is generally added directly during the spinning process after esterification and before polycondensation, without preheating the pigment dispersion. The temperature of the esterified polyester oligomer is higher, generally higher than 210 ℃, and the phenomena of instant volatilization of glycol and agglomeration of carbon black particles are easy to occur when the carbon black dispersoid is added due to larger temperature difference; according to the invention, the carbon black dispersion is heated to 170-180 ℃, and then added into the polyester oligomer, so that the temperature difference between the preheated carbon black dispersion and the polyester oligomer is small, the phenomena of instant volatilization of ethylene glycol and agglomeration of carbon black particles are avoided, and the occurrence of material flushing is avoided.
(5) The carbon black dispersoid has small particle size and good storage stability, the filter pressing value of the black polyester chip prepared by the carbon black dispersoid is low, the spinnability is good, and the prepared black polyester fiber has higher fiber elongation at break and breaking strength, higher soaping resistance color fastness and dry/wet rubbing fastness.
Detailed Description
The technical solutions in the present invention will be described clearly and completely with reference to specific embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The surfactant B used in the invention has a structure shown in a general formula (I):
Figure BDA0003345766590000081
in the following examples, the surfactants B1, B2, B3 and B4 all have the structures represented by the general formula (I) above; in the surfactant B1, n is 6, M1Is H, M2Is CH3，R1And R2Are all H; in the surfactant B2, n is 30, M1And M2Are all CH3，R1And R2Are all Na; in the surfactant B3, n is 20, M1And M2Are all CH3，R1And R2Are all NH4(ii) a In the surfactant B4, n is 15, M1Is H, M2Is CH3，R1And R2Are all H.
Surfactant a in the following examples is modified lignin; the modified lignin is prepared by modifying lignin by epichlorohydrin and diethanolamine. The specific preparation process comprises the following steps: dissolving lignin with 30% sodium hydroxide water solution, adding epichlorohydrin, and reacting at 76 deg.C for 3-4 h; and adding diethanol amine, and reacting at 145 ℃ for 8h under the protection of nitrogen to obtain the modified lignin.
Example 1
Adding carbon black with hydroxyl on the surface and p-hydroxybenzoic acid in a mass ratio of 1:0.05, adding N, N-dimethylformamide accounting for 15% of the mass of the carbon black with hydroxyl on the surface, uniformly dispersing, and kneading for 45min by using a kneading machine to obtain modified carbon black;
dispersing 3 parts by mass of a surfactant A and 3 parts by mass of a surfactant B1 in 74 parts by mass of ethylene glycol, adding 20 parts by mass of modified carbon black, fully mixing, adjusting the pH value to 8.0 by using sodium hydroxide, dispersing, grinding, filtering and defoaming to obtain a carbon black dispersion.
Example 2
Adding carbon black with hydroxyl on the surface and m-hydroxybenzoic acid in a mass ratio of 1:0.06, adding N, N-dimethylformamide accounting for 10% of the mass of the carbon black with hydroxyl on the surface, uniformly dispersing, and kneading for 30min by using a kneading machine to obtain modified carbon black;
dispersing 2 parts by mass of a surfactant A and 5 parts by mass of a surfactant B2 in 63 parts by mass of ethylene glycol, adding 30 parts by mass of modified carbon black, fully mixing, adjusting the pH value to 7.0 by using potassium hydroxide, dispersing, grinding, filtering and defoaming to obtain a carbon black dispersion.
Example 3
Adding carbon black containing hydroxyl on the surface and 3, 5-dihydroxybenzoic acid in a mass ratio of 1:0.07, adding N, N-dimethylformamide accounting for 16% of the mass of the carbon black containing hydroxyl on the surface, uniformly dispersing, and kneading by a kneader for 40min to obtain the modified carbon black.
Dispersing 5 parts by mass of a surfactant A and 4 parts by mass of a surfactant B3 into 51 parts by mass of ethylene glycol, adding 40 parts by mass of modified carbon black and 0.01 part by mass of 1, 2-benzisothiazolin-3-one, fully mixing, adjusting the pH value to 9.0 by using potassium hydroxide, and dispersing, grinding, filtering and defoaming to obtain a carbon black dispersion.
Example 4
Adding carbon black containing hydroxyl on the surface and 3,4, 5-trihydroxybenzoic acid in a mass ratio of 1:0.08, adding N, N-dimethylformamide accounting for 20% of the mass of the carbon black containing hydroxyl on the surface, uniformly dispersing, and kneading for 60min by using a kneading machine to obtain the modified carbon black.
Dispersing 4 parts by mass of a surfactant A and 2 parts by mass of a surfactant B4 in 84 parts by mass of ethylene glycol, adding 10 parts by mass of modified carbon black, fully mixing, adjusting the pH value to 8.5 by using triethanolamine, and dispersing, grinding, filtering and defoaming to obtain a carbon black dispersion.
Comparative example 1 (carbon Black is not modified compared with example 1)
Dispersing 3 parts by mass of a surfactant A and 3 parts by mass of a surfactant B1 in 74 parts by mass of ethylene glycol, adding 20 parts by mass of carbon black, fully mixing, adjusting the pH value to 8.0 with sodium hydroxide, dispersing, grinding, filtering and defoaming to obtain a carbon black dispersion.
Comparative example 2 (comparison with example 1, without addition of surfactant A)
Adding carbon black with hydroxyl on the surface and p-hydroxybenzoic acid in a mass ratio of 1:0.05, adding N, N-dimethylformamide accounting for 15% of the mass of the carbon black with hydroxyl on the surface, uniformly dispersing, and kneading for 45min by using a kneading machine to obtain the modified carbon black.
Dispersing 6 parts by mass of surfactant B1 in 74 parts by mass of ethylene glycol, adding 20 parts by mass of modified carbon black, mixing thoroughly, adjusting pH to 8.0 with sodium hydroxide, dispersing, grinding, filtering, and defoaming to obtain a carbon black dispersion.
Comparative example 3 (comparison with example 1, replacement of surfactant A with nonylphenol polyoxyethylene ether)
Adding carbon black with hydroxyl on the surface and p-hydroxybenzoic acid in a mass ratio of 1:0.05, adding N, N-dimethylformamide accounting for 15% of the mass of the carbon black with hydroxyl on the surface, uniformly dispersing, and kneading for 45min by using a kneading machine to obtain the modified carbon black.
Dispersing 3 parts by mass of nonylphenol polyoxyethylene ether and 3 parts by mass of surfactant B1 into 74 parts by mass of ethylene glycol, adding 20 parts by mass of modified carbon black, fully mixing, adjusting the pH value to 8.0 by using sodium hydroxide, dispersing, grinding, filtering and defoaming to obtain the carbon black dispersion.
Comparative example 4 (comparison with example 1, without addition of surfactant B1)
Adding carbon black containing hydroxyl on the surface and p-hydroxybenzoic acid in a mass ratio of 1:0.05, adding N, N-dimethylformamide accounting for 15% of the mass of the carbon black containing hydroxyl on the surface, uniformly dispersing, and kneading for 45min by a kneader to obtain the modified carbon black.
Dispersing 6 parts by mass of surfactant A into 74 parts by mass of ethylene glycol, adding 20 parts by mass of modified carbon black, fully mixing, adjusting the pH value to 8.0 by using sodium hydroxide, and dispersing, grinding, filtering and defoaming to obtain a carbon black dispersion.
Comparative example 5 (comparison with example 1, replacement of surfactant B1 with nonylphenol polyoxyethylene ether)
Adding carbon black with hydroxyl on the surface and p-hydroxybenzoic acid in a mass ratio of 1:0.05, adding N, N-dimethylformamide accounting for 15% of the mass of the carbon black with hydroxyl on the surface, uniformly dispersing, and kneading for 45min by using a kneading machine to obtain the modified carbon black.
Dispersing 3 parts by mass of surfactant A and 3 parts by mass of nonylphenol polyoxyethylene ether into 74 parts by mass of ethylene glycol, adding 20 parts by mass of modified carbon black, fully mixing, adjusting the pH value to 8.0 by using sodium hydroxide, dispersing, grinding, filtering and defoaming to obtain the carbon black dispersion.
Comparative example 6 (comparing with example 1, only nonylphenol polyoxyethylene ether is used)
Adding carbon black containing hydroxyl on the surface and p-hydroxybenzoic acid in a mass ratio of 1:0.05, adding N, N-dimethylformamide accounting for 15% of the mass of the carbon black containing hydroxyl on the surface, uniformly dispersing, and kneading for 45min by a kneader to obtain the modified carbon black.
Dispersing 6 parts by mass of nonylphenol polyoxyethylene ether into 74 parts by mass of ethylene glycol, adding 20 parts by mass of modified carbon black, fully mixing, adjusting the pH value to 8.0 by using sodium hydroxide, and dispersing, grinding, filtering and defoaming to obtain a carbon black dispersion.
Carbon Black Dispersion Performance test
Testing the particle size distribution: the particle size distributions of the carbon black dispersions prepared in examples 1 to 4 and comparative examples 1 to 6 were measured by Zetasizer Nano ZS90 model, Malvern instruments Ltd, UK, and the results of the measurement were that D50 represents the minimum particle size at which 50% of the particles in the granules tested can pass, D90 represents the minimum particle size at which 90% of the particles in the granules tested can pass, and D50 and D90 represent the particle size distributions.
And (4) testing the storage stability: after 10 carbon black dispersions prepared in examples 1 to 4 and comparative examples 1 to 6 were placed in a closed state at 25 ℃ for 180 days, the presence or absence of significant precipitation, flocculation and the like of carbon black, which seriously affect the stability, was visually observed. "√" indicates that no carbon black precipitation, flocculation or the like is found; ". o" indicates visible precipitation, flocculation of carbon black, but needs to be observed carefully to be found; "X" indicates that precipitation and flocculation of the carbon black were clearly observed.
And (3) testing the filter pressing value: preheating the 10 carbon black dispersions prepared in the examples 1-4 and the comparative examples 1-6 to 170-180 ℃, and adding the carbon black dispersions into a polyester oligomer for uniformly mixing before polycondensation after esterification; wherein the mass of the carbon black accounts for 2% of that of the polyester oligomer, then carrying out polycondensation to obtain a black polyester chip, and testing the filter pressing value of the black polyester chip. The specific testing steps are as follows: firstly, 200g of polyester slices are extruded out of a filter pressing performance tester, and the balance pressure is recorded as the initial pressure P0Then 2000g of the prepared black polyester chip is extruded out of the filter pressing performance tester, 200g of the polyester chip is extruded out of the filter pressing performance tester, and the balance pressure is recorded as the termination pressure P1The filter pressing value DF (unit MPa cm) is calculated according to the formula (1)2/g)：
DF＝(P1-P0) S/M … … … … … … … … … … formula (1)
In equation (1): p1End pressure in MPa; p is0Initial pressure in MPa; s is filterArea of the net in cm2(ii) a M is the mass of pigment (carbon black) in g. In this experiment, S was 6.15cm2And M is 40 g.
Application Performance testing of carbon Black dispersions
10 black polyester chips were spun at 275 ℃ and 285 ℃ at a take-up speed of 4500m/min to obtain black polyester Fully Drawn Yarns (FDY) of 75D/72F, which were woven into a welt and subjected to the following tests:
soaping color fastness test: the soaping color fastness of the 10 kinds of the socks is tested according to GB/T3921-2008 soaping color fastness of textile color fastness test.
Color fastness to rubbing test: according to GB/T3920-.
Fiber dry breaking strength and elongation at break test: according to GB/T14344-.
The results of the above performance tests are shown in table 1.
TABLE 1
Figure BDA0003345766590000141
As can be seen from the test results of the carbon black dispersions of examples 1 to 4 and comparative examples 1 to 6, the carbon black dispersions prepared in the examples have small particle size and good storage stability, the black polyester chips prepared from the carbon black dispersions have low filter pressing value and good spinnability, and the prepared black polyester fibers have higher fiber elongation at break and breaking strength and higher soaping color fastness and dry/wet rubbing fastness. The test result shows that the carbon black dispersoid prepared by carrying out surface modification on the carbon black and using two surfactants with special structures has good compatibility with the polyester and can be stably dispersed in the polyester.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.

Claims (6)

1. The carbon black dispersion is characterized by comprising the following components in parts by mass: 10-40 parts of modified carbon black, 2-5 parts of surfactant A, 2-5 parts of surfactant B, 40-90 parts of liquid dispersion medium and 0-0.1 part of additive; wherein the modified carbon black is prepared by esterification reaction of a modified substance C and carbon black with hydroxyl on the surface;
the surfactant A is modified lignin; the modified lignin is prepared by modifying lignin by epichlorohydrin and diethanolamine;
the surfactant B is a surfactant containing a phosphate ester structure; the surfactant B has a structure shown in a general formula (I):
Figure DEST_PATH_IMAGE001
（Ⅰ）
wherein n is an integer between 6 and 30, and comprises 6 and 30; m1And M2Independently of one another, H or CH3；R1And R2Independently of one another, H, K, Na, NH4Or a quaternary ammonium salt;
the structure of the modifying substance C contains 1 carboxyl, 1 benzene ring and at least 1 hydroxyl.
2. The carbon black dispersion according to claim 1, characterized in that: the surfactant B is at least one of 2,4, 6-tri (1-methyl-1-phenylethyl) phenol polyoxyethylene ether phosphate or 2,4, 6-tri (1-phenylethyl) phenol polyoxyethylene ether phosphate.
3. The carbon black dispersion according to claim 1, characterized in that: the modified substance C is at least one of p-hydroxybenzoic acid, o-hydroxybenzoic acid, m-hydroxybenzoic acid, 2, 3-dihydroxybenzoic acid, 3, 5-dihydroxybenzoic acid, 2, 6-dihydroxybenzoic acid, 3,4, 5-trihydroxybenzoic acid and 2,4, 6-trihydroxybenzoic acid.
4. The carbon black dispersion according to claim 1, characterized in that: the liquid dispersion medium is ethylene glycol.
5. A method for producing the carbon black dispersion as described in any one of claims 1 to 4, characterized in that: dispersing a surfactant A and a surfactant B in a liquid dispersion medium, adding modified carbon black, selectively adding an additive according to a formula, fully mixing to obtain a carbon black pre-dispersion body, and then dispersing, grinding, filtering and defoaming to obtain the carbon black dispersion body.
6. Use of the carbon black dispersion according to any one of claims 1 to 4 for the coloration of a stock solution of polyester fibers, characterized in that: preheating the carbon black dispersion to 170-180 ℃, and adding the carbon black dispersion into the polyester oligomer after esterification and before polycondensation in the production process of the polyester fiber.
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