CN115852716B - Aramid fiber dyeing method adopting biological enzyme pretreatment - Google Patents
Aramid fiber dyeing method adopting biological enzyme pretreatment Download PDFInfo
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Abstract
The invention relates to an aramid fiber dyeing method of biological enzyme pretreatment, which comprises the steps of firstly pretreating aramid fiber and then dyeing the pretreated aramid fiber; the pretreatment adopts biological enzyme and allyl glycidyl ether monomer, and the biological enzyme activates benzene rings in the aramid fiber to form free radical I in the pretreatment process, and the free radical I and the allyl glycidyl ether monomer undergo free radical active polymerization. The dyeing method is efficient and practical, and has mild and environment-friendly conditions; the aramid fiber dyed by the method has good color fastness, level dyeing degree and bright color.
Description
Technical Field
The invention belongs to the technical field of aramid fiber textile production, and relates to an environment-friendly aramid fiber dyeing method with biological enzyme pretreatment.
Background
The aramid fiber is prepared by polycondensation and spinning of aromatic compounds serving as raw materials, is a rigid molecule, has high molecular symmetry, crystallinity and glass transition temperature, and has excellent performances such as high specific strength, high specific modulus and fatigue resistance, so that the aramid fiber is widely applied to the fields of aerospace, sports goods, rubber industry and the like.
The structural characteristics of the aramid fiber make the dyeing very difficult, and the dyeing is difficult by adopting a conventional dyeing method, specifically because: (1) the molecular chain of the aramid fiber contains benzene rings, the benzene rings separate amide groups on the molecular structure and form pi conjugated effect with the amide groups, and the internal rotation energy is very high; (2) the covalent bond forming the main chain of the aramid fiber is very large, the molecular chain links are in a planar rigid linear extending conformation, polyamide molecules are stacked in parallel through the hydrogen bond connection with medium strength between the chains to form flaky microcrystals, and the hydrogen bond planes enable the flaky microcrystals to form liquid crystals under the action of shearing and stretching flow, so that the fiber axially generates crystallization and orientation, and therefore, the aramid fiber has higher strength and crystallinity; (3) the macromolecules are arranged in parallel, the intermolecular gaps are smaller, the interaction force is stronger, and the molecules contain more polar groups, so that the modulus is higher.
At present, three dyeing methods are generally adopted for aramid fiber: hot melt dyeing, high temperature and high pressure dyeing and carrier dyeing.
The hot melt dyeing method can realize continuous production, and has high dyeing production efficiency, low water consumption and less sewage. However, there are several drawbacks, such as: certain condition limitations are imposed on the dyes used, such as high sublimation fastness requirements on the dyes used; the dyed fabric has poor hand feeling and color brightness due to the fact that the fabric is stressed greatly during dyeing; high dyeing temperatures need to be provided, and therefore energy consumption is great; the occupied area of the equipment is large; the dye utilization is low.
The high-temperature high-pressure dyeing method is suitable for low-temperature dye varieties with low sublimation fastness and small molecular weight, the dye has good level dyeing property, bright color, good hand feeling and high fabric core penetration degree, is suitable for small-batch and multi-variety production, is commonly used for dyeing polyester-cotton blended fabrics, and is suitable for dyeing deep and dense color. However, the pH value is generally controlled to be 5-6 during dyeing, high pressure and high temperature are required to be maintained, acetic acid and monoammonium phosphate are commonly used for adjusting the pH value, and in addition, dispersing agents and high-temperature leveling agents are required to be added for keeping the dye bath stable during dyeing.
The carrier dyeing method is a low-temperature dyeing method which adds carrier auxiliary agent into the dye bath to ensure that the disperse dye has higher dye uptake and adsorption capacity under the condition of about 100 ℃ at normal pressure. However, the dyeing effect of the aramid fiber is still to be further improved.
The aramid fiber is modified before dyeing, so that the dyeing effect of the aramid fiber can be improved. The dyeing process [ J ]. Dyeing and finishing of aramid 1414 yarns, 2011, (19): 28-32.) adopts an acid (15 g/L phosphoric acid) and alkali (8 g/L sodium hydroxide) modification method to pretreat the aramid, and the fiber is dyed by selecting proper dye, fiber modification method and dyeing method, discussing the influence of modification condition, dye type and dosage, dye bath pH value, dyeing temperature, dyeing time and the like on dyeing performance, and finding that the breaking strength and breaking elongation of the pretreated aramid are obviously reduced, thereby greatly limiting the application of the method and not being applicable to practical production; document 2 (a method for modifying, dyeing and multifunctional composite finishing of aramid fibers: china, 101570940[ P ] 2009-11-04.). Before dyeing the aramid fibers, the cleaned fibers are placed in a reaction chamber of a plasma generator for treatment, and dyeing performance, ultraviolet aging resistance and moisture absorption and ventilation of the dyed fibers are all enhanced compared with those of untreated fibers, but the operation flow is complicated.
An enzyme is a biocatalyst that changes only the reaction rate without changing the direction and equilibrium point of the reaction and does not change after the reaction. The enzyme has the advantages of high selectivity, mild reaction condition, high catalytic efficiency and the like, and the enzyme catalytic reaction has attractive application prospect in various fields, especially in high and new industries. At present, the biological enzyme is used for preprocessing the high polymer synthetic fiber and is applied to the field of aramid fiber dyeing.
In summary, various aramid fiber dyeing methods have various advantages due to the structural characteristics of the aramid fiber, but various disadvantages exist, such as dyeing the aramid fiber by a biological enzyme pretreatment method, which is expected to make up for the defects of the prior art.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a biological enzyme pretreatment aramid fiber dyeing method, which can obviously improve the dyeing effect of aramid fiber by simply treating the aramid fiber.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the aramid fiber dyeing method with biological enzyme pretreatment includes the steps of firstly, pretreating aramid fiber, and then dyeing the pretreated aramid fiber; the pretreatment adopts biological enzyme and allyl glycidyl ether monomer, and the biological enzyme activates benzene rings in the aramid fiber to form free radicals I in the pretreatment process, and the free radicals I and the allyl glycidyl ether monomer undergo free radical active polymerization;
in the aspect of material pretreatment, the biological enzyme pretreatment has the advantages of mild reaction conditions, high catalytic efficiency and the like, so that the biological enzyme pretreatment can effectively modify the aramid fiber with surface hydrophobicity, and the problems caused by other modification methods in the modification of the aramid fiber are avoided; the method has mild process conditions, low energy consumption and small influence on the usability of the material, and is an environment-friendly pretreatment technology;
in addition to the aspects of maintaining structural performance and improving dyeing performance of the aramid fiber, the method disclosed by the invention also introduces the combination innovation points in the field of dyeing the aramid fiber by using a mild method such as biological enzyme, and compared with the previous research work, the research focus of dyeing the aramid fiber is more concentrated on a hot melt dyeing method, a high-temperature high-pressure dyeing method and a carrier dyeing method, and the defects of the existing known dyeing method of the aramid fiber are overcome by using the biological enzyme pretreatment dyeing method of the aramid fiber, so that the application of the method in the aspect of environment-friendly dyeing method of the aramid fiber is more important and urgent.
As a preferable technical scheme:
the aramid fiber dyeing method for the biological enzyme pretreatment comprises the step of carrying out pretreatment on the aramid fiber by using a biological enzyme, wherein the biological enzyme is horseradish peroxidase, bovine liver catalase or xanthine peroxidase.
According to the aramid fiber dyeing method for biological enzyme pretreatment, hydrogen peroxide is also adopted for pretreatment, benzene rings in the aramid fiber are activated by the hydrogen peroxide in the pretreatment process to form free radicals II, and the free radicals II and allyl glycidyl ether monomers undergo free radical active polymerization.
The aramid fiber dyeing method pretreated by biological enzyme comprises the following specific steps:
(1) Cleaning aramid fiber;
(2) Adding the cleaned aramid fiber, biological enzyme and allyl glycidyl ether monomer into phosphate buffer solution, and then degassing;
(3) Dropwise adding hydrogen peroxide solution into the system in the step (2);
(4) Heating the system of the step (3) to obtain pretreated aramid fibers;
(5) Dyeing the pretreated aramid fiber.
In the aramid fiber dyeing method for biological enzyme pretreatment, in the step (1), the aramid fiber is para-aramid fiber, meta-aramid fiber or heterocyclic aramid fiber, and the average breaking strength of monofilaments of the aramid fiber is 35-50 cN; the cleaning process comprises the following steps: and cleaning the aramid fiber with acetone, petroleum ether and deionized water respectively, and drying.
According to the aramid fiber dyeing method with the biological enzyme pretreatment, in the step (2), the concentration of the phosphate buffer solution is 0.067-0.20 mol/L, and the pH value is 6.4-7.6.
According to the aramid fiber dyeing method with the biological enzyme pretreatment, in the step (3), the volume fraction of the hydrogen peroxide solution is 20% -30%, and the dripping rate is 10-20 mL/h; after the dripping is finished, the molar ratio of the hydrogen peroxide, the allyl glycidyl ether monomer and the biological enzyme in the system in the step (3) is 100-200:50-80:1, and the mass ratio of the aramid fiber to the allyl glycidyl ether monomer is 100-1000:1.
According to the aramid fiber dyeing method with the biological enzyme pretreatment, in the step (4), the heating temperature is 35-50 ℃, the time is 20-30 h, and the grafting rate of the allyl glycidyl ether monomer of the pretreated aramid fiber is 40-70%.
In the above-mentioned aramid fiber dyeing method pretreated by biological enzyme, in the step (5), the dyeing process is as follows: placing the pretreated aramid fiber into a dispersion type dyeing carrier at 40-60 ℃, then gradually adding a dyeing agent and a dyeing auxiliary agent into a dye bath, dyeing for 45-75 min under the conditions of 0.1MPa, 4.5-6 pH and 110-130 ℃, finally taking out, cleaning and drying; wherein the mass ratio of the aramid fiber to the disperse type dyeing carrier to the dyeing agent to the dyeing auxiliary is 50-200:1:2-5:1-3.
According to the aramid fiber dyeing method with the biological enzyme pretreatment, the disperse dyeing carrier is dimethyl terephthalate, methyl salicylate and carbonic acid acrylic ester, which are all ester compounds, and the aramid fiber dyeing method is nontoxic, easy to decompose, easy to remove and free from influence on the environment; the dyeing agent is disperse brilliant red SF-B, disperse yellow G or disperse deep blue HGL; the dyeing auxiliary is dyeing auxiliary A-N, dyeing auxiliary P and dyeing auxiliary PNS.
According to the aramid fiber dyeing method with the biological enzyme pretreatment, the soap solution with the concentration of 1-3 g/L is used for cleaning at the temperature of 45-60 ℃, and the aramid fiber is dried in vacuum at the temperature of 105-120 ℃ for 10-15 h after cleaning.
According to the aramid fiber dyeing method with the biological enzyme pretreatment, the dyeing rate of the dyed aramid fiber is 90% -100%, the soaping-resistant color fastness is 4-5 levels, and the soaping-resistant color fading fastness is 4-5 levels.
The principle of the invention is as follows:
the invention enhances the dyeability and color fastness of the aramid fiber by pretreating the aramid fiber, and the main reasons are as follows:
dyeability promotes: after the biological enzyme and benzene rings in the hydrogen peroxide activated aramid fiber form free radicals, the free radicals and allyl glycidyl ether monomers undergo free radical active polymerization, so that the active functional groups are modified on the surface of the aramid fiber, the types of the active functional groups on the surface of the aramid fiber are changed (from hydrogen atoms to hydroxyl groups), meanwhile, the active functional groups and the surface roughness of the aramid fiber are increased after the aramid fiber is treated by the biological enzyme, the whole crystallinity of the aramid fiber is reduced due to the change of the active functional groups, the contact angle of the aramid fiber to deionized water and ethylene glycol is reduced due to the increase of the number of the active functional groups and the surface roughness, and the free energy of the surface of the aramid fiber is increased, so that the bonding performance of the surface of the aramid fiber and dye molecules is improved, hydrogen bonds among the aramid fiber macromolecules can be damaged to a certain extent, the Van der Waals force among the aramid molecules is reduced, and dye entering the inside the fiber is facilitated, and the dye dyeing rate is improved.
And (3) improving color fastness: on one hand, functional groups such as hydroxyl groups on the surface of the aramid fiber and dye molecules form strong intermolecular interactions such as hydrogen bonds, so that the binding force of the aramid fiber and dye molecules is increased; on the other hand, as the surface roughness of the aramid fiber is improved, the overall crystallinity of the aramid fiber is reduced, dye molecules are easier to enter an amorphous region of the aramid fiber, and the attachment degree of the dye molecules is improved, so that the method improves the dyeing color fastness of the aramid fiber.
In addition, due to the high selectivity of the biological enzyme, the molecular structure of the aramid polymer is not damaged, the internal crystal structure of the treated aramid fiber, namely, the highly-straightened rigid chain conformation, the high crystallinity and the highly-ordered microfiber structure are maintained, and the mechanical property of the fiber is not affected.
Advantageous effects
(1) The aramid fiber dyeing method pretreated by biological enzyme has the characteristics of environmental friendliness, simplicity in operation, less raw material use and the like, and can cause pollution to the environment;
(2) According to the aramid fiber dyeing method for biological enzyme pretreatment, the aramid fiber has high dye-uptake, high soaping-resistant color fastness after dyeing and good leveling property;
(3) The aramid fiber dyeing method of biological enzyme pretreatment provided by the invention avoids the problems of high crystallization and high orientation of an aramid fiber structure, and the biological enzyme pretreatment method is utilized to activate the surface of the aramid fiber without affecting the mechanical properties of the fiber.
Detailed Description
The invention is further described below in conjunction with the detailed description. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Further, it is understood that various changes and modifications may be made by those skilled in the art after reading the teachings of the present invention, and such equivalents are intended to fall within the scope of the claims appended hereto.
The manufacturers and brands of the related substances in the following examples are as follows:
horseradish peroxidase: the brand is AMRESCO, and the product number is 0417-100000U;
bovine liver catalase: brand PERFEMIKER, cat# PM11586;
xanthine peroxidase: the brand is Gentishold, and the product number is X1189;
disperse brilliant red SF-B: the manufacturer is Zhejiang leap soil stock limited company;
disperse yellow G: the manufacturer is Hubei Xinming Tai chemical;
disperse deep blue HGL: the manufacturer is Hubei Heng Jing Rui chemical industry Co., ltd;
dyeing auxiliary A-N: the manufacturer is a common commercial Yuxi chemical Co., ltd;
dyeing auxiliary P: the manufacturer is Jiangsu Paishimei polymer new material Co., ltd;
dyeing assistant PNS: the manufacturer is Bo' an Mei Innovative technology Co., ltd;
acetone: analytically pure, manufacturer is national pharmaceutical group chemical reagent company, inc;
petroleum ether: boiling point is 60-90 ℃, and content is more than or equal to 95%; the manufacturer is a national medicine group chemical reagent company;
the test method of the correlation performance in each of the following examples is as follows:
the method for testing the mechanical properties of the aramid fiber comprises the following steps: measuring the linear density, the average breaking strength, the breaking strength and the breaking elongation of monofilaments of the aramid fiber before and after modification and before and after dyeing by using an XQ-1 type fiber fineness gauge and an XQ-1C type fiber strength gauge; in order to ensure the accuracy of the test result, each group of samples is measured for 30-50 times, and then the average value is taken as the experimental result.
The dyeing rate of an aramid fiber after dyeing is the ratio of the amount of dye dyed on the fiber to the total amount in the initial dyeing bath, generally expressed in percent, and is measured as follows:
respectively accurately measuring 2mL of dye liquor before dyeing and 7mL of dye liquor after dyeing, respectively transferring to 25mL volumetric flasks at 20 ℃ to dilute to scale, shaking uniformly, and standing to be measured; then, absorbance of the dye solution before and after dyeing was measured using a model 721 spectrophotometer, and the percentage of dye-uptake was calculated according to the formula: f (%) = (1-nA) 1 /mA 0 ) ×100%；
Wherein: f (%) -percent dye-uptake;
m-fold of dye liquor dilution before dyeing;
n-fold of dye liquor dilution after dyeing;
A 0 absorbance after m-fold dilution of the dye solution before dyeing;
A 1 absorbance after n-fold dilution of the dye solution after dyeing.
The method for testing the soaping and staining fastness and the soaping and fading fastness of the dyed aramid fiber comprises the following steps: according to GB/T3921-2008 "fastness to washing of textiles color fastness test"; stitching a suitable amount of the dyed fiber sample with a multicomponent backing fabric (SDC DW multi-fiber cloth, SDC inc., uk) to form a combined sample; then washing for 30min on an SW-12 type washing fastness tester under the conditions that the mass concentration of the soap solution is 5.0g/L, the bath ratio is 1:50 and the temperature is 40 ℃; taking out the combined sample after washing, washing the combined sample with flowing clean water, and naturally airing the combined sample at room temperature; finally, under the D65 light source, the fading sample card and the staining sample card are used for respectively grading the fading of the sample and the staining fastness of the lining fabric.
Example 1
A biological enzyme pretreatment aramid fiber dyeing method comprises the following specific steps:
(1) Preparing raw materials:
aramid fiber: a heterocyclic aramid fiber with an average breaking strength of 35cN, a linear density of 1.55dtex, an average breaking strength of 35cN, a breaking strength of 13cN/dtex and an elongation at break of 2.5%;
biological enzyme: xanthine peroxidase;
allyl glycidyl ether monomer;
hydrogen peroxide solution (water as solvent, the following are given): the volume fraction is 22%;
phosphate buffer: the concentration is 0.067mol/L, and the pH value is 6.4;
dyeing agent: disperse yellow G;
dyeing auxiliary: dyeing auxiliary A-N;
disperse dye carrier: a carbonic acid acrylic ester;
(2) Pretreatment of aramid fiber:
(2.1) respectively cleaning the aramid fiber with acetone, petroleum ether and deionized water, and drying;
(2.2) adding the cleaned aramid fiber, biological enzyme and allyl glycidyl ether monomer into phosphate buffer solution, and then degassing;
(2.3) dropwise adding hydrogen peroxide solution into the system in the step (2.2) at the dropwise adding rate of 10mL/h;
after the dripping is finished, the molar ratio of hydrogen peroxide, allyl glycidyl ether monomer and biological enzyme in the system is 124:50:1, and the mass ratio of aramid fiber to allyl glycidyl ether monomer is 100:1;
(2.4) heating the system of the step (2.3) for 30 hours at the temperature of 35 ℃ to obtain pretreated aramid fibers;
the grafting rate of the allyl glycidyl ether monomer of the pretreated aramid fiber is 40%, the linear density of the aramid fiber is 1.54dtex, the average breaking strength of monofilaments is 34cN, the breaking strength is 12.5cN/dtex, and the elongation at break is 2.4%;
(3) Dyeing the pretreated aramid fiber:
placing the pretreated aramid fiber into a dispersion type dyeing carrier at 40 ℃, gradually adding a dyeing agent and a dyeing auxiliary agent into a dye bath, dyeing for 75min under the conditions of 0.1MPa, 6 pH and 110 ℃, finally taking out, washing with a soap solution with the concentration of 1g/L at 48 ℃, and vacuum drying for 10h at 107 ℃ after washing, wherein the mass ratio of the aramid fiber, the dispersion type dyeing carrier, the dyeing agent and the dyeing auxiliary agent is 50:1:2:1;
the dyeing rate of the dyed aramid fiber is 90%, the soaping-resistant color fastness is 4 level, the soaping-resistant color fading fastness is 5 level, the linear density is 1.54dtex, the average breaking strength of monofilaments is 33cN, the breaking strength is 12.3cN/dtex, and the breaking elongation is 2.4%.
Comparative example 1
An aramid dyeing method is basically the same as in example 1, except that the aramid fiber is not pretreated.
The dyeing rate of the dyed aramid fiber is 50%, the soaping-resistant color fastness is 2 levels, and the soaping-resistant color fading fastness is 2 levels.
As can be seen by comparing example 1 with comparative example 1, other conditions are the same, the aramid fiber is not pretreated, the dyeing rate of the aramid fiber is low, and the soaping-resistant color fastness and the soaping-resistant color fading fastness are lower, because the pretreatment can enable the surface of the aramid fiber to form more active sites, the interaction with dye molecules is more sufficient, and the dyeing rate and the combination degree of the dye are improved.
Example 2
A biological enzyme pretreatment aramid fiber dyeing method comprises the following specific steps:
(1) Preparing raw materials:
aramid fiber: a heterocyclic aramid fiber with an average filament breaking strength of 37cN, a linear density of 1.64dtex, an average filament breaking strength of 37cN, a breaking strength of 13.5cN/dtex and an elongation at break of 2.7%;
biological enzyme: horseradish peroxidase;
allyl glycidyl ether monomer;
hydrogen peroxide solution: the volume fraction is 20%;
phosphate buffer: the concentration is 0.15mol/L, and the pH value is 7;
dyeing agent: disperse brilliant red SF-B;
dyeing auxiliary: dyeing auxiliary P;
disperse dye carrier: dimethyl terephthalate;
(2) Pretreatment of aramid fiber:
(2.1) respectively cleaning the aramid fiber with acetone, petroleum ether and deionized water, and drying;
(2.2) adding the cleaned aramid fiber, biological enzyme and allyl glycidyl ether monomer into phosphate buffer solution, and then degassing;
(2.3) dropwise adding hydrogen peroxide solution into the system in the step (2.2) at a dropwise adding rate of 12mL/h;
after the dripping is finished, the mole ratio of hydrogen peroxide, allyl glycidyl ether monomer and biological enzyme in the system is 134:55:1, and the mass ratio of aramid fiber to allyl glycidyl ether monomer is 200:1;
(2.4) heating the system in the step (2.3) for 27 hours at the temperature of 40 ℃ to obtain pretreated aramid fibers;
the grafting rate of the allyl glycidyl ether monomer of the pretreated aramid fiber is 45%, the linear density of the aramid fiber is 1.61dtex, the average breaking strength of monofilaments is 36.6cN, the breaking strength is 13.4cN/dtex, and the elongation at break is 2.6%;
(3) Dyeing the pretreated aramid fiber:
placing the pretreated aramid fiber into a dispersion type dyeing carrier at 40 ℃, gradually adding a dyeing agent and a dyeing auxiliary agent into a dye bath, dyeing for 75min under the conditions of 0.1MPa, 5.5 pH and 110 ℃, finally taking out, washing with a soap solution with the concentration of 1.5g/L at 45 ℃, and vacuum drying for 15h at 105 ℃, wherein the mass ratio of the aramid fiber to the dispersion type dyeing carrier to the dyeing agent to the dyeing auxiliary agent is 80:1:3:2;
the dyeing rate of the dyed aramid fiber is 92%, the soaping-resistant color-staining fastness is 5 level, the soaping-resistant color-fading fastness is 4 level, the linear density is 1.6dtex, the average breaking strength of monofilaments is 36.5cN, the breaking strength is 13.3cN/dtex, and the breaking elongation is 2.58%.
Example 3
A biological enzyme pretreatment aramid fiber dyeing method comprises the following specific steps:
(1) Preparing raw materials:
aramid fiber: meta-position aramid fiber with average breaking strength of 40cN, linear density of 1.73dtex, average breaking strength of 40cN, breaking strength of 14.5cN/dtex and elongation at break of 3.3%;
biological enzyme: bovine liver catalase;
allyl glycidyl ether monomer;
hydrogen peroxide solution: the volume fraction is 23%;
phosphate buffer: the concentration is 0.15mol/L, and the pH value is 7.6;
dyeing agent: disperse brilliant red SF-B;
dyeing auxiliary: dyeing auxiliary P;
disperse dye carrier: dimethyl terephthalate;
(2) Pretreatment of aramid fiber:
(2.1) respectively cleaning the aramid fiber with acetone, petroleum ether and deionized water, and drying;
(2.2) adding the cleaned aramid fiber, biological enzyme and allyl glycidyl ether monomer into phosphate buffer solution, and then degassing;
(2.3) dropwise adding hydrogen peroxide solution into the system in the step (2.2) at a dropwise adding rate of 15mL/h;
after the dripping is finished, the molar ratio of hydrogen peroxide, allyl glycidyl ether monomer and biological enzyme in the system is 130:60:1, and the mass ratio of aramid fiber to allyl glycidyl ether monomer is 350:1;
(2.4) heating the system in the step (2.3) at 40 ℃ for 25 hours to obtain pretreated aramid fibers;
the grafting rate of the allyl glycidyl ether monomer of the pretreated aramid fiber is 52 percent, the linear density of the aramid fiber is 1.72dtex, the average breaking strength of monofilaments is 39cN, the breaking strength is 14.3cN/dtex, and the elongation at break is 3.2 percent;
(3) Dyeing the pretreated aramid fiber:
placing the pretreated aramid fiber into a dispersion type dyeing carrier at 45 ℃, gradually adding a dyeing agent and a dyeing auxiliary agent into a dye bath, dyeing for 65min under the conditions of 0.1MPa, 5.5 pH and 120 ℃ temperature, finally taking out, washing with soap solution with the concentration of 2g/L at 46 ℃, and vacuum drying for 11h at 109 ℃ after washing, wherein the mass ratio of the aramid fiber, the dispersion type dyeing carrier, the dyeing agent and the dyeing auxiliary agent is 100:1:4:1;
the dyeing rate of the dyed aramid fiber is 94%, the soaping-resistant color-staining fastness is 4 levels, the soaping-resistant color-fading fastness is 5 levels, the linear density is 1.7dtex, the average breaking strength of monofilaments is 38.8cN, the breaking strength is 14.2cN/dtex, and the breaking elongation is 3.1%.
Example 4
A biological enzyme pretreatment aramid fiber dyeing method comprises the following specific steps:
(1) Preparing raw materials:
aramid fiber: meta-position aramid fiber with average breaking strength of 42cN, linear density of 1.88dtex, average breaking strength of 42cN, breaking strength of 15cN/dtex and elongation at break of 3.8%;
biological enzyme: horseradish peroxidase;
allyl glycidyl ether monomer;
hydrogen peroxide solution: the volume fraction is 25%;
phosphate buffer: the concentration is 0.067mol/L, and the pH value is 7;
dyeing agent: disperse yellow G;
dyeing auxiliary: dyeing auxiliary A-N;
disperse dye carrier: methyl salicylate;
(2) Pretreatment of aramid fiber:
(2.1) respectively cleaning the aramid fiber with acetone, petroleum ether and deionized water, and drying;
(2.2) adding the cleaned aramid fiber, biological enzyme and allyl glycidyl ether monomer into phosphate buffer solution, and then degassing;
(2.3) dropwise adding hydrogen peroxide solution into the system in the step (2.2) at a dropwise adding rate of 17mL/h;
after the dripping is finished, the mole ratio of hydrogen peroxide, allyl glycidyl ether monomer and biological enzyme in the system is 135:62:1, and the mass ratio of aramid fiber to allyl glycidyl ether monomer is 500:1;
(2.4) heating the system of the step (2.3) at 45 ℃ for 23 hours to obtain pretreated aramid fibers;
the grafting rate of the allyl glycidyl ether monomer of the pretreated aramid fiber is 55%, the linear density of the aramid fiber is 1.8dtex, the average breaking strength of monofilaments is 39.5cN, the breaking strength is 14.9cN/dtex, and the elongation at break is 3.5%;
(3) Dyeing the pretreated aramid fiber:
placing the pretreated aramid fiber into a dispersion type dyeing carrier at 55 ℃, then gradually adding a dyeing agent and a dyeing auxiliary agent into a dye bath, dyeing for 60min under the conditions of 0.1MPa, 5 pH and 120 ℃ temperature, finally taking out, cleaning with a soap solution with the concentration of 2.4g/L at 50 ℃, and vacuum drying for 12h at 112 ℃ after cleaning, wherein the mass ratio of the aramid fiber, the dispersion type dyeing carrier, the dyeing agent and the dyeing auxiliary agent is 120:1:4:3;
the dyeing rate of the dyed aramid fiber is 95%, the soaping-resistant color-staining fastness is 5 level, the soaping-resistant color-fading fastness is 4 level, the linear density is 1.72dtex, the average breaking strength of monofilaments is 38cN, the breaking strength is 16.1cN/dtex, and the breaking elongation is 3.2%.
Example 5
A biological enzyme pretreatment aramid fiber dyeing method comprises the following specific steps:
(1) Preparing raw materials:
aramid fiber: meta-position aramid fiber with average breaking strength of 45cN, linear density of 2.44dtex, average breaking strength of 45cN, breaking strength of 14.8cN/dtex and elongation at break of 4%;
biological enzyme: xanthine peroxidase;
allyl glycidyl ether monomer;
hydrogen peroxide solution: the volume fraction is 30%;
phosphate buffer: the concentration is 0.2mol/L, and the pH value is 6.4;
dyeing agent: dispersing deep blue HGL;
dyeing auxiliary: dyeing assistant PNS;
disperse dye carrier: methyl salicylate;
(2) Pretreatment of aramid fiber:
(2.1) respectively cleaning the aramid fiber with acetone, petroleum ether and deionized water, and drying;
(2.2) adding the cleaned aramid fiber, biological enzyme and allyl glycidyl ether monomer into phosphate buffer solution, and then degassing;
(2.3) dropwise adding hydrogen peroxide solution into the system in the step (2.2) at a dropwise adding rate of 19mL/h;
after the dripping is finished, the mole ratio of hydrogen peroxide, allyl glycidyl ether monomer and biological enzyme in the system is 150:65:1, and the mass ratio of aramid fiber to allyl glycidyl ether monomer is 750:1;
(2.4) heating the system of the step (2.3) at 45 ℃ for 22 hours to obtain pretreated aramid fibers;
the grafting rate of the allyl glycidyl ether monomer of the pretreated aramid fiber is 58%, the linear density of the aramid fiber is 2.4dtex, the average breaking strength of monofilaments is 44cN, the breaking strength is 14.5cN/dtex, and the elongation at break is 3.8%;
(3) Dyeing the pretreated aramid fiber:
placing the pretreated aramid fiber into a disperse type dyeing carrier at 60 ℃, gradually adding a dyeing agent and a dyeing auxiliary agent into a dye bath, dyeing for 50min under the conditions of 0.1MPa, 5 pH and 125 ℃ temperature, finally taking out, cleaning with a soap solution with the concentration of 2.7g/L at 60 ℃, and vacuum drying for 10h at 120 ℃ after cleaning, wherein the mass ratio of the aramid fiber, the disperse type dyeing carrier, the dyeing agent and the dyeing auxiliary agent is 150:1:2:2;
the dyeing rate of the dyed aramid fiber is 97%, the soaping-resistant color fastness is 5-grade, the soaping-resistant color fading fastness is 5-grade, the linear density is 2.3dtex, the average breaking strength of monofilaments is 43.5cN, the breaking strength is 14cN/dtex, and the breaking elongation is 3.7%.
Example 6
A biological enzyme pretreatment aramid fiber dyeing method comprises the following specific steps:
(1) Preparing raw materials:
aramid fiber: para-aramid fiber with average breaking strength of 49cN, linear density of 2.60dtex, average breaking strength of 49cN, breaking strength of 17cN/dtex and elongation at break of 4.3%;
biological enzyme: bovine liver catalase;
allyl glycidyl ether monomer;
hydrogen peroxide solution: the volume fraction is 28%;
phosphate buffer: the concentration is 0.2mol/L, and the pH value is 7.6;
dyeing agent: dispersing deep blue HGL;
dyeing auxiliary: dyeing assistant PNS;
disperse dye carrier: methyl salicylate;
(2) Pretreatment of aramid fiber:
(2.1) respectively cleaning the aramid fiber with acetone, petroleum ether and deionized water, and drying;
(2.2) adding the cleaned aramid fiber, biological enzyme and allyl glycidyl ether monomer into phosphate buffer solution, and then degassing;
(2.3) dropwise adding hydrogen peroxide solution into the system in the step (2.2) at a dropwise adding rate of 20mL/h;
after the dripping is finished, the molar ratio of hydrogen peroxide, allyl glycidyl ether monomer and biological enzyme in the system is 190:77:1, and the mass ratio of aramid fiber to allyl glycidyl ether monomer is 900:1;
(2.4) heating the system of the step (2.3) for 20 hours at 50 ℃ to obtain pretreated aramid fibers;
the grafting rate of the allyl glycidyl ether monomer of the pretreated aramid fiber is 65%, the linear density of the aramid fiber is 2.55dtex, the average breaking strength of monofilaments is 48cN, the breaking strength is 17.2cN/dtex, and the elongation at break is 4.2%;
(3) Dyeing the pretreated aramid fiber:
placing the pretreated aramid fiber into a disperse type dyeing carrier at 60 ℃, gradually adding a dyeing agent and a dyeing auxiliary agent into a dye bath, dyeing for 45min under the conditions of 0.1MPa, 4.5 pH and 130 ℃ temperature, finally taking out, cleaning with soap solution with the concentration of 3g/L at 55 ℃, and vacuum drying for 13h at 118 ℃ after cleaning, wherein the mass ratio of the aramid fiber, the disperse type dyeing carrier, the dyeing agent and the dyeing auxiliary agent is 175:1:2:2;
the dyeing rate of the dyed aramid fiber is 99%, the soaping-resistant color-staining fastness is 4 levels, the soaping-resistant color-fading fastness is 5 levels, the linear density is 2.5dtex, the average breaking strength of monofilaments is 45cN, the breaking strength is 17cN/dtex, and the breaking elongation is 4%.
Example 7
A biological enzyme pretreatment aramid fiber dyeing method comprises the following specific steps:
(1) Preparing raw materials:
aramid fiber: para-aramid fiber with average breaking strength of 50cN, linear density of 2.64dtex, average breaking strength of 50cN, breaking strength of 18cN/dtex and elongation at break of 4.5%;
biological enzyme: xanthine peroxidase;
allyl glycidyl ether monomer;
hydrogen peroxide solution: the volume fraction is 29%;
phosphate buffer: the concentration is 0.2mol/L, and the pH value is 6.4;
dyeing agent: disperse yellow G;
dyeing auxiliary: dyeing auxiliary A-N;
disperse dye carrier: a carbonic acid acrylic ester;
(2) Pretreatment of aramid fiber:
(2.1) respectively cleaning the aramid fiber with acetone, petroleum ether and deionized water, and drying;
(2.2) adding the cleaned aramid fiber, biological enzyme and allyl glycidyl ether monomer into phosphate buffer solution, and then degassing;
(2.3) dropwise adding hydrogen peroxide solution into the system in the step (2.2) at a dropwise adding rate of 20mL/h;
after the dripping is finished, the mole ratio of hydrogen peroxide, allyl glycidyl ether monomer and biological enzyme in the system is 200:80:1, and the mass ratio of aramid fiber to allyl glycidyl ether monomer is 1000:1;
(2.4) heating the system of the step (2.3) for 20 hours at 50 ℃ to obtain pretreated aramid fibers;
the grafting rate of the allyl glycidyl ether monomer of the pretreated aramid fiber is 70%, the linear density of the aramid fiber is 2.63dtex, the average breaking strength of monofilaments is 48cN, the breaking strength is 17.5cN/dtex, and the elongation at break is 4.4%;
(3) Dyeing the pretreated aramid fiber:
placing the pretreated aramid fiber into a disperse type dyeing carrier at 60 ℃, gradually adding a dyeing agent and a dyeing auxiliary agent into a dye bath, dyeing for 45min under the conditions of 0.1MPa, 4.5 pH and 130 ℃ temperature, finally taking out, cleaning with a soap solution with the concentration of 3g/L at 58 ℃, and vacuum drying for 14h at 115 ℃ after cleaning, wherein the mass ratio of the aramid fiber, the disperse type dyeing carrier, the dyeing agent and the dyeing auxiliary agent is 200:1:5:3;
the dyeing rate of the dyed aramid fiber is 100%, the soaping-resistant color-staining fastness is 5 levels, the soaping-resistant color-fading fastness is 5 levels, the linear density is 2.60dtex, the average breaking strength of monofilaments is 47cN, the breaking strength is 17.4cN/dtex, and the breaking elongation is 4.3%.
Example 8
An aramid fiber dyeing method pretreated by biological enzyme is basically the same as in example 7, except that: in step (2.3), not the hydrogen peroxide solution but the same volume of water is added dropwise.
The grafting rate of the allyl glycidyl ether monomer of the pretreated aramid fiber is 55%;
the dyeing rate of the dyed aramid fiber is 96 percent, the soaping-resistant color fastness is 5 grade, and the soaping-resistant color fading fastness is 4 grade.
Claims (9)
1. The aramid fiber dyeing method with biological enzyme pretreatment is characterized in that aramid fiber is pretreated and then dyed; the pretreatment adopts biological enzyme, allyl glycidyl ether monomer and hydrogen peroxide, the biological enzyme activates benzene rings in the aramid fiber to form free radicals I in the pretreatment process, the free radicals I and the allyl glycidyl ether monomer undergo free radical active polymerization, and the hydrogen peroxide activates benzene rings in the aramid fiber to form free radicals II, and the free radicals II and the allyl glycidyl ether monomer undergo free radical active polymerization.
2. The method for dyeing aramid fiber pretreated with biological enzyme according to claim 1, wherein the biological enzyme is horseradish peroxidase, bovine liver catalase or xanthine peroxidase.
3. The method for dyeing aramid fiber pretreated by biological enzyme according to claim 1 or 2, which is characterized by comprising the following specific steps:
(1) Cleaning aramid fiber;
(2) Adding the cleaned aramid fiber, biological enzyme and allyl glycidyl ether monomer into phosphate buffer solution, and then degassing;
(3) Dropwise adding hydrogen peroxide solution into the system in the step (2);
(4) Heating the system of the step (3) to obtain pretreated aramid fibers;
(5) Dyeing the pretreated aramid fiber.
4. The method for dyeing aramid fibers by biological enzyme pretreatment according to claim 3, wherein in the step (1), the aramid fibers are para-aramid fibers, meta-aramid fibers or heterocyclic aramid fibers, and the average breaking strength of monofilaments of the aramid fibers is 35-50 cN.
5. The method for dyeing aramid fiber pretreated by biological enzyme according to claim 3, wherein in the step (2), the concentration of phosphate buffer solution is 0.067-0.20 mol/L, and the pH value is 6.4-7.6.
6. The method for dyeing aramid fiber pretreated by biological enzyme according to claim 3, wherein in the step (3), the volume fraction of the hydrogen peroxide solution is 20% -30%, and the dripping rate is 10-20 mL/h; after the dripping is finished, the molar ratio of the hydrogen peroxide, the allyl glycidyl ether monomer and the biological enzyme in the system in the step (3) is 100-200:50-80:1, and the mass ratio of the aramid fiber to the allyl glycidyl ether monomer is 100-1000:1.
7. The method for dyeing aramid fibers by biological enzyme pretreatment according to claim 3, wherein in the step (4), the heating temperature is 35-50 ℃, the time is 20-30 hours, and the grafting rate of allyl glycidyl ether monomer of the pretreated aramid fibers is 40-70%.
8. A method for dyeing aramid fiber pretreated with biological enzyme as claimed in claim 3, wherein in the step (5), the dyeing process is as follows: placing the pretreated aramid fiber into a dispersion type dyeing carrier at 40-60 ℃, then gradually adding a dyeing agent and a dyeing auxiliary agent into a dye bath, dyeing for 45-75 min under the conditions of 0.1MPa, 4.5-6 pH and 110-130 ℃, finally taking out, cleaning and drying; wherein the mass ratio of the aramid fiber to the disperse type dyeing carrier to the dyeing agent to the dyeing auxiliary is 50-200:1:2-5:1-3; the disperse type dyeing carrier is dimethyl terephthalate, methyl salicylate and carbonic acid acrylic ester; the dyeing agent is disperse brilliant red SF-B, disperse yellow G or disperse deep blue HGL; the dyeing auxiliary is dyeing auxiliary A-N, dyeing auxiliary P and dyeing auxiliary PNS.
9. The method for dyeing the aramid fiber by the biological enzyme pretreatment according to claim 1, wherein the dyeing rate of the dyed aramid fiber is 90% -100%, the soaping-resistant color fastness is 4-5, and the soaping-resistant color fading fastness is 4-5.
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