CN117005047A - Preparation method of micro-nano interface coupling construction of vinasse biological carbon powder and tourmaline powder and prepared functional fiber - Google Patents
Preparation method of micro-nano interface coupling construction of vinasse biological carbon powder and tourmaline powder and prepared functional fiber Download PDFInfo
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- CN117005047A CN117005047A CN202310896367.5A CN202310896367A CN117005047A CN 117005047 A CN117005047 A CN 117005047A CN 202310896367 A CN202310896367 A CN 202310896367A CN 117005047 A CN117005047 A CN 117005047A
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- powder
- tourmaline
- biochar
- vinasse
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- 239000000843 powder Substances 0.000 title claims abstract description 129
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- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 1
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- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
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- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
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- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- 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
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
-
- 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
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
-
- 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
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
-
- 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
- D01F6/90—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 polyamides
-
- 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
According to the invention, the porous carbon powder derived from the micro-nano white spirit vinasse biomass is combined with tourmaline powder characteristics for the first time, the special performances of the micro-nano white spirit vinasse biomass and tourmaline powder are functionally integrated, and the interface combination mode of the micro-nano white spirit vinasse biomass and tourmaline powder is designed on a microscopic scale. Under specific technological conditions, two kinds of powder are combined through chemical reaction at the interface, so that the performance of the two kinds of powder is synergistic and the two kinds of powder are fully functional structurally. The composite material is successfully applied to textiles, so that the composite material has more excellent functions (mildew prevention and warmth retention) and simultaneously has the functions of partial antibiosis, deodorization and anion release. In addition, the invention gives consideration to the abundance, diversity, stability and reliability of raw materials, such as tourmaline is natural ore, white spirit lees is derived from residual biomass resources in the brewing industry, fiber functionalization is realized by combining the tourmaline and the white spirit lees through ingenious design, healthy and comfortable functional fibers are produced, high added value can be provided for the utilization of biomass wastes, and the purposes of changing waste into valuables and improving the economic benefit of enterprises are achieved.
Description
Technical Field
The invention relates to a functional fiber, in particular to a preparation method of a micro-nano interface coupling structure of vinasse biological carbon powder and tourmaline powder and the functional fiber prepared by the method.
Background
"functional fiber" refers to a fiber in which a general fiber imparts a specific function(s) based on basic properties. Common introducing functions include antibiosis, mildew resistance, acarid expelling, temperature and humidity regulation, moisture absorption and quick drying, high emissivity far infrared, capability of generating anions, deodorization, electric conduction, flame retardance, oil resistance, pollution resistance, radiation resistance and the like. The preparation methods of the functional textiles generally comprise two methods: one is to develop and design a functional textile with corresponding functions by directly using the functional fibers; the other is to perform functional after-finishing on common fibers or textiles. The former process of directly preparing functional fibers often involves modifying conventional synthetic fiber materials, such as by blending and composite spinning, to introduce functional additives that are uniformly dispersed in the fibers in addition to the requirements of environmental protection and physiological safety, and that form stable and compatible phase interface materials with the fiber materials, giving the fibers a specific and stable function. Compared with the latter method which uses the after-finishing agent to carry out functional finishing on the fiber, the method for preparing the fiber by directly introducing the functional additive has the advantages of simple process, less produced pollutants and wastes, more stable and durable functions, and the like. "health functional fibers" are typically based on polyester, nylon, polypropylene, cotton, and the like, and include filaments and staple fibers. In recent years, with the development of society and the improvement of living standard, the demand for fibers with health functions for people is increasing. The advent of the emerging nano science and technology, which is made of various nano materials, provides a powerful support for developing various functional fibers, and the development of the industry presents a good development trend.
China is a large country in the wine industry, has rich varieties, and can produce more than ten millions of tons of white wine annually. While obtaining white spirit with rich taste, a great amount of vinasse biomass waste is inevitably produced in the production process of the white spirit. Besides a large amount of water, it is mainly composed of organic matters such as cellulose, hemicellulose, lignin, protein and the like, and contains components such as biological enzymes, alcohols, acids, esters and the like. Therefore, the distillers 'grains are easy to rot and deteriorate, not only can pollute the environment, but also can waste solid waste resources, and the distillers' grains are necessary to be reused. The traditional utilization method is to landfill compost, ferment to prepare methane and process the methane into products with lower added value such as animal feed. Because the distillers 'grains are rich in organic matters and oxygen and nitrogen groups, the distillers' grains biochar with rich pores can be prepared by a physical or chemical treatment method, and materials with higher added values such as soil improvement, catalyst development or additive development can be prepared. However, compared with the high-value carbon nanomaterial, the distillers' grains biomass charcoal has a very high lifting space.
Tourmaline, also called tourmaline or tourmaline, is a silicate mineral with a ring structure containing elements such as boron, aluminum, sodium, iron, magnesium, lithium and the like; the composition is various, and the surface is rich in hydrophilic groups such as hydroxyl groups. The tourmaline can permanently emit far infrared light with the wavelength of 4-14 mu m, has the far infrared emissivity of more than 0.88, and can be matched with a human body for resonance absorption to generate resonance effect and warming effect. Meanwhile, due to good pyroelectric property and piezoelectric effect, spontaneous polarization phenomenon can occur when temperature or pressure changes, and the device has the functions of natural electric polarity, negative ion release and the like.
The prior art with publication number CN 106400158A (a moisture-absorbing breathable and cool-feeling antistatic polyester filament yarn and a preparation method thereof) discloses a moisture-absorbing breathable and cool-feeling antistatic polyester filament yarn, and raw materials of the moisture-absorbing breathable and cool-feeling antistatic polyester filament yarn comprise 3-15 parts of bamboo activated carbon powder and 2-6 parts of nano tourmaline powder, so that the moisture-absorbing breathable and cool-feeling antistatic polyester filament yarn can be obtained, moisture-absorbing, mildew-proof, air-purifying, antibacterial, deinsectization, cool and refreshing and antistatic effects are provided for the polyester filament yarn, and meanwhile, the moisture-absorbing and cool-feeling antistatic polyester filament yarn has an ultraviolet-proof function and a protective effect, the tensile strength of the polyester filament yarn can be further enhanced, the breaking elongation is improved, and the service life of the polyester filament yarn is prolonged. However, the invention directly uses various powders to mix and stir uniformly, and the interfacial chemical reaction can not occur between the various powders, so that a firm micro-nano interface region which can interact can not be formed, that is, the mutual reinforcing effect can not be achieved.
Disclosure of Invention
Aiming at the problems, the invention combines the characteristics of the porous carbon powder derived from the micro-nano white spirit vinasse biomass with the characteristics of tourmaline powder for the first time, functionally integrates the special performances of the micro-nano white spirit vinasse biomass and the tourmaline powder, and microscopically designs the interface combination mode of the micro-nano white spirit vinasse biomass and the tourmaline powder. Under specific process conditions, two powders are combined by chemical reaction at an interface, so that the two powders are synergistic in performance and fully functional in structure. The composite material is successfully applied to textiles, so that the composite material has more excellent functions (mildew prevention and warmth retention) and simultaneously has the functions of partial antibiosis, deodorization and anion release. In addition, the invention gives consideration to the abundance and diversity of raw materials, such as tourmaline is natural ore, white spirit lees is derived from residual biomass resources in the brewing industry, and fiber functionalization is realized by combining the tourmaline and the residual biomass resources through ingenious design, so that not only healthy and comfortable functional fibers are produced, but also high added value is provided for the utilization of biomass wastes, the purposes of changing waste into valuables and improving the economic benefit of enterprises are achieved, and meanwhile, positive contribution is made to environmental pressure reduction.
The invention firstly provides a preparation method of micro-nano interface coupling construction of distillers ' grains biological carbon powder and tourmaline powder, wherein the distillers ' grains biological carbon powder and the tourmaline powder are respectively pretreated and modified to form pretreated and modified distillers ' grains biological carbon powder and pretreated and modified tourmaline powder, the pretreated and modified distillers ' grains biological carbon powder is further mixed with a dispersing agent and dried in vacuum, the pretreated and modified distillers ' grains biological carbon powder is prepared by mixing distillers ' grains dry powder with an activating agent, grinding and modifying biomass carbon powder obtained after carbonization with a surface modifying agent and spray drying, and the pretreated and modified tourmaline powder is prepared by grinding and modifying tourmaline powder with a surface activating agent and spray drying, and the vacuum drying enables the distillers ' grains biological carbon and tourmaline powder particles to form micro-nano interface connection areas.
The invention further provides a functional fiber with mildew resistance and antibacterial property, which is formed by spinning functional master batches, wherein the functional master batches comprise white spirit vinasse charcoal-tourmaline mixed functional powder, the white spirit vinasse charcoal-tourmaline mixed functional powder is formed by mixing raw materials comprising pretreated and modified white spirit vinasse charcoal powder, pretreated and modified tourmaline powder and a dispersing agent, and vacuum drying to form a micro-nano interface connection area between the white spirit vinasse charcoal and tourmaline powder particles, the pretreated and modified white spirit vinasse charcoal powder is formed by mixing white spirit vinasse dry powder and an activating agent, grinding and modifying the carbonized biomass charcoal powder and a surface modifying agent and spray drying, and the pretreated and modified tourmaline powder is formed by grinding and modifying tourmaline powder and a surface active agent and spray drying.
The activator is NaHCO 3 Or ZnCl 2 The surfactant is one of KH550 (APTES), KH570 and dimethyldiethoxysilane (DEDMS); the dispersing agent is selected from one or a mixture of more than two of stearamide, N ' -methyl distearamide, N ' -ethyl distearamide, hydroxyethyl ethylene distearamide and N, N ' -ethylene bis-12-hydroxy stearamide.
The distilled grain biochar-tourmaline mixed functional powder comprises 10-20 parts of pretreated and modified distilled grain biochar powder, 10-20 parts of pretreated and modified tourmaline powder and 1-6 parts of dispersing agent.
Finally, the invention provides a method for preparing a functional fiber with mildew-proof and antibacterial functions according to claim 1, which comprises the following steps:
the first step: pretreatment and surface modification of vinasse biological carbon powder and tourmaline powder
Uniformly mixing vinasse dry powder and an activating agent according to a proper proportion to obtain a preparation precursor of the biochar, and carbonizing the precursor at a high temperature in an inert gas atmosphere to obtain biomass carbon powder, wherein the carbonization temperature is 400-900 ℃ and the carbonization time is 0.5-3 h; mixing the obtained biomass carbon powder with a surface modifier, fully grinding and modifying in a sand mill, and spray-drying to obtain pretreated and modified vinasse biological carbon powder; fully grinding and modifying tourmaline powder and a surface modifier, and spray drying to obtain pretreated and modified tourmaline powder;
and a second step of: mixing and interfacial connection of vinasse biochar and tourmaline powder
Mixing the pretreated and modified vinasse biochar powder, the pretreated and modified tourmaline powder and a dispersing agent according to a certain mass ratio, and then forming a micro-nano interface connection area between the vinasse biochar and tourmaline powder particles under a vacuum drying condition to obtain the white spirit vinasse biochar-tourmaline mixed functional powder, wherein the vacuum drying temperature is 100-200 ℃, the vacuum degree is 0.05-0.1 torr, and the drying time is 2-6 h;
and a third step of: preparation of functional master batch and functional fiber
Mixing, extruding and granulating the white spirit vinasse biochar-tourmaline mixed functional powder, slicing and wetting agent to obtain mildew-proof antibacterial master batches; and carrying out melt spinning on the mildew-proof antibacterial master batch to obtain the fiber with the mildew-proof and antibacterial functions.
The vinasse dry powder in the first step is obtained by drying and crushing fresh white spirit vinasse with the water content of 50-65%, and tourmaline powder is 6000-12000 meshes.
The solid content of the ground material in the sand mill in the first step is 5-50 wt%, preferably 10-30% (solid: water solvent=5/95-50/50), and the grinding time is 0.5-4 h, preferably 1-2 h; the spray drying temperature is 120-160 ℃, the fan speed is 80-90%, the peristaltic pump speed is 30-70%, and the needle is 5-20 s.
The grain diameter of the vinasse biological carbon powder after surface modification in the second step is 50-200 nm, and the grain diameter of tourmaline powder after surface modification is 50-300 nm.
21-46 parts of white spirit vinasse charcoal-tourmaline mixed functional powder, 2-6 parts of wetting agent and 48-87 parts of slice; the slices include, but are not limited to, nylon, polypropylene, polyester slices; the wetting agent is preferably one or more of liquid paraffin, polyethylene wax, oxidized polyethylene wax, polypropylene wax, stearic acid, stearyl alcohol, calcium stearate, and ethyl bisstearamide polar modifier.
And in the third step, one of a single-screw extrusion granulator, a double-screw extrusion granulator, a banburying matched single-screw extrusion granulator, a banburying matched double-screw extrusion granulator and a double-stage extrusion granulator is selected for extrusion granulation, and the granulating temperature is set to be 150-280 ℃.
Compared with the prior art, the invention has the following effects:
1. the invention utilizes the distilled grain biochar to weave functional fibers, belongs to the recycling of residual biomass resources, improves economic benefit, fully recovers carbon-containing resources, and changes waste into valuable and assists the double-carbon policy.
2. According to the invention, the white spirit lees biochar and tourmaline are connected and compounded through interface atoms or molecular layers, so that the porosity and adsorptivity of the carbon material are fully exerted, and the function of tourmaline powder is synergistically enhanced to prepare the mildew-proof thermal insulation fiber with more excellent performance. The surface of the distilled grain biochar is rich in oxygen-containing groups, hydrophilic groups on the surface of the tourmaline are convenient for grafting modification, and the modified coupling agent reacts under specific vacuum and temperature conditions to form interface European chemical bond connection, so that two powders are in close contact to each other to enhance functions. The high specific surface area and the porosity of the distillers 'grains biochar are adjustable, the contact area between the distillers' grains biochar and tourmaline is increased, the far infrared wavelength emission of the tourmaline and the release of negative ions can be facilitated, and the performance of the tourmaline is cooperatively improved.
3. The invention is wet grinding and modified distillers' grains charcoal and tourmaline, and spray drying to obtain powder. Compared with dry ball milling, the powder obtained by wet milling has smaller and more uniform particle size, and the surface modifier is more fully combined.
4. The process improves the mixing uniformity of the product, and the agglomeration problem exists in the high-proportion nano powder in the melt spinning process.
Drawings
FIG. 1a is a diagram of a distillers' grains charcoal pair N obtained in example 1 2 Isothermal adsorption and desorption curves of (2); FIG. 1b is a pore distribution of distillers' grains biochar obtained in example 1A curve.
FIG. 2a is a diagram of a distillers' grains charcoal pair N obtained in example 2 2 Isothermal adsorption and desorption curves of (2); FIG. 2b is a pore distribution curve of the distillers grains biochar obtained in example 2.
FIG. 3a is a diagram of a distillers' grains charcoal pair N obtained in example 3 2 Isothermal adsorption and desorption curves of (2); FIG. 3b is a pore distribution curve of the distillers grains biochar obtained in example 3.
FIG. 4a is an SEM image of "micron-sized" distillers' grains biochar; fig. 4b is an SEM picture of "micro-nano" distillers' grains biochar.
FIG. 5a is an SEM image of "micron-sized" tourmaline powder; fig. 5b is an SEM image of "micro-nano scale" tourmaline powder.
Detailed Description
Example 1: preparation of distillers' grains biochar-tourmaline composite nylon filament
The first step: and (3) carrying out conventional drying and crushing processes on the fresh white spirit lees to obtain dried lees dry powder. Vinasse dry powder and an activator NaHCO 3 Evenly mixing the raw materials according to a proper proportion to obtain the preparation precursor of the biochar. The precursor is put in N 2 T in atmosphere 6 And (3) carbonizing for 2 hours at 600 ℃ to obtain the distillers' grains biological carbon powder. As can be seen from the isothermal adsorption/desorption curve of FIG. 1a, the relative partial pressure P/P 0 The obvious hysteresis between 0.4 and 0.9 shows that the distilled grain biochar is of a mesoporous structure, and as can be seen from the figure 1b, the pore diameter of the prepared distilled grain biochar is concentrated and distributed at 3-4 nm, the pore diameter distribution range is very narrow, and the obtained distilled grain biochar has a larger specific surface area and pore volume.
Grinding and surface modifying the obtained biomass charcoal. The biomass carbon powder obtained was mixed with the surface modifier DEDMS in a certain proportion by means of a sand mill and thoroughly ground for a period of 2h with a solids content of 20wt% (solids: water solvent=1:4) in the ground material. 10000 mesh tourmaline powder is subjected to surface modification by using the same material proportion and grinding conditions. And (3) carrying out spray drying on the ground material suspension to obtain powder, wherein the set temperature of a spray dryer is 150 ℃, the speed of a fan is 80%, the speed of a peristaltic pump is 65%, and the needle is 10 seconds. The dry powder is dried in a conventional oven at 80 ℃ for 24 hours.
And a second step of: the absolute dry mass of the preparation raw materials of the functional master batch is calculated according to 100 parts, and 10 parts of modified distilled grain biochar, 10 parts of modified 10000-mesh tourmaline powder and 3 parts of dispersing agent N, N' -methyl distearamide are respectively taken. Stirring for 20 minutes at 100 revolutions per minute by using a low-speed mixer to obtain the distilled grain biochar-tourmaline mixed functional powder. The powder is dried under vacuum, the vacuum degree is preferably 0.08-0.1 torr, the reaction (drying) time is 4h, and the reaction temperature is 120 ℃.
And a third step of: 23 parts of dried distilled grain biochar-tourmaline mixed functional powder, 3 parts of polyethylene wax and 74 parts of spinning grade nylon slice with the intrinsic viscosity of 2.40dL/g are weighed, and are stirred for 30 minutes at 150 revolutions per minute by using a low-speed mixer, so that the functional master batch preparation raw material is obtained.
Fourth step: adding the functional master batch preparation raw materials into a double-screw extrusion granulator, setting the temperature of each interval of a mixer to be 250 ℃ of a machine head, 220 ℃ of a first area, 250 ℃ of a second area, 250 ℃ of a third area, 250 ℃ of a fourth area, stirring by a screw, extruding a brace, cooling by water, granulating and drying to obtain the distilled grain biochar-tourmaline composite nylon master batch.
Fifth step: uniformly mixing the distilled grain biochar-tourmaline composite nylon master batch with nylon chips according to the mass ratio of 4:96, and producing according to the conventional nylon filament production process and production conditions to obtain the distilled grain biochar-tourmaline composite nylon filament with the filament specification of 75D/72F.
Example 2: preparation of distillers' grains biochar-tourmaline composite polyester staple fiber
The first step: and (3) carrying out conventional drying and crushing processes on the fresh white spirit lees to obtain dried lees dry powder. Vinasse dry powder and activator NaHCO 3 Evenly mixing the raw materials according to a proper proportion to obtain the preparation precursor of the biochar. The precursor is put in N 2 T in atmosphere 5 Carbonizing for 2h at 500 ℃ to obtain the distillers' grains biological carbon powder. As can be seen from the isothermal adsorption/desorption curve of FIG. 2a, the relative partial pressure P/P 0 An obvious hysteresis loop is arranged between 0.45 and 0.9, which indicates that the white spirit lees charcoal is of a mesoporous structure, and is shown by the figure2b, the pore diameter of the prepared distilled grain biochar is concentrated and distributed at 3.5-4 nm, the pore diameter distribution range is very narrow, and the prepared distilled grain biochar has a larger specific surface area and pore volume.
Grinding and surface modifying the obtained biomass charcoal. The biomass carbon powder obtained was mixed with the surface modifier DEDMS in a certain proportion by means of a sand mill and thoroughly ground for a period of 2h with a solids content of 20wt% (solids: water solvent=1:4) in the ground material. 10000 mesh tourmaline powder is subjected to surface modification by using the same material proportion and grinding conditions. The ground material suspension is subjected to spray drying to obtain powder, the spray drying temperature is 150 ℃, the fan speed is 80%, the peristaltic pump speed is 65%, and the needle is 10s. The dry powder is dried in a conventional oven at 80 ℃ for 24 hours.
And a second step of: the absolute dry mass of the preparation raw materials of the functional master batch is calculated according to 100 parts, and 10 parts of white spirit lees biological carbon powder, 10 parts of 12000-mesh tourmaline powder and 2 parts of dispersing agent N, N' -ethylene bis-12-hydroxystearamide are respectively taken. Stirring for 20 minutes at 100 revolutions per minute by using a low-speed mixer to obtain the distilled grain biochar-tourmaline mixed functional powder. The powder is dried under vacuum, the vacuum degree is preferably 0.08-0.1 torr, the reaction (drying) time is 4h, and the reaction temperature is 120 ℃.
And a third step of: 22 parts of dried distilled grain biochar-tourmaline mixed functional powder, 4 parts of polyethylene wax and 74 parts of PET slice with the intrinsic viscosity of 0.65dL/g are weighed, and the mixture is stirred for 30 minutes at 150 revolutions per minute by using a low-speed mixer, so that the functional master batch preparation raw material is obtained.
Fourth step: adding the functional master batch preparation raw materials into a double-screw extrusion granulator, setting the temperature of each section of a mixer to be 250 ℃ at the first section, the second section, the third section, the fourth section and the fourth section, stirring by a screw, extruding a brace, cooling by water, and granulating and drying to obtain the distilled grain biochar-tourmaline composite polyester master batch.
Fifth step: uniformly mixing the distilled grain biochar-tourmaline composite polyester master batch and the spinning-grade polyester chips according to the mass ratio of 5:95, and producing according to the conventional polyester staple fiber production process and production conditions to obtain the distilled grain biochar-tourmaline composite polyester staple fiber with the staple fiber specification of 3.33dtex 64mm.
Example 3: preparation of distillers' grains biochar-tourmaline composite "polypropylene staple fiber
The first step: and (3) carrying out conventional drying and crushing processes on the fresh white spirit lees to obtain dried lees dry powder. Vinasse dry powder and activator NaHCO 3 Evenly mixing the raw materials according to a proper proportion to obtain the preparation precursor of the biochar. The precursor is put in N 2 T in atmosphere 4 Carbonizing for 2h at 400 ℃ to obtain the distillers' grains biological carbon powder. As can be seen from the isothermal adsorption/desorption curve of FIG. 3a, the relative partial pressure P/P 0 The obvious hysteresis between 0.45 and 0.9 shows that the distilled grain biochar is of a mesoporous structure, and as can be seen from fig. 3b, the pore diameter of the prepared distilled grain biochar is concentrated and distributed at 3.5-4 nm, the pore diameter distribution range is very narrow, and the prepared distilled grain biochar has a larger specific surface area and pore volume.
Grinding and surface modifying the obtained biomass charcoal. The biomass carbon powder obtained was mixed with the surface modifier DEDMS in a certain proportion by means of a sand mill and thoroughly ground for a period of 2h with a solids content of 20wt% (solids: water solvent=1:4) in the ground material. 10000 mesh tourmaline powder is subjected to surface modification by using the same material proportion and grinding conditions. The ground material suspension is subjected to spray drying to obtain powder, the spray drying temperature is 150 ℃, the fan speed is 80%, the peristaltic pump speed is 65%, and the needle is 10s. The dry powder is dried in a conventional oven at 80 ℃ for 24 hours.
And a second step of: the absolute dry mass of the preparation raw materials of the functional master batch is calculated according to 100 parts, and 12 parts of vinasse biological carbon powder, 12 parts of 10000-mesh tourmaline powder and 3 parts of dispersing agent N, N' -ethylene bis-12-hydroxystearamide are respectively taken. Stirring for 20 minutes at 100 revolutions per minute by using a low-speed mixer to obtain the distilled grain biochar-tourmaline mixed functional powder. The mixture is dried (reacted) under vacuum, preferably at a vacuum of 0.08 to 0.1torr, for a reaction time of 4 hours and at a reaction temperature of 120 ℃.
And a third step of: 27 parts of dried distilled grain biochar-tourmaline mixed functional powder, 4 parts of calcium stearate and 69 parts of PP slices with the melt index of 40g/10min are weighed, and are stirred for 30 minutes at 150 revolutions per minute by using a low-speed mixer, so that the functional master batch preparation raw material is obtained.
Fourth step: adding the functional master batch preparation raw materials into a double-screw extrusion granulator, setting the temperature of each section of a mixer to be 215 ℃ of a machine head, 190 ℃ of a first section, 240 ℃ of a second section, 240 ℃ of a third section and 240 ℃ of a fourth section, stirring by a screw, extruding a brace, cooling by water, granulating and drying to obtain the distilled grain biochar-tourmaline composite polypropylene master batch.
Fifth step: uniformly mixing the distilled grain biochar-tourmaline composite polypropylene master batch with spinning-grade polypropylene chips according to the mass ratio of 4:96, and producing according to the conventional polypropylene short fiber production process and production conditions to obtain the distilled grain biochar-tourmaline composite polypropylene short fiber with the short fiber specification of 3.33dtex 32mm.
Comparative example 1: preparation of nylon filament containing only distilled grain biochar
The first step: comparative example 1, modified distillers' grains biochar powder was prepared.
And a second step of: and respectively taking 10 parts of white spirit vinasse charcoal and 2 parts of dispersing agent N, N' -methyl distearamide, and stirring for 20 minutes at 100 revolutions per minute by using a low-speed mixer to obtain white spirit vinasse charcoal functional powder.
And a third step of: 12 parts of dried distilled grain biochar functional powder, 2 parts of polyethylene wax and 86 parts of spinning grade nylon slices with the intrinsic viscosity of 2.40dL/g are weighed, and are stirred for 30 minutes at 150 revolutions per minute by using a low-speed mixer, so that the functional master batch preparation raw material is obtained.
Fourth step: adding the functional master batch preparation raw materials into a double-screw extrusion granulator, setting the temperature of each interval of a mixer to be 250 ℃ of a machine head, 220 ℃ of a first area, 250 ℃ of a second area, 250 ℃ of a third area, 250 ℃ of a fourth area, stirring by a screw, extruding a brace, cooling by water, granulating and drying to obtain the distilled grain biochar nylon master batch.
Fifth step: uniformly mixing the distilled grain biochar nylon master batch and nylon slices according to the mass ratio of 4:96, and producing the distilled grain biochar nylon filaments according to the conventional nylon filament production process and production conditions to obtain the distilled grain biochar nylon filaments with the filament specification of 75D/72F.
Comparative example 2: preparation of polyester staple fiber containing tourmaline only
The first step: in comparative example 2, 10 parts of modified tourmaline powder and 2 parts of dispersant N, N' -ethylenebis-12-hydroxystearamide were taken respectively, based on 100 parts of absolute dry mass of the preparation raw material of the functional master batch. Stirring for 20 minutes at 100 revolutions per minute by using a low-speed mixer to obtain tourmaline functional powder.
And a second step of: 12 parts of dried tourmaline mixed functional powder, 2 parts of polyethylene wax and 86 parts of PET slices with the intrinsic viscosity of 0.65dL/g are weighed, and stirred for 30 minutes at 150 revolutions per minute by using a low-speed mixer to obtain a functional masterbatch preparation raw material.
And a third step of: adding the functional master batch preparation raw materials into a double-screw extrusion granulator, setting the temperature of each section of the mixer to be 250 ℃ at the first section, the second section, the third section, the fourth section and the fourth section, stirring by a screw, extruding a brace, cooling by water, and granulating and drying to obtain the tourmaline polyester master batch.
Fourth step: the tourmaline polyester master batch and the spinning grade polyester chips are uniformly mixed according to the mass ratio of 5:95, and are produced according to the conventional polyester staple fiber production process and production conditions, so that the tourmaline polyester staple fiber is obtained, and the staple fiber specification is 3.33dtex 64mm.
Comparative example 3: preparation of distilled grain biochar-tourmaline composite nylon filament without vacuum drying (reaction)
In comparative example 1, the modified powder was directly mixed by a low-speed mixer, but was not dried (reacted) under vacuum, and a micro-nano interface connection region could not be formed between the distillers' grains carbon powder and tourmaline powder. Granulating the mixed powder and then discharging the filaments.
Comparative example 4: no modification of distiller's grains carbon powder and tourmaline powder
Such an embodiment does not. The unmodified powder has strong surface hydrophilicity and poor compatibility with the surface of the high-molecular polymer slice, and can not be directly used for spinning.
The following are test results of the mildew-proof and warm-keeping functions.
The distilled grain biochar-tourmaline composite fiber obtained in example 1, example 2 and example 3 was tested for mildew resistance according to the national standard "evaluation of mildew resistance of GB/T24346-2009 textiles", and the test results are shown in Table 1 below. Wherein comparative example 1 is a nylon filament containing only distillers' grains biochar. Comparative case 3 is a distilled grain biochar-tourmaline powder composite "nylon filament" without a vacuum drying (reaction) step.
TABLE 1 mildew resistance test results
As can be seen from table 1: the mildew resistance of the distilled grain biochar-tourmaline composite fiber obtained in the embodiment 1, the embodiment 2 and the embodiment 3 is higher than that of the comparative examples 1 and 2, and the mildew resistance grade reaches 0 grade. The results show that compared with the distilled grain biochar fiber and the distilled grain biochar-tourmaline composite fiber which is not subjected to vacuum drying (reaction), the fiber obtained by the embodiment has better mildew-proof effect.
Description:
1. "evaluation of GB/T24346-2009 textile mildew resistance", as shown in Table 2 below.
TABLE 2 evaluation criteria for mildew resistance
| Mold growth condition | Mildew resistant grade |
| No obvious mould growth under magnifying glass | 0 |
| Mold growth is rare or local, and the coverage area on the surface of the sample is less than 10 percent | 1 |
| The coverage area of mould on the surface of the sample is less than 30% | 2 |
| The coverage area of the mould on the surface of the sample is less than 60 percent (30 to 60 percent) | 3 |
| The coverage area of mould on the surface of the sample reaches or exceeds 60 percent | 4 |
The far infrared ray can generate resonance effect and warm effect with human body, so that the temperature of the body sensing environment is increased, heat preservation and heat accumulation are realized, the microcirculation of human blood is improved, and the activity of the organism is improved. The invention tests the warm-keeping effect according to the national standard GB/T30127-2013 detection and evaluation of far infrared performance of textiles, and the test results are shown in the following Table 3. Examples 1, 2 and 3 are white spirit vinasse biochar-tourmaline composite fibers, and comparative example 2 is polyester staple fiber only containing tourmaline. Comparative case 3 is a distilled grain biochar-tourmaline powder composite "nylon filament" without a vacuum drying (reaction) step.
TABLE 3 far infrared test results
As can be seen from table 3: the distilled grain biochar-tourmaline composite fiber obtained in example 1, example 2 and example 3 has higher far infrared radiation temperature rise and far infrared emissivity than those of comparative example 2 and higher far infrared emissivity than those of comparative example 3. The results show that compared with tourmaline fiber, distilled grain biochar-tourmaline composite fiber without vacuum drying (reaction), the fiber obtained by the embodiment has better far infrared emission effect.
Description:
1. "detection and evaluation of far infrared performance of GB/T30127-2013 textile", the evaluation criteria for far infrared performance of fiber samples are shown in Table 4 below.
TABLE 4 evaluation criteria for far infrared Performance of fiber samples
| Standard value | Single item determination | |
| Far infrared radiation temperature rise (DEG C) | ≥1.7 | Compliance with |
| Far infrared emissivity | ≥0.83 | Compliance with |
Claims (10)
1. A preparation method of micro-nano interface coupling construction of vinasse biological carbon powder and tourmaline powder is characterized in that the vinasse biological carbon powder and the tourmaline powder are respectively pretreated and modified to form pretreated and modified vinasse biological carbon powder and pretreated and modified tourmaline powder, the pretreated and modified tourmaline powder is further mixed with a dispersing agent and dried in vacuum to form a micro-nano interface connection area between the vinasse biological carbon and tourmaline powder particles, the pretreated and modified vinasse biological carbon powder is formed by grinding and modifying biomass carbon powder obtained by mixing and carbonizing vinasse dry powder and an activating agent with a surface modifying agent and spray-drying the biomass carbon powder obtained by grinding and modifying the vinasse dry powder with the surface activating agent, and the pretreated and modified tourmaline powder is formed by grinding and modifying the tourmaline powder with the surface activating agent and spray-drying the tourmaline powder.
2. The functional fiber with mildew resistance and antibacterial property is formed by spinning functional master batches, and is characterized in that the functional master batches comprise distilled grain biochar-tourmaline mixed functional powder, the distilled grain biochar-tourmaline mixed functional powder is formed by mixing and vacuum drying raw materials comprising pretreated and modified distilled grain biochar powder, pretreated and modified tourmaline powder and a dispersing agent, the pretreated and modified distilled grain biochar powder is formed by grinding and modifying biomass carbon powder obtained by mixing and carbonizing distilled grain dry powder with an activating agent, a surface modifying agent and spray drying, and the pretreated and modified tourmaline powder is formed by grinding and modifying tourmaline powder and a surface active agent and spray drying.
3. The functional fiber of claim 2, wherein the activator is NaHCO 3 Or ZnCl 2 The surfactant is one of KH550 (APTES), KH570 and dimethyldiethoxysilane (DEDMS); the dispersing agent is selected from one or a mixture of more than two of stearamide, N ' -methyl distearamide, N ' -ethyl distearamide, hydroxyethyl ethylene distearamide and N, N ' -ethylene bis-12-hydroxy stearamide.
4. The functional fiber according to claim 2, characterized in that the distilled grain biochar-tourmaline mixed functional powder comprises 10-20 parts of pretreated and modified distilled grain biochar powder, 10-20 parts of pretreated and modified tourmaline powder and 1-6 parts of dispersing agent.
5. A method for preparing the functional fiber with mildew-proof and antibacterial functions according to claim 1, characterized in that the method comprises the following steps:
the first step: pretreatment and surface modification of vinasse biological carbon powder and tourmaline powder
Uniformly mixing vinasse dry powder and an activating agent according to a proper proportion to obtain a preparation precursor of the biochar, and carbonizing the precursor at a high temperature in an inert gas atmosphere to obtain biomass carbon powder, wherein the carbonization temperature is 400-900 ℃ and the carbonization time is 0.5-3 h; mixing the obtained biomass carbon powder with a surface modifier, fully grinding and modifying in a sand mill, and spray-drying to obtain pretreated and modified vinasse biological carbon powder; fully grinding and modifying tourmaline powder and a surface modifier, and spray drying to obtain pretreated and modified tourmaline powder;
and a second step of: mixing and interfacial connection of vinasse biochar and tourmaline powder
Mixing the pretreated and modified vinasse biochar powder, the pretreated and modified tourmaline powder and a dispersing agent according to a certain mass ratio, and then forming a micro-nano interface connection area between the vinasse biochar and tourmaline powder particles under a vacuum drying condition to obtain the white spirit vinasse biochar-tourmaline mixed functional powder, wherein the vacuum drying temperature is 100-200 ℃, the vacuum degree is 0.05-0.1 torr, and the drying time is 2-6 h;
and a third step of: preparation of functional master batch and functional fiber
Mixing, extruding and granulating the white spirit vinasse biochar-tourmaline mixed functional powder, slicing and wetting agent to obtain mildew-proof antibacterial master batches; and carrying out melt spinning on the mildew-proof antibacterial master batch to obtain the fiber with the mildew-proof and antibacterial functions.
6. The method according to claim 5, wherein the distillers 'grains dry powder in the first step is obtained by drying and pulverizing fresh distillers' grains with 50-65% water content, and the tourmaline powder is 6000-12000 mesh.
7. The process according to claim 5, wherein the solid content of the ground material in the sand mill in the first step is 5 to 50wt%, preferably 10 to 30%, and the grinding time is 0.5 to 4 hours, preferably 1to 2 hours; the spray drying temperature is 120-160 ℃, the fan speed is 80-90%, the peristaltic pump speed is 30-70%, and the needle is 5-20 s.
8. The preparation method of claim 5, wherein the grain size of the surface-modified distillers' grains biological carbon powder in the second step is 50-200 nm, and the surface-modified tourmaline is further ground to 50-300 nm.
9. The preparation method according to claim 5, wherein the third step comprises 21-46 parts of white spirit lees biochar-tourmaline mixed functional powder, 2-6 parts of wetting agent and 48-87 parts of slices; the slices include, but are not limited to, nylon, polypropylene, polyester slices; the wetting agent is preferably one or more of liquid paraffin, polyethylene wax, oxidized polyethylene wax, polypropylene wax, stearic acid, stearyl alcohol, calcium stearate, and ethyl bisstearamide polar modifier.
10. The method according to claim 5, wherein the extrusion granulating in the third step is one of a single screw extrusion granulator, a twin screw extrusion granulator, a banburying matched single screw extrusion granulator, a banburying matched twin screw extrusion granulator and a double-stage extrusion granulator, and the granulating temperature is set to be 150-280 ℃.
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