CN113550069B - Preparation process of terahertz hot-air cotton - Google Patents
Preparation process of terahertz hot-air cotton Download PDFInfo
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- CN113550069B CN113550069B CN202110893277.1A CN202110893277A CN113550069B CN 113550069 B CN113550069 B CN 113550069B CN 202110893277 A CN202110893277 A CN 202110893277A CN 113550069 B CN113550069 B CN 113550069B
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/541—Composite fibres, e.g. sheath-core, sea-island or side-by-side; Mixed fibres
- D04H1/5412—Composite fibres, e.g. sheath-core, sea-island or side-by-side; Mixed fibres sheath-core
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- 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
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/541—Composite fibres, e.g. sheath-core, sea-island or side-by-side; Mixed fibres
- D04H1/5418—Mixed fibres, e.g. at least two chemically different fibres or fibre blends
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/542—Adhesive fibres
- D04H1/544—Olefin series
Abstract
The invention discloses a preparation process of terahertz hot air cotton, belonging to the technical field of hot air cotton preparation. According to the invention, wave-absorbing material modified graphene powder and hot air cotton are combined, the application of the novel material in the traditional textile industry is widened, and graphene oxide is loaded with doping particles, wherein the doping particles comprise Fe-TiO 2 The electromagnetic wave absorbing material belongs to metal particles, and both the metal particles are wave absorbing materials, have electromagnetic shielding effectiveness, can absorb electromagnetic radiation, reduce electromagnetic reflection, and convert electromagnetic waves incident to the surface into heat energy as much as possible; in order to enable the modified graphene powder to be firmly combined with hot-air cotton, the modified graphene powder is introduced in a polyester master batch mode, firstly, graphene oxide is loaded with doped particles, then, surface modification is carried out, and then, the polyester master batch is obtained through melt extrusion. The invention has simple and feasible process and is easy for large-scale production.
Description
Technical Field
The invention belongs to the technical field of hot air cotton preparation, and relates to a preparation process of terahertz hot air cotton.
Background
The hot-air cotton belongs to one of non-woven fabrics, is a non-woven fabric which is bonded by heating through hot air in an oven after finishing carding fibers and is applied to heat preservation of various heat transfer and storage devices, machine sound absorption materials, pre-filtration of ventilation systems and KN95 masks. Terahertz (Terahertz, THz) is a cross-disciplinary emerging cross science developed in recent 20 years, and Terahertz waves generally refer to radiation with a frequency of 0.1-10THz, are 'vacuum zones' of electromagnetic spectrum which are researched at the latest, and have important research values in the fields of weapon stealth and the like.
The application of the material in the fields of stealth and anti-stealth can be expanded by combining the traditional textile hot air cotton with a new terahertz technology, and the problem to be solved in the industry is how to effectively combine the traditional textile hot air cotton with the new terahertz technology and realize simple, convenient and feasible preparation method.
Disclosure of Invention
The invention aims to provide a preparation process of terahertz hot-air cotton, and solves the technical problems mentioned in the background technology.
The purpose of the invention can be realized by the following technical scheme:
a preparation process of terahertz hot-air cotton comprises the following steps:
a1, extruding and melting polyethylene by a single-screw extruder to obtain a skin material melt;
step A2, extruding and melting the polyester master batch by a single-screw extruder to obtain a core material melt;
step A3, mixing the skin material melt and the core material melt, spraying melt trickle through a core spinneret plate, cooling and solidifying, oiling, drafting and heat setting, and finally winding and forming to prepare the PE fiber;
step A4, feeding the PE fibers and the PP fibers into a cotton mixer for full mixing, then feeding the mixture into a carding machine for carding, carding the fibers into monofilament shapes, and paving the monofilament shapes into uniform cotton nets;
and step A5, feeding the cotton net into a hot air oven, melting the PE fibers through hot air flow, bonding the PE fibers and the PP fibers together to form a non-woven fabric, carrying out spunlace treatment on the non-woven fabric, washing off an oil agent, then feeding the non-woven fabric into the oven for drying treatment, and cooling and shaping the dried non-woven fabric through cold air flow to obtain the terahertz hot air cotton.
Further, the set temperature of the single screw extruder in the step A1 is 180 to 220 ℃.
Further, the set temperature of the single screw extruder in the step A2 is 220-250 ℃.
Further, in the step A3, the mass ratio of the skin material melt to the core material melt is 1-2:1.3-2.3.
Further, the mass ratio of the PE fibers to the PP fibers in the step A4 is 0.6-1:1.
further, the temperature of the hot air oven in the step A5 is 145-155 ℃; the pressure of the spunlace treatment is 25-35MPa; the drying temperature is 110-125 ℃.
The polyester master batch is prepared by the following steps:
step S1, adding tetrabutyl titanate into absolute ethyl alcohol under magnetic stirring, dropwise adding concentrated nitric acid with the mass fraction of 60% to adjust the pH value to 6.2-6.5, recording as liquid A, dissolving ferric nitrate into an ethanol solution with the volume fraction of 91%, dropwise adding concentrated nitric acid with the mass fraction of 78% to adjust the pH value to 3, recording as liquid B, dropwise adding liquid B into the liquid A, stirring uniformly, standing for 3-4h, transferring to 650 ℃, calcining for 2.5-3h, and grinding to obtain doped particles;
s2, dispersing graphene oxide in absolute ethyl alcohol, adding doped particles, heating to 70 ℃, adjusting the pH to 4 by using hydrochloric acid with the mass fraction of 50%, adding an ethanol solution of KH-550, stirring for 3-4h, filtering, and drying a filter cake to obtain modified graphene powder;
and S3, adding the modified graphene powder and the polyester chips into a high-speed mixer, uniformly mixing, performing melt extrusion through a double-screw extruder, and cooling and granulating to obtain the polyester master batch.
Further, in the step S1, the dosage ratio of tetrabutyl titanate, absolute ethyl alcohol, ferric nitrate and ethanol solution with volume fraction of 91 percent is 30.5-35.3g:55.3-60.5mL:7.3-7.8g:46-50mL.
Further, in the step S2, the dosage ratio of the graphene oxide, the absolute ethyl alcohol, the doped particles and the KH-550 ethanol solution is 0.3-0.5g:15-20mL:55-58mg:10-12mL, wherein the dosage ratio of KH-550 to absolute ethyl alcohol in the KH-550 ethanol solution is 1.2-1.5g:10mL.
Further, in the step S3, the mass ratio of the modified graphene powder to the polyester chip is 1:8-10.
Further, the processing temperature of the melt extrusion of the twin-screw extruder in the step S3 is 240 ℃.
The invention has the beneficial effects that:
1) Based on the fact that terahertz belongs to one of wave bands of electromagnetic waves and has great contribution to future stealth and anti-stealth researches, the wave-absorbing material modified graphene powder and the hot air cotton are combined, the application of a novel material in the traditional textile industry is widened, graphene oxide is loaded with doped particles, and the component of the doped particles is Fe-TiO 2 The modified graphene powder belongs to metal particles, both of the modified graphene powder and the modified graphene powder are wave-absorbing materials, have electromagnetic shielding effect, can absorb electromagnetic radiation, reduce electromagnetic reflection and convert electromagnetic waves incident to the surface into heat energy as much as possible, and are introduced in a polyester master batch mode in order to enable the modified graphene powder to be firmly combined with the hot-air cottonFirstly, graphene oxide loads doping particles, then surface modification is carried out to increase the bonding force between the graphene oxide and polyester chips, and then the polyester master batch is obtained by melt extrusion, so that the process is simple and feasible, and the large-scale production is easy to realize.
2) The doped particles are prepared by a sol-gel method, and the main component is Fe-TiO 2 Purpose is Fe 3+ Uniformly dispersing the gel blocks in the titanium sol, and performing heat treatment to form uniformly dispersed Fe-doped TiO 2 Nanoparticles due to Fe 3+ Uniformly dispersed in the viscous sol and further uniformly fixed in a grid of Ti-O-Ti to inhibit the agglomeration of the sol.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Preparing polyester master batch:
step S1, adding 30.5g of tetrabutyl titanate into 55.3mL of absolute ethyl alcohol under magnetic stirring, dropwise adding 60 mass percent of concentrated nitric acid to adjust the pH value to 6.2, marking as solution A, dissolving 7.3g of ferric nitrate into 46mL of 91 volume percent ethanol solution, dropwise adding 78 mass percent of concentrated nitric acid to adjust the pH value to 3, marking as solution B, dropwise adding the solution B into the solution A, stirring uniformly, standing for 3h, transferring to 650 ℃, calcining for 2.5h, and grinding to obtain doped particles;
step S2, dispersing 0.4g of graphene oxide in 17mL of absolute ethyl alcohol, adding 56mg of doped particles, heating to 70 ℃, adjusting the pH to 4 by using hydrochloric acid with the mass fraction of 50%, adding 11mL of KH-550 ethanol solution, stirring for 3h, filtering, and drying a filter cake to obtain modified graphene powder, wherein the dosage ratio of KH-550 to absolute ethyl alcohol in the KH-550 ethanol solution is 1.2g:10mL;
and S3, adding the modified graphene powder and the polyester slices into a high-speed mixer, uniformly mixing, performing melt extrusion and cooling granulation through a double-screw extruder to obtain polyester master batches, wherein the mass ratio of the modified graphene powder to the polyester slices is 1:8, the processing temperature of the melt extrusion of the double-screw extruder is 240 ℃.
Example 2
Preparing polyester master batch:
step S1, adding 30.5g of tetrabutyl titanate into 57.5mL of absolute ethyl alcohol under magnetic stirring, dropwise adding 60 mass percent of concentrated nitric acid to adjust the pH value to 6.3, marking as solution A, dissolving 7.6g of ferric nitrate into 48mL of 91 volume percent ethanol solution, dropwise adding 78 mass percent of concentrated nitric acid to adjust the pH value to 3, marking as solution B, dropwise adding the solution B into the solution A, stirring uniformly, standing for 3h, transferring to 650 ℃, calcining for 2.5h, and grinding to obtain doped particles;
step S2, dispersing 0.4g of graphene oxide in 17mL of absolute ethyl alcohol, adding 56mg of doped particles, heating to 70 ℃, adjusting the pH to 4 by using hydrochloric acid with the mass fraction of 50%, adding 11mL of KH-550 ethanol solution, stirring for 3h, filtering, and drying a filter cake to obtain modified graphene powder, wherein the dosage ratio of KH-550 to absolute ethyl alcohol in the KH-550 ethanol solution is 1.4g:10mL;
and S3, adding the modified graphene powder and the polyester slices into a high-speed mixer, uniformly mixing, performing melt extrusion and cooling granulation through a double-screw extruder to obtain polyester master batches, wherein the mass ratio of the modified graphene powder to the polyester slices is 1:9, the processing temperature of the melt extrusion of the double-screw extruder is 240 ℃.
Example 3
Preparing polyester master batch:
step S1, adding 35.3g of tetrabutyl titanate into 60.5mL of absolute ethyl alcohol under magnetic stirring, dropwise adding 60 mass percent of concentrated nitric acid to adjust the pH value to 6.5, marking as solution A, dissolving 7.8g of ferric nitrate into 50mL of 91 volume percent of ethanol solution, dropwise adding 78 mass percent of concentrated nitric acid to adjust the pH value to 3, marking as solution B, dropwise adding the solution B into the solution A, stirring uniformly, standing for 4h, transferring to 650 ℃, calcining for 3h, and grinding to obtain doped particles;
step S2, dispersing 0.5g of graphene oxide in 20mL of absolute ethyl alcohol, adding 58mg of doped particles, heating to 70 ℃, adjusting the pH to 4 by using hydrochloric acid with the mass fraction of 50%, adding 12mL of KH-550 ethanol solution, stirring for 4h, filtering, and drying a filter cake to obtain modified graphene powder, wherein the dosage ratio of KH-550 to absolute ethyl alcohol in the KH-550 ethanol solution is 1.5g:10mL;
step S3, adding the modified graphene powder and the polyester chips into a high-speed mixer, uniformly mixing, performing melt extrusion through a double-screw extruder, and performing cooling and grain cutting to obtain polyester master batches, wherein the mass ratio of the modified graphene powder to the polyester chips is 1:10, the processing temperature of the melt extrusion of the double-screw extruder is 240 ℃.
Example 4
A preparation process of terahertz hot-air cotton comprises the following steps:
step A1, extruding and melting polyethylene by a single-screw extruder to obtain a skin material melt, wherein the set temperature of the single-screw extruder is 180 ℃;
step A2, extruding and melting the polyester master batch prepared in the embodiment 1 by using a single-screw extruder to obtain a core material melt, wherein the set temperature of the single-screw extruder is 220 ℃;
step A3, mixing the skin material melt and the core material melt according to a mass ratio of 1:1.3, spraying melt trickle through a core spinneret plate, cooling and solidifying, oiling, drafting and heat setting, and finally winding and forming to prepare the PE fiber;
step A4, mixing PE fibers and PP fibers in a mass ratio of 0.6:1, sending the mixture into a cotton mixer for full mixing, sending the mixture into a carding machine for carding, carding fibers into monofilament shapes, and laying the monofilament shapes into uniform cotton nets;
step A5, feeding the cotton net into a hot air oven, melting PE fibers through hot air flow, enabling the PE fibers and the PP fibers to be bonded together to form a non-woven fabric, carrying out spunlace treatment on the non-woven fabric, washing away oil, then feeding the non-woven fabric into the oven for drying treatment, and cooling and shaping the dried non-woven fabric through cold air flow to obtain the terahertz hot air cotton, wherein the temperature of the hot air oven is 145 ℃; the pressure of the spunlace treatment is 25MPa; the drying temperature is 110 ℃.
Example 5
A preparation process of terahertz hot-air cotton comprises the following steps:
a1, extruding and melting polyethylene by a single-screw extruder to obtain a skin material melt, wherein the set temperature of the single-screw extruder is 200 ℃;
step A2, extruding and melting the polyester master batch prepared in the embodiment 2 by using a single-screw extruder to obtain a core material melt, wherein the set temperature of the single-screw extruder is 230 ℃;
step A3, mixing the skin material melt and the core material melt according to a mass ratio of 1.5:1.8, spraying melt trickle through a core spinneret plate, cooling and solidifying, oiling, drafting and heat setting, and finally winding and forming to prepare PE fiber;
step A4, mixing the PE fibers and the PP fibers in a mass ratio of 0.8:1, sending the mixture into a cotton mixer for full mixing, sending the mixture into a carding machine for carding, carding fibers into monofilament shapes, and laying the monofilament shapes into uniform cotton nets;
step A5, feeding the cotton net into a hot air oven, melting PE fibers through hot air flow, bonding the PE fibers and PP fibers together to form a non-woven fabric, carrying out spunlace treatment on the non-woven fabric, washing off an oil agent, then feeding the non-woven fabric into the oven for drying treatment, and cooling and shaping the dried non-woven fabric through cold air flow to obtain the terahertz hot air cotton, wherein the temperature of the hot air oven is 150 ℃; the pressure of the spunlace treatment is 30MPa; the drying temperature is 120 ℃.
Example 6
A preparation process of terahertz hot-air cotton comprises the following steps:
a1, extruding and melting polyethylene by a single-screw extruder to obtain a skin material melt, wherein the set temperature of the single-screw extruder is 220 ℃;
step A2, extruding and melting the polyester master batch prepared in the embodiment 3 through a single-screw extruder to obtain a core material melt, wherein the set temperature of the single-screw extruder is 250 ℃;
step A3, mixing the skin material melt and the core material melt according to the mass ratio of 2:2.3 after mixing, spraying melt trickle through a core spinneret plate, cooling and solidifying, oiling, drafting and heat setting, and finally winding and forming to prepare the PE fiber;
step A4, mixing the PE fibers and the PP fibers in a mass ratio of 1:1, sending the mixture into a cotton mixer for full mixing, sending the mixture into a carding machine for carding, carding fibers into monofilament shapes, and laying the monofilament shapes into uniform cotton nets;
step A5, feeding the cotton net into a hot air oven, melting PE fibers through hot air flow, bonding the PE fibers and PP fibers together to form a non-woven fabric, carrying out spunlace treatment on the non-woven fabric, washing off an oil agent, then feeding the non-woven fabric into the oven for drying treatment, and cooling and shaping the dried non-woven fabric through cold air flow to obtain the terahertz hot air cotton, wherein the temperature of the hot air oven is 155 ℃; the pressure of the spunlace treatment is 35MPa; the drying temperature was 125 ℃.
Comparative example 1
Refer to the terahertz hot-air cotton prepared in example 1 of the chinese patent CN111809270 a.
Comparative example 2
Comparative example 2 method for manufacturing hot-air cotton referring to example 4, the difference is that PE fiber is replaced with commercial ordinary PE fiber.
Comparative example 3
Comparative example 3 method for preparing hot-air cotton referring to example 5, the difference is that modified graphene powder is replaced with graphene oxide.
The hot air cottons obtained in examples 4 to 6 and comparative examples 1 to 3 were subjected to the following performance tests, (1) testing the optical characteristics of the THz band of the sample by using a terahertz time-domain spectroscopy (THz-TDS) system model Z-3 (Zo-mega corporation), in a range of 0 to 10THz, at a temperature of 20.0 ℃, using a femtosecond laser MaiTai (American Spectroscopy physical Co., ltd.) to generate a laser having a center wavelength of 800nm and a pulse width of < 100fs, an average femtosecond pulse of 150mW, a bias voltage of 100V, and absorption values, and the test results are shown in Table 1:
TABLE 1
As can be seen from table 1, the hot air cottons prepared in examples 4 to 6 have superior electromagnetic wave absorption ability compared to comparative examples 1 to 3.
In the description of the specification, reference to the description of "one embodiment," "an example," "a specific example" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (1)
1. A preparation process of terahertz hot-air cotton is characterized by comprising the following steps:
a1, extruding and melting polyethylene by a single-screw extruder to obtain a skin material melt;
step A2, extruding and melting the polyester master batch by a single-screw extruder to obtain a core material melt;
step A3, mixing the skin material melt and the core material melt, spraying melt trickle through a core spinneret plate, cooling and solidifying, oiling, drafting and heat setting, and finally winding and forming to prepare the PE fiber;
step A4, conveying the PE fibers and the PP fibers into a cotton mixer for mixing, then conveying the mixture into a carding machine for carding, carding the fibers into monofilaments, and paving the monofilaments into uniform cotton nets;
step A5, feeding the cotton net into a hot air oven, melting the PE fibers through hot air flow, bonding the PE fibers and the PP fibers together to form a non-woven fabric, carrying out spunlace treatment on the non-woven fabric, then feeding the non-woven fabric into the oven for drying treatment, and cooling and shaping the dried non-woven fabric through cold air flow to obtain the terahertz hot air cotton;
the set temperature of the single screw extruder in the step A1 is 180-220 ℃;
the set temperature of the single screw extruder in the step A2 is 220-250 ℃;
in the step A3, the mass ratio of the skin material melt to the core material melt is 1-2:1.3-2.3;
in the step A4, the mass ratio of the PE fibers to the PP fibers is 0.6-1:1;
the temperature of the hot air oven in the step A5 is 145-155 ℃; the pressure of the spunlace treatment is 25-35MPa; the drying temperature is 110-125 ℃;
the polyester master batch is prepared by the following steps:
adding the modified graphene powder and the polyester slices into a high-speed mixer, uniformly mixing, performing melt extrusion through a double-screw extruder, and performing cooling and grain cutting to obtain polyester master batches;
the mass ratio of the modified graphene powder to the polyester chip is 1:8-10; the processing temperature of the melt extrusion of the double-screw extruder is 240 ℃;
the modified graphene powder is prepared by the following steps:
step S1, adding tetrabutyl titanate into absolute ethyl alcohol under magnetic stirring, dropwise adding concentrated nitric acid to adjust the pH to 6.2-6.5, marking as solution A, dissolving ferric nitrate into an ethanol solution with the volume fraction of 91%, dropwise adding concentrated nitric acid with the mass fraction of 78% to adjust the pH to 3, marking as solution B, dropwise adding the solution B into the solution A, stirring uniformly, standing for 3-4h, transferring to 650 ℃, calcining for 2.5-3h, and grinding to obtain doped particles;
s2, dispersing graphene oxide in absolute ethyl alcohol, adding doped particles, heating to 70 ℃, adjusting the pH to 4 with hydrochloric acid, adding an ethanol solution of KH-550, stirring for 3-4h, filtering, and drying a filter cake to obtain modified graphene powder;
in the step S1, the dosage ratio of tetrabutyl titanate, absolute ethyl alcohol, ferric nitrate and ethanol solution with volume fraction of 91 percent is 30.5-35.3g:55.3-60.5mL:7.3-7.8g:46-50mL; in the step S2, the dosage ratio of the graphene oxide, the absolute ethyl alcohol, the doped particles and the KH-550 ethanol solution is 0.3-0.5g:15-20mL:55-58mg:10-12mL, wherein the dosage ratio of KH-550 to absolute ethyl alcohol in the KH-550 ethanol solution is 1.2-1.5g:10mL.
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