CN113680314A - Fly ash loaded nano spherical magnesium hydroxide composite material and preparation method and application thereof - Google Patents

Fly ash loaded nano spherical magnesium hydroxide composite material and preparation method and application thereof Download PDF

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CN113680314A
CN113680314A CN202110949999.4A CN202110949999A CN113680314A CN 113680314 A CN113680314 A CN 113680314A CN 202110949999 A CN202110949999 A CN 202110949999A CN 113680314 A CN113680314 A CN 113680314A
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fly ash
magnesium hydroxide
composite material
hydroxide composite
spherical magnesium
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王彩丽
王斌
杨润全
王怀法
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Taiyuan University of Technology
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/041Oxides or hydroxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/3078Thermal treatment, e.g. calcining or pyrolizing
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/288Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4875Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
    • B01J2220/4887Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds

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Abstract

A fly ash loaded nanometer spherical magnesium hydroxide composite material and a preparation method and application thereof belong to the field of mineral material processing and environmental management, and can solve the problems that nanometer magnesium hydroxide is poor in dispersibility and processing flowability in a polymer and difficult to recover adsorbed heavy metal ions, and the problems that a fly ash filled polymer is high in abrasion and poor in compatibility, has a small specific surface area when used as an adsorbent and is poor in adsorbability. The fly ash loaded nanometer spherical magnesium hydroxide composite material is prepared by taking fly ash as a raw material and sodium hydroxide and magnesium chloride as coating agents and adopting a chemical precipitation method. The invention has important significance for the improvement of fly ash surface modification technology, heavy metal ion removal technology in sewage and nylon 6 mechanical property and flame retardant property technology.

Description

Fly ash loaded nano spherical magnesium hydroxide composite material and preparation method and application thereof
Technical Field
The invention belongs to the field of mineral material processing and environmental management, and particularly relates to a fly ash loaded nanometer spherical magnesium hydroxide composite material and a preparation method and application thereof.
Background
Toxic heavy metals of copper and lead ions in the wastewater not only bring serious environmental pollution, but also threaten the health of human beings. Therefore, the removal of copper and lead ions from the waste water is imminent. In recent years, researchers have treated heavy metal ions in sewage by various methods, among which the adsorption method is considered to be one of the most effective methods because it is low in cost, environment-friendly, and simple in operation, and the adsorbent can be regenerated by a suitable desorption process. The nano magnesium hydroxide is non-toxic and harmless, can slowly release hydroxide ions in a solution, has functional groups such as hydroxyl and the like as adsorption active sites, and is considered as a promising environment-friendly water treatment adsorbent. However, since the nano magnesium hydroxide has a fine particle size, it requires a long time of centrifugation or filtration after adsorption of heavy metal ions.
Nylon 6 is one of engineering plastics with the largest dosage, but the nylon 6 is easy to burn, and the application of the nylon in industries such as automobiles, electronics and the like is seriously influenced. In order to improve the mechanical property and the flame retardant property of nylon 6, a flame retardant is added by a melting method in the traditional method, but the flame retardant property and other important properties of nylon 6 cannot be simultaneously considered in the existing flame retardant system. The nano magnesium hydroxide has the advantages of high whiteness, flame retardance, smoke abatement, drop resistance, fine particle size, small abrasion to equipment and the like, the mechanical property and the flame retardance of the filled nylon 6 can be improved, but the nano magnesium hydroxide has poor dispersibility and processing flowability in polymers.
The fly ash is waste burnt by a power plant, is low in price and has-OH on the surface, so that the fly ash is used for adsorbing heavy metal ions in sewage by students, but the adsorption performance of untreated fly ash is very limited. The flame retardant property of the polymer can be improved to a certain extent by the polymer filled with the fly ash, but the polymer is seriously abraded to equipment when being filled, and the compatibility with a matrix is poor.
Disclosure of Invention
The invention aims to provide a preparation method and application of a fly ash loaded nanometer spherical magnesium hydroxide composite material, and nanometer composite powder is prepared by loading nanometer magnesium hydroxide on the surface of micron-sized fly ash. The composite powder can solve the problems of poor dispersibility and processing flowability of the nano magnesium hydroxide in the polymer and difficult recovery of adsorbed heavy metal ions, and can also solve the problems of high abrasion, poor compatibility, smaller specific surface area of the used adsorbent and poor adsorbability of the fly ash filled polymer.
The invention adopts the following technical scheme:
the fly ash loaded nanometer spherical magnesium hydroxide composite material is prepared by taking fly ash as a raw material and sodium hydroxide and magnesium chloride as coating agents through a chemical precipitation method, wherein the mass ratio of the magnesium hydroxide to the fly ash is 7-9: 10.
A preparation method of a fly ash loaded nanometer spherical magnesium hydroxide composite material comprises the following steps:
firstly, placing the fly ash in a muffle furnace to calcine at 800-900 ℃ for 90-150 min;
secondly, dissolving the calcined fly ash in 40-60mL of water, stirring and dispersing to obtain a suspension;
thirdly, placing the suspension in a water bath to be continuously stirred, heating to 80-100 ℃, and stirring at the rotating speed of 300-500 rpm;
fourthly, respectively preparing 0.2-0.4 mol/L sodium hydroxide solution and 0.1-0.2 mol/L magnesium chloride solution;
fifthly, simultaneously dripping a sodium hydroxide solution and a magnesium chloride solution into the calcined fly ash suspension at a dripping speed of 4-6 ml/min by a constant flow pump;
sixthly, after the dropwise addition is finished, continuously stirring for 80-100 min to continuously react;
and seventhly, filtering and washing the product obtained in the sixth step, adjusting the pH value to 9-11, filtering again, and drying at 100-120 ℃ for 360-480 min to obtain the fly ash loaded nano spherical magnesium hydroxide composite material.
Further, in the second step, the mass of the calcined fly ash is 10g, the mass ratio of the calcined fly ash to water is 1: 4-1: 6, and the stirring speed is 300-500 rpm.
Further, the reaction temperature in the fifth step is 80-100 ℃.
The composite material of fly ash loaded nanometer spherical magnesium hydroxide is used in eliminating heavy metal ion from waste water.
Further, the heavy metal ions are copper ions and lead ions, and the removal method comprises the following steps: 50ml of copper and lead ion solution with the concentration of 50-100 mg/L is measured by a measuring cylinder and respectively poured into a container, 0.025G-0.05G of composite material is weighed and poured into the container, the mixture is stirred and adsorbed for 120-180 min at the rotating speed of 200-300 rpm of a magnetic stirrer and at the temperature of 20-40 ℃, the mixed suspension is poured into a centrifuge tube for centrifugal separation for 10-20 min, and the concentration of copper and lead ions is measured by taking supernatant by a 721G visible spectrophotometer.
A composite material of fly ash loaded nanometer spherical magnesium hydroxide is applied to filling nylon 6.
Further, the application method comprises the following steps: drying nylon 6 in a vacuum oven at 100 ℃ for 24 hours, then blending the pure composite material and the nylon 6 by mass percent of 5-10% on a double-screw extruder, wherein the extrusion temperature is 190, 200, 210, 220, 230 and 240 ℃, the rotating speed is 200-300 r/min, the feeding speed is 10-20 r/min, mixing, extruding and granulating, drying in the vacuum oven at 100 ℃ for 24 hours, and then performing injection molding on a micro injection molding machine to obtain a sample strip for testing, wherein the injection molding temperature is 210, 220, 230 and 240 ℃. According to GB/T1634.1-2004, testing the thermal deformation temperature on a thermal deformation testing machine at a heating rate of 120 ℃/h and a load of 0.45 MPa; testing the tensile property on an electronic universal tester at the speed of 50mm/min according to GB/T1040-92; testing the bending performance on an electronic universal testing machine at the speed of 2mm/min according to GB/T1040-92; according to GB/T1043-93, the gap is 2mm, and the impact toughness is tested on a pendulum impact tester; melt index was tested on a melt index instrument at 240 ℃ according to GB/T3682-2000; the limiting oxygen index was tested on a limiting oxygen index tester according to GB/T2406-80.
The principle of the invention is as follows:
the invention takes fly ash as raw material and sodium hydroxide and magnesium chloride as coating agent; when the fly ash is subjected to inorganic precipitation coating modification, magnesium chloride and sodium hydroxide react on the surfaces of fly ash particles to precipitate magnesium hydroxide. Si-O-Mg-OH is formed between Si-OH on the surface of the fly ash and magnesium hydroxide, so that the composite powder with a stable shell-core structure is formed. During the precipitation of magnesium hydroxide from magnesium chloride solution, nucleation and crystal growth processes determine the size and morphology of the magnesium hydroxide particles. In the growth process of the magnesium hydroxide crystal grains, the solution is rotated and overturned by continuous stirring, the supersaturation degree of crystal substances around the magnesium hydroxide crystal grains is similar, and the growth opportunities and the growth speeds of the crystal in all directions are the same, so that the magnesium hydroxide crystal grains can grow into a spherical shape.
The invention has the following beneficial effects:
the invention has important significance for the improvement of fly ash surface modification technology, heavy metal ion removal technology in sewage and nylon 6 mechanical property and flame retardant property technology. The specific surface area of the fly ash loaded nano magnesium hydroxide composite powder prepared by the method is increased, so that the problems of poor dispersibility and processing flowability of nano magnesium hydroxide in a polymer and difficulty in recovering adsorbed heavy metal ions can be solved, and the problems of high abrasion, poor compatibility, smaller specific surface area and poorer adsorbability of a fly ash filled polymer as an adsorbent can be solved.
Drawings
FIG. 1 is SEM images of the fly ash of the present invention before and after loading with nano-magnesium hydroxide. FIG. 1a is a scanning electron micrograph of calcined fly ash; FIG. 1b is an SEM image of the fly ash-supported nano magnesium hydroxide composite powder prepared in example 1; FIG. 1c is an SEM image of the fly ash-supported nano magnesium hydroxide composite powder prepared in example 2; FIG. 1d is an SEM image of the fly ash-supported nano magnesium hydroxide composite powder prepared in example 3.
FIG. 2 is an XRD pattern of the fly ash of the present invention before and after loading with nano-magnesium hydroxide. FIG. 2a is an XRD pattern for calcined fly ash; FIG. 2b is an XRD pattern of the fly ash supported nano magnesium hydroxide composite powder prepared in example 1; FIG. 2c is an XRD pattern of the fly ash supported nano magnesium hydroxide composite powder prepared in example 2; fig. 2d is an XRD chart of the fly ash supported nano magnesium hydroxide composite powder prepared in example 3.
FIG. 3 is an FTIR chart of the fly ash of the present invention before and after loading with nano-magnesium hydroxide. FIG. 3a is a FTIR plot of calcined fly ash; FIG. 3b is an FTIR chart of the fly ash supported nano magnesium hydroxide composite powder prepared in example 1; FIG. 3c is an FTIR chart of the fly ash supported nano magnesium hydroxide composite powder prepared in example 2; fig. 3d is an FTIR chart of the fly ash supported nano magnesium hydroxide composite powder prepared in example 3.
Detailed Description
The present invention is further illustrated by, but is not limited to, the following examples.
Example 1
Calcining the fly ash in a muffle furnace for 90min at 800 ℃, weighing 10g of calcined fly ash and 40ml of water, and heating to 80 ℃ at the rotating speed of 300 rpm; weighing 8g of sodium hydroxide, dissolving in 1L of water, and preparing into 0.2mol/L sodium hydroxide solution; weighing 9.5g of magnesium chloride, and dissolving in 1L of water to prepare 0.1mol/L magnesium chloride solution; dropwise adding a sodium hydroxide solution and a magnesium chloride solution into the calcined fly ash suspension at a dropwise adding speed of 4ml/min by using a constant flow pump; after the dropwise adding is finished, continuously stirring for 80 min; and filtering and washing the product, adjusting the pH value to 9, filtering again, and drying at 100 ℃ for 360min to obtain the fly ash loaded nano spherical magnesium hydroxide composite material.
FIG. 1b is a scanning electron microscope image of the fly ash-loaded nano-magnesium hydroxide composite powder prepared in example 1; FIG. 2b is an XRD pattern of the fly ash supported nano-magnesium hydroxide composite powder prepared in example 1; fig. 3b is an FTIR chart of the fly ash-supported nano magnesium hydroxide composite powder prepared in example 1, and it can be seen that nano magnesium hydroxide particles are successfully supported on the surface of the fly ash of the composite powder prepared in example 1.
Measuring the specific surface area by adopting a BET method; the test results are shown in table 1. Table 1 shows the specific surface areas of the calcined fly ash and the samples of the examples. As can be seen from Table 1, in example 1, the specific surface area of the fly ash increases from 1.71m after loading the nano-magnesium hydroxide2The/g is increased to 57.25m2/g。
Application 1: using CuSO4•5H2O and waterPreparing a solution with copper ion concentration of 100 mg/L. 50ml of copper ion solution with the concentration of 100mg/L is measured by a measuring cylinder and poured into a beaker, 0.05G of composite powder is weighed and poured into the beaker, the mixture is stirred and adsorbed for 150min at the rotating speed of 300rpm of a magnetic stirrer and the temperature of 25 ℃, the mixed suspension is poured into a centrifugal tube for centrifugal separation for 10min, and the concentration of copper ions is measured by a 721G visible spectrophotometer from the supernatant. With Pb (NO)3)2And water to prepare a solution with lead ion concentration of 100 mg/L. Weighing 50ml of lead ion solution with the concentration of 100mg/L by using a measuring cylinder, pouring into a beaker, weighing 0.05G of composite powder, pouring into the beaker, stirring and adsorbing for 180min at the rotating speed of 300rpm of a magnetic stirrer and at the temperature of 25 ℃, pouring the mixed suspension into a centrifugal tube, carrying out centrifugal separation for 10min, and taking supernatant to measure the lead ion concentration by using a 721G visible spectrophotometer.
Application 1 data are shown in tables 2 and 3.
Application 2: drying nylon 6 in a vacuum oven at 100 ℃ for 24 hours, then blending the pure composite powder with the nylon 6 in a double-screw extruder according to the mass fraction of 5%, wherein the extrusion temperature is 190, 200, 210, 220, 230 and 240 ℃, the rotating speed is 250r/min, and the feeding speed is 15 r/min. Mixing, extruding and granulating, drying in a vacuum oven at 100 ℃ for 24 hours, and performing injection molding on a micro injection molding machine at injection molding temperatures of 210, 220, 230 and 240 ℃ to obtain test sample strips. The impact property, bending strength, bending modulus, tensile strength, heat distortion temperature, melt index and oxygen index of the alloy are tested.
Application 2 data are shown in table 4.
Example 2
Calcining the fly ash in a muffle furnace at 850 ℃ for 120min, weighing 10g of calcined fly ash and 50ml of water, and heating to 90 ℃ at the rotation speed of 400 rpm; weighing 12g of sodium hydroxide, dissolving in 1L of water, and preparing into 0.3mol/L sodium hydroxide solution; weighing 14.25g of magnesium chloride, and dissolving the magnesium chloride in 1L of water to prepare a 0.15mol/L magnesium chloride solution; dropwise adding a sodium hydroxide solution and a magnesium chloride solution into the calcined fly ash suspension at a dropwise adding speed of 5ml/min by using a constant flow pump; after the dropwise adding is finished, continuously stirring for 90 min; and filtering and washing the product, adjusting the pH value to 10, filtering again, and drying at 100 ℃ for 420min to obtain the fly ash loaded nano spherical magnesium hydroxide composite material.
FIG. 1c is a scanning electron microscope image of the fly ash-loaded nano-magnesium hydroxide composite powder prepared in example 2; FIG. 2c is an XRD pattern of the fly ash supported nano-magnesium hydroxide composite powder prepared in example 2; fig. 3c is an FTIR chart of the fly ash-supported nano magnesium hydroxide composite powder prepared in example 2, and it can be seen that nano magnesium hydroxide particles are successfully supported on the surface of the fly ash of the composite powder prepared in example 2.
Measuring the specific surface area by adopting a BET method; the test results are shown in table 1. Table 1 shows the specific surface areas of the calcined fly ash and the samples of the examples. As can be seen from Table 1, in example 2, the specific surface area of the fly ash is increased from 1.71m after the nano-magnesium hydroxide is loaded2The/g is increased to 58.59m2/g。
Application 1: using CuSO4•5H2O and water are used for preparing a solution with the copper ion concentration of 100 mg/L. 50ml of copper ion solution with the concentration of 100mg/L is measured by a measuring cylinder and poured into a beaker, 0.05G of composite powder is weighed and poured into the beaker, the mixture is stirred and adsorbed for 150min at the rotating speed of 300rpm of a magnetic stirrer and the temperature of 25 ℃, the mixed suspension is poured into a centrifugal tube for centrifugal separation for 10min, and the concentration of copper ions is measured by a 721G visible spectrophotometer from the supernatant. With Pb (NO)3)2And water to prepare a solution with lead ion concentration of 100 mg/L. Weighing 50ml of lead ion solution with the concentration of 100mg/L by using a measuring cylinder, pouring into a beaker, weighing 0.05G of composite powder, pouring into the beaker, stirring and adsorbing for 180min at the rotating speed of 300rpm of a magnetic stirrer and at the temperature of 25 ℃, pouring the mixed suspension into a centrifugal tube, carrying out centrifugal separation for 10min, and taking supernatant to measure the lead ion concentration by using a 721G visible spectrophotometer.
Application 1 data are shown in tables 2 and 3.
Application 2: nylon 6 was placed in a vacuum oven: drying for 24 hours at 100 ℃, then blending the pure composite powder with nylon 6 in a mass fraction of 5% on a double-screw extruder, wherein the extrusion temperature is 190, 200, 210, 220, 230 and 240 ℃, the rotating speed is 250r/min, and the feeding speed is 15 r/min. Mixing, extruding and granulating, drying in a vacuum oven at 100 ℃ for 24 hours, and performing injection molding on a micro injection molding machine at injection molding temperatures of 210, 220, 230 and 240 ℃ to obtain test sample strips. The impact property, bending strength, bending modulus, tensile strength, heat distortion temperature, melt index and oxygen index of the alloy are tested.
Application 2 data are shown in table 4.
Example 3
Calcining the fly ash in a muffle furnace at 900 ℃ for 150min, weighing 10g of calcined fly ash and 60ml of water, and heating to 100 ℃ at the rotating speed of 500 rpm; weighing 16g of sodium hydroxide, dissolving in 1L of water, and preparing into 0.4mol/L sodium hydroxide solution; weighing 19g of magnesium chloride, and dissolving the magnesium chloride in 1L of water to prepare a 0.2mol/L magnesium chloride solution; dropwise adding a sodium hydroxide solution and a magnesium chloride solution into the calcined fly ash suspension at a dropwise adding speed of 6ml/min by using a constant flow pump; after the dripping is finished, continuously stirring for 100 min; and filtering and washing the product, adjusting the pH value to 11, filtering again, and drying at 100 ℃ for 480min to obtain the fly ash loaded nano spherical magnesium hydroxide composite material.
FIG. 1d is a scanning electron microscope image of the fly ash-loaded nano-magnesium hydroxide composite powder prepared in example 3; FIG. 2d is an XRD pattern of the fly ash supported nano-magnesium hydroxide composite powder prepared in example 3; fig. 3d is an FTIR chart of the fly ash-supported nano magnesium hydroxide composite powder prepared in example 3, and it can be seen that nano magnesium hydroxide particles are successfully supported on the surface of the fly ash of the composite powder prepared in example 3.
Measuring the specific surface area by adopting a BET method; the test results are shown in table 1. Table 1 shows the specific surface areas of the calcined fly ash and the samples of the examples. As can be seen from Table 1, in example 3, the specific surface area of the fly ash is increased from 1.71m after the nano-magnesium hydroxide is loaded2The/g is increased to 59.34m2/g。
Application 1: using CuSO4•5H2O and water are used for preparing a solution with the copper ion concentration of 100 mg/L. 50ml of copper ion solution with the concentration of 100mg/L is measured by a measuring cylinder and poured into a beaker, 0.05G of composite powder is weighed and poured into the beaker, the mixture is stirred and adsorbed for 150min at the rotating speed of 300rpm of a magnetic stirrer and the temperature of 25 ℃, the mixed suspension is poured into a centrifugal tube for centrifugal separation for 10min, and the concentration of copper ions is measured by a 721G visible spectrophotometer from the supernatant. With Pb (NO)3)2And water to prepare a solution with lead ion concentration of 100 mg/L. Measuring 50ml concentration with a measuring cylinderPouring 100mg/L lead ion solution into a beaker, weighing 0.05G of composite powder, pouring into the beaker, stirring and adsorbing for 180min at the rotating speed of 300rpm of a magnetic stirrer and the temperature of 25 ℃, pouring the mixed suspension into a centrifuge tube, carrying out centrifugal separation for 10min, and taking supernatant and measuring the concentration of lead ions by a 721G visible spectrophotometer.
Application 1 data are shown in tables 2 and 3.
Application 2: drying nylon 6 in a vacuum oven at 100 ℃ for 24 hours, then blending the pure composite powder with the nylon 6 in a double-screw extruder according to the mass fraction of 5%, wherein the extrusion temperature is 190, 200, 210, 220, 230 and 240 ℃, the rotating speed is 250r/min, and the feeding speed is 15 r/min. Mixing, extruding and granulating, drying in a vacuum oven at 100 ℃ for 24 hours, and performing injection molding on a micro injection molding machine at injection molding temperatures of 210, 220, 230 and 240 ℃ to obtain test sample strips. The impact property, bending strength, bending modulus, tensile strength, heat distortion temperature, melt index and oxygen index of the alloy are tested.
Application 2 data are shown in table 4.
Embodiments 1-3 of the invention provide a preparation method and application of a fly ash loaded nanometer spherical magnesium hydroxide composite material. For comparison, 3 specific examples were prepared in different parts and the same in the same part.
Table 1 shows the results of the specific surface area measurements of the calcined fly ash and the samples of the examples. Table 2 shows the results of the copper ion removal detection analysis of the calcined fly ash and the samples of the examples. Table 3 shows the results of the lead ion removal detection analysis of the calcined fly ash and the samples of the examples. Table 4 shows the performance test results of pure nylon 6, calcined fly ash and the filled nylon 6 of the example.
As can be seen from table 1, the specific surface areas of the fly ash-supported nano magnesium hydroxide composite powders prepared in examples 1, 2 and 3 are all larger than the specific surface area of the calcined fly ash.
As can be seen from tables 2 and 3, the removal rate of the copper ions and lead ions adsorbed by the fly ash loaded nano magnesium hydroxide composite powder prepared in examples 1, 2 and 3 is higher than that of calcined fly ash, and the composite powder loaded with nano magnesium hydroxide can solve the problem that the nano magnesium hydroxide is difficult to recover heavy metal ions, and can also solve the problem of poor adsorbability when the fly ash is used as an adsorbent.
As can be seen from table 4, the mechanical properties and flame retardant properties of the fly ash loaded nano magnesium hydroxide composite powder filled nylon 6 prepared in examples 1, 2 and 3 are higher than those of pure nylon 6. The composite powder loaded with the nano magnesium hydroxide can solve the problems of poor dispersibility and processing flowability of the nano magnesium hydroxide in the polymer and also can solve the problems of high abrasion and poor compatibility of the fly ash filled polymer.
TABLE 1 specific surface area of calcined fly ash and example samples
Figure DEST_PATH_IMAGE002
TABLE 2 calcined fly ash and test results of copper ion removal analysis of the samples of examples
Figure DEST_PATH_IMAGE004
TABLE 3 calcined fly ash and test results of lead ion removal assay of the samples of examples
Figure DEST_PATH_IMAGE006
TABLE 4 Performance test results for pure nylon 6 and calcined fly ash, example sample filled nylon 6
Figure DEST_PATH_IMAGE008

Claims (8)

1. A fly ash loaded nanometer spherical magnesium hydroxide composite material is characterized in that: the fly ash is used as a raw material, sodium hydroxide and magnesium chloride are used as coating agents, and a chemical precipitation method is adopted to prepare the fly ash loaded nanometer spherical magnesium hydroxide composite material, wherein the mass ratio of the magnesium hydroxide to the fly ash is 7-9: 10.
2. The preparation method of the fly ash-loaded nano spherical magnesium hydroxide composite material as claimed in claim 1, which is characterized by comprising the following steps: the method comprises the following steps:
firstly, placing the fly ash in a muffle furnace to calcine at 800-900 ℃ for 90-150 min;
secondly, dissolving the calcined fly ash in 40-60mL of water, stirring and dispersing to obtain a suspension;
thirdly, placing the suspension in a water bath to be continuously stirred, heating to 80-100 ℃, and stirring at the rotating speed of 300-500 rpm;
fourthly, respectively preparing 0.2-0.4 mol/L sodium hydroxide solution and 0.1-0.2 mol/L magnesium chloride solution;
fifthly, simultaneously dripping a sodium hydroxide solution and a magnesium chloride solution into the calcined fly ash suspension at a dripping speed of 4-6 ml/min by a constant flow pump;
sixthly, after the dropwise addition is finished, continuously stirring for 80-100 min to continuously react;
and seventhly, filtering and washing the product obtained in the sixth step, adjusting the pH value to 9-11, filtering again, and drying at 100-120 ℃ for 360-480 min to obtain the fly ash loaded nano spherical magnesium hydroxide composite material.
3. The preparation method of the fly ash-loaded nano spherical magnesium hydroxide composite material according to claim 2, characterized by comprising the following steps: in the second step, the mass of the calcined fly ash is 10g, the mass ratio of the calcined fly ash to water is 1: 4-1: 6, and the stirring speed is 300-500 rpm.
4. The preparation method of the fly ash-loaded nano spherical magnesium hydroxide composite material according to claim 2, characterized by comprising the following steps: in the fifth step, the reaction temperature is 80-100 ℃.
5. The fly ash-loaded nano spherical magnesium hydroxide composite material as claimed in claim 1 is applied to removal of heavy metal ions in wastewater.
6. Use according to claim 5, characterized in that: the heavy metal ions are copper ions and lead ions, and the removal method comprises the following steps: 50ml of copper and lead ion solution with the concentration of 50-100 mg/L is measured by a measuring cylinder and respectively poured into a container, 0.025G-0.05G of composite material is weighed and poured into the container, the mixture is stirred and adsorbed for 120-180 min at the rotating speed of 200-300 rpm of a magnetic stirrer and at the temperature of 20-40 ℃, the mixed suspension is poured into a centrifuge tube for centrifugal separation for 10-20 min, and the concentration of copper and lead ions is measured by taking supernatant by a 721G visible spectrophotometer.
7. The fly ash-loaded nano spherical magnesium hydroxide composite material as claimed in claim 1 is applied to filled nylon 6.
8. Use according to claim 7, characterized in that: the application method comprises the following steps: drying nylon 6 in a vacuum oven at 100 ℃ for 24 hours, then blending the pure composite material and the nylon 6 by mass percent of 5-10% on a double-screw extruder, wherein the extrusion temperature is 190, 200, 210, 220, 230 and 240 ℃, the rotating speed is 200-300 r/min, the feeding speed is 10-20 r/min, mixing, extruding and granulating, drying in the vacuum oven at 100 ℃ for 24 hours, and then performing injection molding on a micro injection molding machine to obtain a sample strip for testing, wherein the injection molding temperature is 210, 220, 230 and 240 ℃.
CN202110949999.4A 2021-08-18 2021-08-18 Fly ash loaded nano spherical magnesium hydroxide composite material and preparation method and application thereof Pending CN113680314A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114259977A (en) * 2021-12-10 2022-04-01 太原理工大学 Preparation method and application of fly ash-loaded hydrated magnesium carbonate composite material
CN114685861A (en) * 2022-03-14 2022-07-01 太原理工大学 Fly ash loaded nano antimony doped tin oxide composite material and preparation method thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102869811A (en) * 2010-03-12 2013-01-09 科学与工业研究委员会 Process for the surface-modification of flyash and industrial applications thereof
CN103342857A (en) * 2013-06-25 2013-10-09 陕西理工学院 Method for preparing epoxy resin reinforced polypropylene-fly ash composite material
CN105885409A (en) * 2016-06-24 2016-08-24 随身科技(北京)有限公司 Flyash/nylon composite and preparation method and use
CN107446163A (en) * 2017-07-17 2017-12-08 太原理工大学 A kind of coal fly ash hollow micro bead Surface coating nano-sized magnesium hydroxide composite powder material and preparation method thereof
CN109433161A (en) * 2018-12-12 2019-03-08 太原理工大学 A kind of flyash cladding ZIF-8 composite powder material and its preparation method and application
CN110422864A (en) * 2019-08-27 2019-11-08 营口理工学院 A kind of modified Nano magnesium hydroxide and its preparation method and application

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102869811A (en) * 2010-03-12 2013-01-09 科学与工业研究委员会 Process for the surface-modification of flyash and industrial applications thereof
US20130095995A1 (en) * 2010-03-12 2013-04-18 Satyajit Vishnu Shukla Process For The Surface-Modification Of Flyash And Industrial Applications Thereof
CN103342857A (en) * 2013-06-25 2013-10-09 陕西理工学院 Method for preparing epoxy resin reinforced polypropylene-fly ash composite material
CN105885409A (en) * 2016-06-24 2016-08-24 随身科技(北京)有限公司 Flyash/nylon composite and preparation method and use
CN107446163A (en) * 2017-07-17 2017-12-08 太原理工大学 A kind of coal fly ash hollow micro bead Surface coating nano-sized magnesium hydroxide composite powder material and preparation method thereof
CN109433161A (en) * 2018-12-12 2019-03-08 太原理工大学 A kind of flyash cladding ZIF-8 composite powder material and its preparation method and application
CN110422864A (en) * 2019-08-27 2019-11-08 营口理工学院 A kind of modified Nano magnesium hydroxide and its preparation method and application

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
CAILI WANG等: "Preparation of Mg(OH)2/Calcined Fly Ash Nanocomposite for Removal of Heavy Metals from Aqueous Acidic Solutions", 《MATERIALS》 *
王彩丽等: "核壳结构粉煤灰基复合粉体制备及填充聚合物的性能", 《高分子材料科学与工程》 *
王静等: "纳米Mg(OH)2 包覆粉煤灰空心微珠复合粉体的制备及表征", 《中国粉体技术》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114259977A (en) * 2021-12-10 2022-04-01 太原理工大学 Preparation method and application of fly ash-loaded hydrated magnesium carbonate composite material
CN114685861A (en) * 2022-03-14 2022-07-01 太原理工大学 Fly ash loaded nano antimony doped tin oxide composite material and preparation method thereof

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