CN115011162A - Attapulgite-reinforced carbon nanotube wave-absorbing material and preparation method thereof - Google Patents
Attapulgite-reinforced carbon nanotube wave-absorbing material and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 62
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 62
- 239000011358 absorbing material Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229960000892 attapulgite Drugs 0.000 claims abstract description 71
- 229910052625 palygorskite Inorganic materials 0.000 claims abstract description 71
- 239000000843 powder Substances 0.000 claims abstract description 27
- 239000013543 active substance Substances 0.000 claims abstract description 21
- 239000006096 absorbing agent Substances 0.000 claims abstract description 17
- 239000003085 diluting agent Substances 0.000 claims abstract description 14
- 239000003292 glue Substances 0.000 claims abstract description 13
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 9
- 239000004593 Epoxy Substances 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000011230 binding agent Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 63
- 239000000725 suspension Substances 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 239000004927 clay Substances 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 18
- 239000002736 nonionic surfactant Substances 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 14
- 239000000853 adhesive Substances 0.000 claims description 12
- 230000001070 adhesive effect Effects 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 239000002131 composite material Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000003822 epoxy resin Substances 0.000 claims description 9
- 229920000647 polyepoxide Polymers 0.000 claims description 9
- XPEKDHWAGKXPST-UHFFFAOYSA-N dysprosium(3+);propan-2-olate Chemical compound [Dy+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] XPEKDHWAGKXPST-UHFFFAOYSA-N 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000013504 Triton X-100 Substances 0.000 claims description 6
- 229920004890 Triton X-100 Polymers 0.000 claims description 6
- 230000002745 absorbent Effects 0.000 claims description 6
- 239000002250 absorbent Substances 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 238000001179 sorption measurement Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 239000004115 Sodium Silicate Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- ZPIRTVJRHUMMOI-UHFFFAOYSA-N octoxybenzene Chemical compound CCCCCCCCOC1=CC=CC=C1 ZPIRTVJRHUMMOI-UHFFFAOYSA-N 0.000 claims description 4
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 4
- 239000000243 solution Substances 0.000 description 9
- 150000002894 organic compounds Chemical class 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 239000007767 bonding agent Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003607 modifier Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 235000011037 adipic acid Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011852 carbon nanoparticle Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002048 multi walled nanotube Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/32—Radiation-absorbing paints
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses an attapulgite reinforced carbon nanotube wave-absorbing material and a preparation method thereof, belonging to the field of wave-absorbing materials. An attapulgite reinforced carbon nanotube wave-absorbing material comprises the following raw materials in parts by weight: 20-25 parts of waterborne epoxy AB glue, 25-30 parts of attapulgite/carbon nanotube wave absorber powder, 2-5 parts of an active agent, 2-3 parts of a binder, 0.1-0.5 part of a defoaming agent and 30-40 parts of a diluent.
Description
Technical Field
The invention relates to the field of wave-absorbing materials, in particular to an attapulgite reinforced carbon nanotube wave-absorbing material and a preparation method thereof.
Background
The stealth capability of a weapon system in modern war is the core science and technology for determining survival, so that the development of the research of the wave-absorbing material becomes the key of the stealth technology. Research shows that the wave absorbing material coated on the surface of a weapon system can effectively reduce electromagnetic wave signals to achieve a stealth effect, carbon nanotubes are used as a wave absorbing agent to achieve ideal dielectric loss, but have small magnetic loss to electromagnetic waves, and meanwhile, the carbon nanotubes have poor hydrophilicity, are easy to agglomerate when the wave absorbing material is prepared, are easy to burn and lose under the condition of high-temperature air at 500 ℃, and are easy to burn and lose at high-temperature parts such as tail nozzles of airplanes and the like, the working temperature of the high-temperature parts is often above 700 ℃, and the wave absorbing performance is easily removed by simply using the carbon nanotubes, and document CN104479626B discloses a graphitized multi-walled carbon nanotube/nanoparticle composite wave absorbing agent and a preparation method thereof, which have good wave absorbing performance, but the coating is easy to peel off under high-temperature and high-speed air scouring, and the wave absorbing performance of the wave absorbing material is seriously influenced.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an attapulgite reinforced carbon nanotube wave-absorbing material and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
an attapulgite reinforced carbon nanotube wave-absorbing material comprises the following raw materials in parts by weight:
20-25 parts of water-based epoxy AB glue, 25-30 parts of attapulgite/carbon nano tube wave absorbing agent powder, 2-5 parts of an active agent, 2-3 parts of a binder, 0.1-0.5 part of a defoaming agent and 30-40 parts of a diluent.
Optionally, the active agent is polyethylene glycol octyl phenyl ether type nonionic surfactant.
Optionally, the adhesive is a mixed adhesive and is prepared by mixing polyvinyl butyral and hydrated sodium silicate according to a ratio of 1:1.
Optionally, the preparation method of the attapulgite/carbon nanotube wave absorber powder comprises the following steps:
step 1, weighing 100g of attapulgite clay with the fineness of 200-; adding 5-10ml of composite active agent into the treated suspension, then dropwise adding NaOH solution to adjust the pH value of the suspension to 6-8, stirring for 2-4 hours at 1500 rpm by using a cross stirring blade stirrer, standing for 10 hours, and separating the attapulgite clay suspension;
step 2, Dy (OC) 3 H 7 ) 3 And water according to a molar ratio of 1: 60-80 deg.C in reflux device and 70-80 deg.CStirring for 2-4 hr to completely hydrolyze dysprosium isopropoxide, stirring hydrolyzed mixture DyO (OH) at 90 deg.C, and adding HNO 3 And Dy (OC) 3 H 7 ) 3 In a molar ratio of 0.05-0.07:1, adding HNO 3 Continuously stirring for 2 hours at the temperature of 60-85 ℃ to enable the solution to be colloidal;
step 3, putting 10g of carbon nano tube into a glass bottle, then adding 500ml of deionized water, adding 2-4ml of Triton X-100 nonionic surfactant, stirring in a constant-temperature water bath, keeping the rotating speed at 350-; slowly adding the sol into a system according to the volume ratio of 1:2, dropwise adding ammonia water, adjusting the pH value of the system to 9-10, ultrasonically mixing for 30 minutes at 50 ℃, standing and aging for 12 hours at 60 ℃, cooling to room temperature, washing for 3-5 times by using deionized water, and drying for 24 hours in a vacuum drying oven at 80 ℃; calcining the mixture for 1 hour in the atmosphere of 400-500 ℃ to obtain Dy wrapped on the surface 2 O 3 A particulate carbon nanotube;
step 4, adding 10-20g of carbon nano tubes into the separated attapulgite suspension, utilizing the adsorption property of the attapulgite surface to bond the carbon nano tubes,
step 5, ultrasonically dispersing the attapulgite clay suspension for 1-2h at the temperature of 70-90 ℃, standing for 10-20min, centrifuging for 2-5 times in a centrifuge, each time for 5 min, filtering and recovering solids;
and 6, drying the recovered solid at 70-100 ℃ for 24h, and grinding the dried solid with an agate mortar to obtain the attapulgite/carbon nanotube absorbent powder with excellent wave-absorbing performance.
5. A preparation method of a wave-absorbing material comprises the following steps:
step 1, pouring 20-25 parts of diluent into a stirrer, adding the waterborne epoxy resin A glue into the stirrer and stirring the mixture;
step 2, adding 25-30 parts of attapulgite/carbon nanotube wave absorbing agent powder and 2-5 parts of active agent into the mixed system in the step 1 and stirring;
step 3, pouring the rest of the diluent into a stirrer, adding the waterborne epoxy resin B glue, 2-3 parts of the adhesive and 0.1-0.5 part of the defoaming agent into the stirrer, and putting the mixture into a cross stirring blade stirrer for fully stirring to prepare a component B for later use;
and 4, putting the components A and B into a container for stirring to prepare the wave-absorbing material.
Optionally, the active agent is polyethylene glycol octyl phenyl ether type nonionic surfactant.
Optionally, the adhesive is a mixed adhesive and is prepared by mixing polyvinyl butyral and hydrated sodium silicate according to a ratio of 1:1.
Optionally, the preparation method of the attapulgite/carbon nanotube wave absorber powder comprises the following steps:
step 1, weighing 100g of attapulgite clay with the fineness of 200-; adding 5-10ml of composite active agent into the treated suspension, then dropwise adding NaOH solution to adjust the pH value of the suspension to 6-8, stirring for 2-4 hours at 1500 rpm by using a cross stirring blade stirrer, standing for 10 hours, and separating the attapulgite clay suspension;
step 2, Dy (OC) 3 H 7 ) 3 The molar ratio of the water to the water is 1: 60-80 placing in reflux device, stirring at 70-80 deg.C for 2-4 hr to completely hydrolyze dysprosium isopropoxide, stirring hydrolyzed mixture DyO (OH) at 90 deg.C, and adding HNO 3 And Dy (OC) 3 H 7 ) 3 In a molar ratio of 0.05-0.07:1, adding HNO 3 Continuously stirring for 2 hours at the temperature of 60-85 ℃ to enable the solution to be colloidal;
step 3, putting 10g of carbon nano tube into a glass bottle, then adding 500ml of deionized water, adding 2-4ml of Triton X-100 nonionic surfactant, stirring in a constant-temperature water bath, keeping the rotating speed at 350-; slowly adding the sol into a system according to the volume ratio of 1:2, dropwise adding ammonia water, adjusting the pH value of the system to 9-10, ultrasonically mixing for 30 minutes at 50 ℃, standing and aging for 12 hours at 60 ℃, cooling to room temperature, washing for 3-5 times by using deionized water, and drying for 24 hours in a vacuum drying oven at 80 ℃; calcining the mixture for 1 hour in the atmosphere of 400-500 ℃ to obtain Dy wrapped on the surface 2 O 3 A particulate carbon nanotube;
step 4, adding 10-20g of carbon nano tubes into the separated attapulgite suspension, and utilizing the adsorption property of the attapulgite surface to bond the carbon nano tubes;
step 5, ultrasonically dispersing the attapulgite clay suspension for 1-2h at the temperature of 70-90 ℃, standing for 10-20min, centrifuging for 2-5 times in a centrifuge, each time for 5 min, filtering and recovering solids;
and 6, drying the recovered solid for 24 hours at 70-100 ℃, and grinding the dried solid into powder by using an agate mortar, wherein the powder is the attapulgite/carbon nanotube absorbent.
The invention has the beneficial effects that: to pair
Compared with the prior art, the invention has the following advantages:
the attapulgite clay powder is coated with a layer of composite active agent mixed by organic compounds and nonionic surfactants, which can inhibit the polymerization reaction among the attapulgite clay powder, improve the compatibility and the dispersibility of the attapulgite clay powder in aqueous solution, obtain high-dispersibility attapulgite clay suspension, adsorb the attapulgite clay suspension on the surface of the attapulgite clay powder by utilizing the high activity of carbon nano tubes, carry out surface curing through aqueous epoxy resin, form coatings with excellent wave-absorbing efficiency on the surfaces of various substrates, have simple and convenient process and can be used for construction treatment of large-scale equipment and site surfaces.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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:
an attapulgite reinforced carbon nanotube wave-absorbing material is prepared from the following raw materials in parts by weight: 20 parts of waterborne epoxy AB glue, 25 parts of attapulgite/carbon nanotube wave absorbing agent powder, 5 parts of an active agent, 2 parts of a bonding agent, 0.5 part of a defoaming agent and 30 parts of a diluent.
The preparation method comprises the following steps:
step 1, pouring 20 parts of diluent into a stirrer, adding the aqueous epoxy resin A glue into the stirrer, and fully stirring the mixture at the stirring speed of 2500 rpm for 50 minutes.
And 2, adding the attapulgite/carbon nano tube wave absorbing agent powder and the active agent into the mixed system in the step 1, and fully stirring for 1-2 hours.
And 3, pouring the rest diluent into a stirrer, adding the waterborne epoxy resin B glue, the adhesive and the defoaming agent into the stirrer, and putting the mixture into a cross-shaped stirring knife stirrer for fully stirring at the stirring speed of 2000 revolutions per minute for 30 minutes to prepare a component B for later use.
And 4, putting the components A and B into a container for stirring, stirring the components A and B in an electric stirrer at the speed of 200 rpm for 30 minutes to prepare the wave-absorbing material, uniformly coating the stirred spraying material on the surfaces of various matrixes through special spraying equipment, and drying the materials for 2 hours to achieve a good wave-absorbing effect.
The preparation method of the attapulgite/carbon nanotube wave absorber powder comprises the following process steps:
step 1, weighing 100g of attapulgite clay with fineness of 300 meshes, putting the attapulgite clay into 800ml of distilled water, stirring the attapulgite clay for 2 hours by using a stirrer, and treating the attapulgite clay for 2 hours at 80 ℃ by using 80ml of hydrochloric acid with solubility of lmol/L; adding 5ml of composite active agent into the treated suspension, then dropwise adding NaOH solution to adjust the pH value of the suspension to 7, stirring for 3 hours at 1500 rpm by using a cross stirring blade stirrer, standing for 10 hours, and separating the attapulgite clay suspension.
Step 2, dysprosium isopropoxide (Dy (OC) 3 H 7 ) 3 ) The molar ratio of the water to the water is 1: 60 placing in a reflux device, stirring at 70 deg.C for 3 hr to completely hydrolyze dysprosium isopropoxide, stirring hydrolyzed mixture DyO (OH) at 90 deg.C, and performing HNO 3 And Dy (OC) 3 H 7 ) 3 In a molar ratio of 0.05:1, adding HNO 3 Stirring was continued for 2h at 60 ℃ to make the solution gummy and ready for use.
Step 3, adding 10Putting the carbon nano tube into a glass bottle, adding 500ml of deionized water, adding 4ml of Triton X-100 nonionic surfactant, stirring in a constant-temperature water bath, keeping the rotating speed at 350r.min < -1 >, and keeping the temperature of the system at 50 ℃. Slowly adding the sol into the system according to the volume ratio of 1:2, dropwise adding ammonia water, adjusting the pH value of the system to 10, ultrasonically mixing for 30 minutes at 50 ℃, standing and aging for 12 hours at 60 ℃, cooling to room temperature, washing for 3-5 times by using deionized water, and drying for 24 hours in a vacuum drying oven at 80 ℃. Finally, calcining for 1h in the atmosphere of 400 ℃ to obtain Dy wrapped on the surface 2 O 3 Carbon nanotubes of particles.
Step 4, adding 10g of carbon nano tubes into the separated attapulgite suspension, utilizing the adsorption property of the attapulgite surface to bond the carbon nano tubes,
step 5, ultrasonically dispersing the attapulgite clay suspension at the temperature of 90 ℃ for 2 hours, standing for 20min, centrifuging for 2 times in a centrifuge, each time for 5 minutes, and filtering to recover solids;
step 6, drying the recovered solid for 24 hours at 100 ℃, and grinding the dried solid by using an agate mortar to obtain attapulgite/carbon nanotube absorbent powder with excellent wave-absorbing performance;
the composite modifier comprises an organic compound and a nonionic surfactant, wherein the volume ratio of the organic compound to the nonionic surfactant is 1:1, and the organic compound is adipic acid; a nonionic surfactant (OP-10) type active agent;
example 2:
an attapulgite reinforced carbon nanotube wave-absorbing material is prepared from the following raw materials in parts by weight: 25 parts of waterborne epoxy AB glue, 30 parts of attapulgite/carbon nanotube wave absorbing agent powder, 4 parts of an active agent, 3 parts of a bonding agent, 0.5 part of a defoaming agent and 40 parts of a diluent.
The preparation method comprises the following steps:
step 1, pouring 25 parts of diluent into a stirrer, adding the waterborne epoxy resin A glue into the stirrer, and fully stirring the mixture at the stirring speed of 2000 rpm for 40 minutes;
step 2, adding attapulgite/carbon nano tube wave absorbing agent powder and an active agent into the mixed system in the step 1, and fully stirring for 2 hours;
step 3, pouring the rest of the diluent into a stirrer, adding the waterborne epoxy resin B glue, the adhesive and the defoaming agent into the stirrer, putting the mixture into a cross-shaped stirring knife stirrer, and fully stirring the mixture at the stirring speed of 1500 revolutions per minute for 60 minutes to prepare a component B for later use;
and 4, putting the components A and B into a container for stirring, stirring the components A and B in an electric stirrer at the speed of 500 rpm for 30 minutes to prepare the wave-absorbing material, uniformly coating the stirred spraying material on the surfaces of various matrixes through special spraying equipment, and drying the materials for 2 hours to achieve a good wave-absorbing effect.
The preparation method of the attapulgite/carbon nanotube wave absorber powder comprises the following process steps:
step 1, weighing 100g of attapulgite clay with the fineness of 200 meshes, putting the attapulgite clay into 800ml of distilled water, stirring the attapulgite clay for 4 hours by using a stirrer, and treating the attapulgite clay for 3 hours at 100 ℃ by using 80ml of hydrochloric acid with the solubility of lmol/L; adding 8ml of composite active agent into the treated suspension, then dropwise adding NaOH solution to adjust the pH value of the suspension to 6, stirring for 4 hours at 1500 rpm by using a cross stirring blade stirrer, standing for 10 hours, and separating the attapulgite clay suspension;
step 2, dysprosium isopropoxide (Dy (OC) 3 H 7 ) 3 ) The molar ratio of the compound to water is 1: 70 placing in a reflux device, stirring at 80 deg.C for 4 hr to completely hydrolyze dysprosium isopropoxide, stirring hydrolyzed mixture DyO (OH) at 90 deg.C, and performing HNO 3 And Dy (OC) 3 H 7 ) 3 In an amount of 0.07:1, HNO is added 3 Continuously stirring for 2 hours at the temperature of 60-85 ℃ to enable the solution to be colloidal for later use;
and 3, putting 10g of carbon nano tube into a glass bottle, adding 500ml of deionized water, adding 3ml of Triton X-100 nonionic surfactant, stirring in a constant-temperature water bath, keeping the rotating speed at 350r.min < -1 >, and maintaining the temperature of the system at 50 ℃. Slowly adding the sol into the system according to the volume ratio of 1:2, dropwise adding ammonia water, adjusting the pH value of the system to 10, ultrasonically mixing for 30 minutes at 50 ℃, standing at 60 DEG CAging for 12h, cooling to room temperature, washing with deionized water for 3-5 times, and drying in a vacuum drying oven at 80 deg.C for 24 h. Finally, calcining the mixture for 1 hour in the atmosphere at the temperature of 400-500 ℃ to obtain Dy wrapped on the surface 2 O 3 Carbon nanotubes of particles.
Step 4, adding 15g of carbon nano tubes into the separated attapulgite suspension, utilizing the adsorption property of the attapulgite surface to bond the carbon nano tubes,
step 5, ultrasonically dispersing the attapulgite clay suspension for 2 hours at the temperature of 90 ℃, standing for 20min, centrifuging for 4 times in a centrifuge, each time for 5 minutes, and filtering to recover solids;
step 6, drying the recovered solid for 24 hours at 100 ℃, and grinding the dried solid by using an agate mortar to obtain attapulgite/carbon nanotube absorbent powder with excellent wave-absorbing performance;
the composite modifier comprises an organic compound and a nonionic surfactant, wherein the volume ratio of the organic compound to the nonionic surfactant is 1:1.5, and the organic compound is stearic acid; the nonionic surfactant is an S80 type surfactant.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean 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 shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed.
Claims (8)
1. An attapulgite reinforced carbon nanotube wave-absorbing material is characterized by comprising the following raw materials in parts by weight:
20-25 parts of water-based epoxy AB glue, 25-30 parts of attapulgite/carbon nano tube wave absorbing agent powder, 2-5 parts of an active agent, 2-3 parts of a binder, 0.1-0.5 part of a defoaming agent and 30-40 parts of a diluent.
2. The attapulgite-reinforced carbon nanotube wave-absorbing material of claim 1, wherein the active agent is a polyethylene glycol octyl phenyl ether type nonionic surfactant.
3. The attapulgite-reinforced carbon nanotube wave-absorbing material of claim 1, wherein the adhesive is a mixed adhesive prepared by mixing polyvinyl butyral and sodium silicate hydrate in a ratio of 1:1.
4. The attapulgite-reinforced carbon nanotube wave-absorbing material according to claim 1, wherein the preparation method of the attapulgite/carbon nanotube wave-absorbing agent powder comprises the following steps:
step 1, weighing 100g of attapulgite clay with the fineness of 200-; adding 5-10ml of composite active agent into the treated suspension, then dropwise adding NaOH solution to adjust the pH value of the suspension to 6-8, stirring for 2-4 hours at 1500 rpm by using a cross stirring blade stirrer, standing for 10 hours, and separating the attapulgite clay suspension;
step 2, Dy (OC) 3 H 7 ) 3 And water according to a molar ratio of 1: 60-80 placing in reflux device, stirring at 70-80 deg.C for 2-4 hr to completely hydrolyze dysprosium isopropoxide, stirring hydrolyzed mixture DyO (OH) at 90 deg.C, and adding HNO 3 And Dy (OC) 3 H 7 ) 3 In a molar ratio of 0.05-0.07:1, adding HNO 3 Continuously stirring for 2 hours at the temperature of 60-85 ℃ to enable the solution to be colloidal;
step 3, putting 10g of carbon nano tube into a glass bottle, then adding 500ml of deionized water, adding 2-4ml of Triton X-100 nonionic surfactant, stirring in a constant-temperature water bath, keeping the rotating speed at 350-; slowly adding the sol into a system according to the volume ratio of 1:2, dropwise adding ammonia water, adjusting the pH value of the system to 9-10, ultrasonically mixing for 30 minutes at 50 ℃, standing and aging for 12 hours at 60 ℃, cooling to room temperature, washing for 3-5 times by using deionized water, and drying for 24 hours in a vacuum drying oven at 80 ℃; calcining the mixture for 1 hour in the atmosphere of 400-500 ℃ to obtain Dy wrapped on the surface 2 O 3 A particulate carbon nanotube;
step 4, adding 10-20g of carbon nano tubes into the separated attapulgite suspension, utilizing the adsorption property of the attapulgite surface to bond the carbon nano tubes,
step 5, ultrasonically dispersing the attapulgite clay suspension for 1-2h at the temperature of 70-90 ℃, standing for 10-20min, centrifuging for 2-5 times in a centrifuge, each time for 5 min, filtering and recovering solids;
and 6, drying the recovered solid at 70-100 ℃ for 24h, and grinding the dried solid with an agate mortar to obtain the attapulgite/carbon nanotube absorbent powder with excellent wave-absorbing performance.
5. A preparation method of a wave-absorbing material comprises the following steps:
step 1, pouring 20-25 parts of diluent into a stirrer, adding waterborne epoxy resin A glue into the diluent, and stirring;
step 2, adding 25-30 parts of attapulgite/carbon nanotube wave absorbing agent powder and 2-5 parts of active agent into the mixed system in the step 1 and stirring;
step 3, pouring the rest diluent into a stirrer, adding the waterborne epoxy resin B glue, 2-3 parts of adhesive and 0.1-0.5 part of defoaming agent into the stirrer, and putting the mixture into a cross stirring blade stirrer for fully stirring to prepare a component B for later use;
and 4, putting the components A and B into a container and stirring to prepare the wave-absorbing material.
6. The method for preparing the wave-absorbing material according to claim 5, wherein the active agent is polyethylene glycol octyl phenyl ether type nonionic surfactant.
7. A preparation method of the wave-absorbing material according to claim 5, wherein the adhesive is a mixed adhesive prepared by mixing polyvinyl butyral and sodium silicate hydrate according to a ratio of 1:1.
8. The preparation method of the wave-absorbing material according to claim 5, wherein the preparation method of the attapulgite/carbon nanotube wave-absorbing agent powder comprises the following steps:
step 1, weighing 100g of attapulgite clay with the fineness of 200-; adding 5-10ml of composite active agent into the treated suspension, then dropwise adding NaOH solution to adjust the pH value of the suspension to 6-8, stirring for 2-4 hours at 1500 rpm by using a cross stirring blade stirrer, standing for 10 hours, and separating the attapulgite clay suspension;
step 2, Dy (OC) 3 H 7 ) 3 The molar ratio of the water to the water is 1: 60-80 placing in reflux device, stirring at 70-80 deg.C for 2-4 hr to completely hydrolyze dysprosium isopropoxide, stirring hydrolyzed mixture DyO (OH) at 90 deg.C, and adding HNO 3 And Dy (OC) 3 H 7 ) 3 In a molar ratio of 0.05-0.07:1, adding HNO 3 Continuously stirring for 2 hours at the temperature of 60-85 ℃ to enable the solution to be colloidal;
step 3, putting 10g of carbon nano tube into a glass bottle, then adding 500ml of deionized water, adding 2-4ml of Triton X-100 nonionic surfactant, stirring in a constant-temperature water bath, keeping the rotating speed at 350-; slowly adding the sol into the system according to the volume ratio of 1:2, dropwise adding ammonia water, adjusting the pH value of the system to 9-10, ultrasonically mixing for 30 minutes at 50 ℃, standing and aging for 12 hours at 60 ℃, cooling to room temperature, washing for 3-5 times by using deionized water, and drying 2 in a vacuum drying oven at 80 DEG C4 h; calcining the mixture for 1 hour in the atmosphere of 400-500 ℃ to obtain Dy wrapped on the surface 2 O 3 A particulate carbon nanotube;
step 4, adding 10-20g of carbon nano tubes into the separated attapulgite suspension, and utilizing the adsorption property of the attapulgite surface to bond the carbon nano tubes;
step 5, ultrasonically dispersing the attapulgite clay suspension for 1-2h at the temperature of 70-90 ℃, standing for 10-20min, centrifuging for 2-5 times in a centrifuge, each time for 5 min, filtering and recovering solids;
and 6, drying the recovered solid for 24 hours at 70-100 ℃, and grinding the dried solid into powder by using an agate mortar, wherein the powder is the attapulgite/carbon nanotube absorbent.
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