CN113755132A - Preparation method of hydroxyapatite/carbon composite particles with strong absorption of mid-infrared light - Google Patents
Preparation method of hydroxyapatite/carbon composite particles with strong absorption of mid-infrared light Download PDFInfo
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Abstract
A preparation method of hydroxyapatite/carbon composite particles with strong absorption of mid-infrared light belongs to the technical field of functional material preparation. Firstly, preparing an aqueous solution containing calcium hydroxide and citric acid, slowly dripping the aqueous solution containing phosphoric acid until the pH value of the reaction solution is reduced to 10, and washing the reaction solution by using an ammonium chloride aqueous solution to prepare a colloidal solution; adding beta-cyclodextrin and potassium dihydrogen phosphate, treating at 140 ℃ for 3.5 hours, adding methylene blue and glucose, treating at 140-180 ℃ for 4 hours, washing and drying precipitates to obtain the hydroxyapatite/carbon composite particles. The method has simple preparation process, the prepared hydroxyapatite/carbon composite particles are easily suitable for subsequent processes such as spraying, spin coating, composite material filling modification and the like, and the absorption capacity in the mid-infrared region can be regulated and controlled by changing the preparation process conditions so as to meet the requirements of different application fields.
Description
Technical Field
A preparation method of hydroxyapatite/carbon composite particles with strong absorption of mid-infrared light belongs to the technical field of functional material preparation.
Background
When infrared radiation of an object passes through the atmosphere, water vapor and CO contained in the atmosphere2Etc. will attenuate the radiation in the partial band, butThe other 4 bands with higher transmittance are called atmospheric windows, which are respectively: near infrared (0.75-2.7 microns), mid infrared (3-5 microns), far infrared (8-14 microns) and ultra far infrared (50-1000 microns). Most of organic and inorganic substances have fundamental frequency absorption bands in an infrared region of 2-20 microns, and the mid-infrared technology has wide application value in the fields of environmental monitoring, pollution control, night infrared scanning imaging, national defense stealth technology and the like, and is particularly important for researching and developing infrared absorption materials or wave-absorbing materials.
The infrared stealth technology is to reduce or change the infrared radiation signal of the target to reduce the detectability of the target, and the essence of the infrared stealth is to weaken the radiation characteristics such as energy, frequency band, heat source and direction through various technical measures, reduce the infrared radiation difference between the target and the background, make the detector not receive enough energy, and thus reduce the probability of the target being discovered. The main working wave bands of the infrared detector are 3-5 micrometers and 8-14 micrometers, so that the infrared detector is an absorption material with a good absorption effect on infrared light with a specific wavelength, can reduce target radiation signals, and can play a beneficial effect in the aspect of infrared stealth technology.
The literatures "preparation of mesoporous carbon-metal nanocomposite and radar/infrared stealth characteristics" (doctor's paper of Nanjing aerospace university, 2010), "development of several low-emissivity infrared stealth materials" (Master of Harbin Industrial university, 2007) mention the related technologies of infrared stealth coating and binder, and the selected materials include metal powders such as aluminum powder, silver powder, copper powder and reduced iron powder, and also semiconductor materials including tin-doped indium oxide, aluminum-doped zinc oxide and titanium dioxide/titanium nitride, and exhibit good infrared stealth capability. The document "Pine D J. Self Assembly of Low-Emissivity Materials (SALEM). 2000" reports that Japanese scholars dope inorganic phosphate into scaly aluminum to obtain a thin film with Low infrared Emissivity, and the thin film has good wave-absorbing performance at 10.6 microns. The document "precise measurement of profile in antenna housing and technical research of coping process" (doctor of university, etc. of university of japan, 2004) mentions that germany, etc., is, etc., has used in a material, in a coating, it, can realize that it is a material, when the coating, can realize the coating, can be stealthy, when the coating, it is, can realize the infrared stealthy.
Document "Effect of heat treatment on induced reflection property of Al-doped ZnO films" (Solar Energy Materials)& Solar Cells，127(2014)163-168）、“Preparation, characterization and infrared emissivity study of helical polyurethane@SiO2core-shell composition (Applied Surface Science 256 (2009) 1404-1408) and "Preparation, characterization, and enhanced emissive property of optical active polyurethane/TiO2/SiO2multilayered microspheres (Journal of Solid State Chemistry 184 (2011) 2617-2622) refers to the research of infrared wave-absorbing materials, and the main research focuses on aluminum-doped ZnO and SiO2And TiO2Etc. to oxidize the semiconductor material. However, no research on the strong absorption capacity of the hydroxyapatite/carbon composite particles in the mid-infrared region is reported.
Disclosure of Invention
One object of the present invention is to provide a method for preparing hydroxyapatite/carbon composite particles having strong absorption of mid-infrared light, which is characterized by comprising the following steps:
(1) preparing 100 ml of aqueous solution containing 5.00 g of calcium hydroxide and 1.00 g of citric acid, slowly dripping 4wt.% of phosphoric acid aqueous solution, stopping dripping when the pH value of the reaction solution is reduced to 10, continuously stirring for 2 hours, standing, aging for 12 hours, then performing centrifugal separation, collecting precipitate, dispersing the precipitate into 100 ml of water, dripping 100 ml of aqueous solution containing 4wt.% of ammonium chloride, stirring for 15 minutes, performing centrifugal separation, collecting precipitate, and re-dispersing the precipitate into 200 ml of aqueous solution to prepare hydroxyapatite colloidal solution;
(2) adding 3.66 g of beta-cyclodextrin and 0.91 g of monopotassium phosphate into the hydroxyapatite colloidal solution prepared in the step (1), putting the reaction solution into a hydrothermal reaction kettle, carrying out hydrothermal treatment at 140 ℃ for 3.5 hours, and cooling to obtain a cyclodextrin modified hydroxyapatite colloidal solution;
(3) adding 1.00 g of methylene blue into the cyclodextrin modified hydroxyapatite colloidal solution prepared in the step (2), stirring for 2 hours, adding 9.90-99 g of glucose, stirring for 15 minutes, putting the reaction solution into a hydrothermal reaction kettle, carrying out hydrothermal treatment at 140-180 ℃ for 4 hours, cooling after the reaction is finished, carrying out centrifugal separation, collecting precipitates, washing with ethanol and deionized water twice respectively, and finally drying the collected colloid at 80 ℃ for 12 hours to obtain the hydroxyapatite/carbon composite particles.
The preparation method comprises the steps of taking calcium hydroxide as a calcium source and phosphoric acid as a phosphorus source, preparing citric acid modified hydroxyapatite by a chemical precipitation method, grafting cyclodextrin in a hydrothermal reaction at 140 ℃, and depositing a carbon shell on the surface of the hydroxyapatite by utilizing intermolecular dehydration and crosslinking reactions of glucose molecules to prepare the hydroxyapatite/carbon composite particles, so that the particles have strong absorption performance in a middle infrared region. The hydroxyapatite/carbon composite particles with different mid-infrared wave absorption capacities are prepared by changing the adding amount of glucose in the reaction solution and the hydrothermal treatment temperature.
The invention has the beneficial effects that:
1. the preparation process adopted by the method is simple, the device is simple, the price of the reagent is low, and the industrial production is easy to realize;
2. the hydroxyapatite/carbon composite particles prepared by the method have small particle size and light specific gravity, have high adaptability to construction methods in subsequent application, and can be suitable for processes such as spraying, spin coating, composite material filling modification and the like;
3. the absorption capacity of the hydroxyapatite/carbon composite particles prepared by the method in the mid-infrared region, especially in the range of 3-5 mu m, can be regulated and controlled by changing the preparation process conditions so as to meet the requirements of different mid-infrared absorption application fields.
Drawings
Fig. 1 is an infrared absorption spectrum of hydroxyapatite/carbon composite particles prepared in example 1 of the present invention.
Fig. 2 is an infrared absorption spectrum of the hydroxyapatite/carbon composite particle prepared in example 2 of the present invention.
Fig. 3 is an infrared absorption spectrum of the hydroxyapatite/carbon composite particle prepared in example 3 of the present invention.
Fig. 4 is an infrared absorption spectrum of the hydroxyapatite/carbon composite particle prepared in example 4 of the present invention.
Fig. 5 is an infrared absorption spectrum of the hydroxyapatite/carbon composite particle prepared in comparative example 1 of the present invention.
Detailed Description
Example 1
(1) Preparing 100 ml of aqueous solution containing 5.00 g of calcium hydroxide and 1.00 g of citric acid, slowly dripping 4wt.% of phosphoric acid aqueous solution, stopping dripping when the pH value of the reaction solution is reduced to 10, continuously stirring for 2 hours, standing, aging for 12 hours, then performing centrifugal separation, collecting precipitate, dispersing the precipitate into 100 ml of water, dripping 100 ml of aqueous solution containing 4wt.% of ammonium chloride, stirring for 15 minutes, performing centrifugal separation, collecting precipitate, and re-dispersing the precipitate into 200 ml of aqueous solution to prepare hydroxyapatite colloidal solution;
(2) adding 3.66 g of beta-cyclodextrin and 0.91 g of monopotassium phosphate into the hydroxyapatite colloidal solution prepared in the step (1), putting the reaction solution into a hydrothermal reaction kettle, carrying out hydrothermal treatment at 140 ℃ for 3.5 hours, and cooling to obtain a cyclodextrin modified hydroxyapatite colloidal solution;
(3) adding 1.00 g of methylene blue into the cyclodextrin modified hydroxyapatite colloidal solution prepared in the step (2), stirring for 2 hours, adding 9.90 g of glucose, stirring for 15 minutes, putting the reaction solution into a hydrothermal reaction kettle, carrying out hydrothermal treatment at 180 ℃ for 4 hours, cooling after the reaction is finished, carrying out centrifugal separation, collecting precipitates, washing with ethanol and deionized water twice respectively, and finally drying the collected colloid at 80 ℃ for 12 hours to obtain the hydroxyapatite/carbon composite particles.
Example 2
(1) Preparing 100 ml of aqueous solution containing 5.00 g of calcium hydroxide and 1.00 g of citric acid, slowly dripping 4wt.% of phosphoric acid aqueous solution, stopping dripping when the pH value of the reaction solution is reduced to 10, continuously stirring for 2 hours, standing, aging for 12 hours, then performing centrifugal separation, collecting precipitate, dispersing the precipitate into 100 ml of water, dripping 100 ml of aqueous solution containing 4wt.% of ammonium chloride, stirring for 15 minutes, performing centrifugal separation, collecting precipitate, and re-dispersing the precipitate into 200 ml of aqueous solution to prepare hydroxyapatite colloidal solution;
(2) adding 3.66 g of beta-cyclodextrin and 0.91 g of monopotassium phosphate into the hydroxyapatite colloidal solution prepared in the step (1), putting the reaction solution into a hydrothermal reaction kettle, carrying out hydrothermal treatment at 140 ℃ for 3.5 hours, and cooling to obtain a cyclodextrin modified hydroxyapatite colloidal solution;
(3) adding 1.00 g of methylene blue into the cyclodextrin modified hydroxyapatite colloidal solution prepared in the step (2), stirring for 2 hours, adding 19.8 g of glucose, stirring for 15 minutes, putting the reaction solution into a hydrothermal reaction kettle, carrying out hydrothermal treatment at 180 ℃ for 4 hours, cooling after the reaction is finished, carrying out centrifugal separation, collecting precipitates, washing with ethanol and deionized water twice respectively, and finally drying the collected colloid at 80 ℃ for 12 hours to obtain the hydroxyapatite/carbon composite particles.
Example 3
(1) Preparing 100 ml of aqueous solution containing 5.00 g of calcium hydroxide and 1.00 g of citric acid, slowly dripping 4wt.% of phosphoric acid aqueous solution, stopping dripping when the pH value of the reaction solution is reduced to 10, continuously stirring for 2 hours, standing, aging for 12 hours, then performing centrifugal separation, collecting precipitate, dispersing the precipitate into 100 ml of water, dripping 100 ml of aqueous solution containing 4wt.% of ammonium chloride, stirring for 15 minutes, performing centrifugal separation, collecting precipitate, and re-dispersing the precipitate into 200 ml of aqueous solution to prepare hydroxyapatite colloidal solution;
(2) adding 3.66 g of beta-cyclodextrin and 0.91 g of monopotassium phosphate into the hydroxyapatite colloidal solution prepared in the step (1), putting the reaction solution into a hydrothermal reaction kettle, carrying out hydrothermal treatment at 140 ℃ for 3.5 hours, and cooling to obtain a cyclodextrin modified hydroxyapatite colloidal solution;
(3) adding 1.00 g of methylene blue into the cyclodextrin modified hydroxyapatite colloidal solution prepared in the step (2), stirring for 2 hours, adding 99 g of glucose, stirring for 15 minutes, putting the reaction solution into a hydrothermal reaction kettle, carrying out hydrothermal treatment at 180 ℃ for 4 hours, cooling after the reaction is finished, carrying out centrifugal separation, collecting precipitates, washing with ethanol and deionized water twice respectively, and finally drying the collected colloids at 80 ℃ for 12 hours to obtain the hydroxyapatite/carbon composite particles.
Example 4
(1) Preparing 100 ml of aqueous solution containing 5.00 g of calcium hydroxide and 1.00 g of citric acid, slowly dripping 4wt.% of phosphoric acid aqueous solution, stopping dripping when the pH value of the reaction solution is reduced to 10, continuously stirring for 2 hours, standing, aging for 12 hours, then performing centrifugal separation, collecting precipitate, dispersing the precipitate into 100 ml of water, dripping 100 ml of aqueous solution containing 4wt.% of ammonium chloride, stirring for 15 minutes, performing centrifugal separation, collecting precipitate, and re-dispersing the precipitate into 200 ml of aqueous solution to prepare hydroxyapatite colloidal solution;
(2) adding 3.66 g of beta-cyclodextrin and 0.91 g of monopotassium phosphate into the hydroxyapatite colloidal solution prepared in the step (1), putting the reaction solution into a hydrothermal reaction kettle, carrying out hydrothermal treatment at 140 ℃ for 3.5 hours, and cooling to obtain a cyclodextrin modified hydroxyapatite colloidal solution;
(3) adding 1.00 g of methylene blue into the cyclodextrin modified hydroxyapatite colloidal solution prepared in the step (2), stirring for 2 hours, adding 9.90 g of glucose, stirring for 15 minutes, putting the reaction solution into a hydrothermal reaction kettle, carrying out hydrothermal treatment at 140 ℃ for 4 hours, cooling after the reaction is finished, carrying out centrifugal separation, collecting precipitates, washing with ethanol and deionized water twice respectively, and finally drying the collected colloid at 80 ℃ for 12 hours to obtain the hydroxyapatite/carbon composite particles.
Comparative example 1
(1) Preparing 100 ml of aqueous solution containing 5.00 g of calcium hydroxide and 1.00 g of citric acid, slowly dripping 4wt.% of phosphoric acid aqueous solution, stopping dripping when the pH value of the reaction solution is reduced to 10, continuously stirring for 2 hours, standing, aging for 12 hours, then performing centrifugal separation, collecting precipitate, dispersing the precipitate into 100 ml of water, dripping 100 ml of aqueous solution containing 4wt.% of ammonium chloride, stirring for 15 minutes, performing centrifugal separation, collecting precipitate, and re-dispersing the precipitate into 200 ml of aqueous solution to prepare hydroxyapatite colloidal solution;
(2) adding 1.00 g of methylene blue into the hydroxyapatite colloidal solution prepared in the step (1), stirring for 2 hours, adding 9.90 g of glucose, stirring for 15 minutes, putting the reaction solution into a hydrothermal reaction kettle, carrying out hydrothermal treatment at 180 ℃ for 4 hours, after the reaction is finished, cooling, carrying out centrifugal separation, collecting precipitates, washing with ethanol and deionized water twice respectively, and finally drying the collected colloid at 80 ℃ for 12 hours to obtain the hydroxyapatite/carbon composite particles.
Claims (1)
1. The preparation method of the hydroxyapatite/carbon composite particles with strong absorption of mid-infrared light is characterized by comprising the following steps:
(1) preparing 100 ml of aqueous solution containing 5.00 g of calcium hydroxide and 1.00 g of citric acid, slowly dripping 4wt.% of phosphoric acid aqueous solution, stopping dripping when the pH value of the reaction solution is reduced to 10, continuously stirring for 2 hours, standing, aging for 12 hours, then performing centrifugal separation, collecting precipitate, dispersing the precipitate into 100 ml of water, dripping 100 ml of aqueous solution containing 4wt.% of ammonium chloride, stirring for 15 minutes, performing centrifugal separation, collecting precipitate, and re-dispersing the precipitate into 200 ml of aqueous solution to prepare hydroxyapatite colloidal solution;
(2) adding 3.66 g of beta-cyclodextrin and 0.91 g of monopotassium phosphate into the hydroxyapatite colloidal solution prepared in the step (1), putting the reaction solution into a hydrothermal reaction kettle, carrying out hydrothermal treatment at 140 ℃ for 3.5 hours, and cooling to obtain a cyclodextrin modified hydroxyapatite colloidal solution;
(3) adding 1.00 g of methylene blue into the cyclodextrin modified hydroxyapatite colloidal solution prepared in the step (2), stirring for 2 hours, adding 9.90-99 g of glucose, stirring for 15 minutes, putting the reaction solution into a hydrothermal reaction kettle, carrying out hydrothermal treatment at 140-180 ℃ for 4 hours, cooling after the reaction is finished, carrying out centrifugal separation, collecting precipitates, washing with ethanol and deionized water twice respectively, and finally drying the collected colloid at 80 ℃ for 12 hours to obtain the hydroxyapatite/carbon composite particles.
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030157014A1 (en) * | 2000-04-27 | 2003-08-21 | Qing Wang | Pyrolyzed hard carbon material, preparation and its applications |
| US20050226939A1 (en) * | 2004-04-07 | 2005-10-13 | National University Of Singapore | Production of nano-sized hydroxyapatite particles |
| CN106215958A (en) * | 2016-07-22 | 2016-12-14 | 中北大学 | A kind of preparation method of the catalysis material of reusable edible |
| CN106389342A (en) * | 2016-09-20 | 2017-02-15 | 山东理工大学 | Preparation method of hydroxyapatite/tannic acid composite particle capable of adjusting and controlling release speed of methylene blue monomer |
| CN106800931A (en) * | 2017-01-10 | 2017-06-06 | 中北大学 | Carbon point/hydroxyapatite composite fluorescence powder one-step synthesis |
| CN107022207A (en) * | 2017-04-24 | 2017-08-08 | 山东理工大学 | A kind of preparation method of hydroxyapatite@ferric tannates/titanium dioxide viridine green containing methylene blue |
Non-Patent Citations (1)
| Title |
|---|
| WEIWEI HUANG，等: "Citric acid-crosslinked β-cyclodextrin for simultaneous removal of bisphenol A, methylene blue and copper: The roles of cavity and surface functional groups" * |
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