CN104841397A - Stable-quality zirconia-loaded adsorbent and preparation method thereof - Google Patents

Abstract

The invention discloses a stable-quality zirconia-loaded adsorbent and a preparation method thereof. The stable-quality zirconia-loaded adsorbent is prepared from 90-100 parts by weight of straw, 0.4-1 part by weight of ammonium bicarbonate, 25-40 parts by weight of n-butyl titanate, 3-4 parts by weight of polyethylene glycol, 6-9 parts by weight of zirconia, 4-7 parts by weight of silicon carbide, 3-5 parts by weight of chitin, 0.4-1 part by weight of a silane coupling agent KH-550 and a proper amount of distilled water. The used zirconia improves adsorbent stability, high temperature resistance and adsorptivity, has a wide source and a low cost, is free of follow-up treatment and does not produce secondary pollution on the environment.

Description

A kind of stay-in-grade loaded zirconia adsorbent and preparation method thereof

Technical field

the present invention relates to a kind of absorbent fields, be specifically related to a kind of stay-in-grade loaded zirconia adsorbent and preparation method thereof.

Background technology

Stalk is an important biomass resource in production estimation system, and its content of cellulose is higher.Native cellulose is a kind of renewable resource and a kind of novel sorbing material, and it take native cellulose as matrix, has good hydrophily and loose structure, has wide material sources, renewable, degradable, environmental friendliness, the multiple advantage such as cheap.China is large agricultural country, has abundant stalk resource, accounts for the left and right of 25% of world's stalk resource, but it is still delayed to its disposal options at present, a large amount of stalk goes out of use in field or directly burns, and this had both caused the waste of a large amount of biomass energies, also brings serious pollution to environment.

Nano titanium oxide, as a kind of friendly photochemical catalyst, has good redox ability, is therefore widely used in the field such as sewage disposal, purification of air.But utilize various carrier to fix the photocatalysis effect of the adsorbent that nano titanium oxide is made in recent years and recovery utilization rate not high, zirconia chemical property torpescence, and the character of high-melting-point, high resistivity, high index of refraction and low thermal coefficient of expansion, make it become important exotic material, ceramic insulating material and ceramic opacifier.The present invention is intended to prepare a kind of cheapness, productive rate is high, less energy consumption, adsorption time are short, the simple adsorbent of preparation technology, and the zirconia of interpolation enhances the stability of adsorbent, heat-resisting quantity and adsorptivity, for the development of adsorbent lays the foundation.

Summary of the invention

The object of this invention is to provide a kind of stay-in-grade loaded zirconia adsorbent and preparation method thereof.

In order to realize object of the present invention, the present invention is by following scheme implementation:

A kind of stay-in-grade loaded zirconia adsorbent and preparation method thereof, is made up of the raw material of following weight portion: stalk 90-100, ammonium hydrogencarbonate 0.4-1, tetrabutyl titanate 25-40, polyethylene glycol 3-4, zirconia 6-9, carborundum 4-7, chitin 3-5, silane resin acceptor kh-550 0.4-1, distilled water are appropriate;

Stay-in-grade loaded zirconia adsorbent of one of the present invention and preparation method thereof, be made up of following concrete steps:

(1) stalk is first cleaned up with distilled water, ovendry power is added to after being broken to 8-20 order in the hydrochloric acid solution of 0.3mol/l and floods, flood and wash into neutral post-drying with distilled water after 1-2 days, again stalk and ammonium hydrogencarbonate mixing are added in Muffle furnace and heat up with the speed of 10 ~ 30 ° of C per minute, raised temperature is to 600-700 ° of C, constant temperature keeps 60-80min, naturally cools to room temperature;

(2) by even to zirconia, carborundum and silane resin acceptor kh-550 mixed grinding, again by the charing stalk mixing and stirring of mixture and chitin, polyethylene glycol, distilled water, step (1) gained, be heated to 50-60 ° of C, form slurry, for subsequent use after spraying dry;

(3) tetrabutyl titanate is added in the absolute ethyl alcohol of 3-4 times amount, the mixture of step (2) gained is added after stirring, accelerate to stir, in the process of stirring, slowly add the ethanol 70-100ml of 75%, regulate PH to 1-2 with nitric acid, after stirring 30min, still aging 1-2 days, places colloidal sol in an oven in 105 ° of C dryings, is ground into powder after drying, put into Muffle furnace, under 480-520 ° of C, calcine 4-6h.

Advantage of the present invention is: the present invention utilizes discarded straw for biomass carbon, achieve twice laid, the active carbon specific area of preparation is large, advantages of good adsorption effect, and utilize silane coupler and other to have adsorbing ground material, enhance the physisorption of material itself, and as the carrier of titanium dioxide, improve the photocatalytic activity of titanium dioxide, and recycle conveniently, increase economic efficiency, the zirconia that the present invention adds enhances the stability of adsorbent, heat-resisting quantity and adsorptivity, and wide material sources, with low cost, without the need to subsequent treatment, secondary pollution is not caused to environment.

Detailed description of the invention

Below by instantiation, the present invention is described in detail.

A kind of stay-in-grade loaded zirconia adsorbent and preparation method thereof, is made up of the raw material of following weight portion (kilogram): stalk 96, ammonium hydrogencarbonate 0.6, tetrabutyl titanate 33, polyethylene glycol 3, zirconia 7, carborundum 6, chitin 5, silane resin acceptor kh-550 0.5, distilled water are appropriate;

Stay-in-grade loaded zirconia adsorbent of one of the present invention and preparation method thereof, be made up of following concrete steps:

(1) stalk is first cleaned up with distilled water, ovendry power is added to after being broken to 8-20 order in the hydrochloric acid solution of 0.3mol/l and floods, flood and wash into neutral post-drying with distilled water after 1-2 days, again stalk and ammonium hydrogencarbonate mixing are added in Muffle furnace and heat up with the speed of 10 ~ 30 ° of C per minute, raised temperature is to 600-700 ° of C, constant temperature keeps 60-80min, naturally cools to room temperature;

(2) by even to zirconia, carborundum and silane resin acceptor kh-550 mixed grinding, again by the charing stalk mixing and stirring of mixture and chitin, polyethylene glycol, distilled water, step (1) gained, be heated to 50-60 ° of C, form slurry, for subsequent use after spraying dry;

(3) tetrabutyl titanate is added in the absolute ethyl alcohol of 3-4 times amount, the mixture of step (2) gained is added after stirring, accelerate to stir, in the process of stirring, slowly add the ethanol 80ml of 75%, regulate PH to 1-2 with nitric acid, after stirring 30min, still aging 1-2 days, places colloidal sol in an oven in 105 ° of C dryings, is ground into powder after drying, put into Muffle furnace, under 480-520 ° of C, calcine 4-6h.

After measured, the adsorbent capacity prepared by the present invention is 4.68mmol/g.

Claims (2)

1. stay-in-grade loaded zirconia adsorbent and preparation method thereof, it is characterized in that, be made up of the raw material of following weight portion: stalk 90-100, ammonium hydrogencarbonate 0.4-1, tetrabutyl titanate 25-40, polyethylene glycol 3-4, zirconia 6-9, carborundum 4-7, chitin 3-5, silane resin acceptor kh-550 0.4-1, distilled water are appropriate.

2. a kind of stay-in-grade loaded zirconia adsorbent and preparation method thereof according to claim 1, is characterized in that, be made up of following concrete steps:

(1) stalk is first cleaned up with distilled water, ovendry power is added to after being broken to 8-20 order in the hydrochloric acid solution of 0.3mol/l and floods, flood and wash into neutral post-drying with distilled water after 1-2 days, again stalk and ammonium hydrogencarbonate mixing are added in Muffle furnace and heat up with the speed of 10 ~ 30 ° of C per minute, raised temperature is to 600-700 ° of C, constant temperature keeps 60-80min, naturally cools to room temperature;

(2) by even to zirconia, carborundum and silane resin acceptor kh-550 mixed grinding, again by the charing stalk mixing and stirring of mixture and chitin, polyethylene glycol, distilled water, step (1) gained, be heated to 50-60 ° of C, form slurry, for subsequent use after spraying dry;

(3) tetrabutyl titanate is added in the absolute ethyl alcohol of 3-4 times amount, the mixture of step (2) gained is added after stirring, accelerate to stir, in the process of stirring, slowly add the ethanol 70-100ml of 75%, regulate PH to 1-2 with nitric acid, after stirring 30min, still aging 1-2 days, places colloidal sol in an oven in 105 ° of C dryings, is ground into powder after drying, put into Muffle furnace, under 480-520 ° of C, calcine 4-6h.