CN103736441A - Method for removing ethene in carbon dioxide by zinc oxide nanorods array purifying system - Google Patents

Method for removing ethene in carbon dioxide by zinc oxide nanorods array purifying system Download PDF

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CN103736441A
CN103736441A CN201310690940.3A CN201310690940A CN103736441A CN 103736441 A CN103736441 A CN 103736441A CN 201310690940 A CN201310690940 A CN 201310690940A CN 103736441 A CN103736441 A CN 103736441A
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zinc
carbon dioxide
preparation
column array
oxide nano
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CN103736441B (en
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金向华
孙猛
李荷庆
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Jinhong Gas Co ltd
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Suzhou Jinhong Gas Co Ltd
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    • Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00—Capture or disposal of greenhouse gases
    • Y02C20/40—Capture or disposal of greenhouse gases of CO2
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

The invention discloses a method for removing ethene in carbon dioxide by zinc oxide nanorods array purifying system. The method is characterized in that a zinc oxide nanorods array is prepared on a substrate by a solution synthesis method, the zinc oxide nanorods array and the substrate are firmly combined, and a plurality of substrates are arranged in a purifier for compositing the purifying system. The method has the advantages that the process is simple, the reaction temperature is low, no size restriction is generated, the cost is low, the purifying system has good ethene adsorption performance, the purifying degree is high, the adsorption quantity is large, and the selectivity is good.

Description

Remove the method for the zinc-oxide nano column array purification system of ethene in carbon dioxide
Technical field
The present invention relates to carbon dioxide recovery technical field, the purification system that especially relates to a kind of substrate composition of preparing depositing zinc oxide nano column array can be used for removing in carbon dioxide recovery technique the new method of ethene.
Background technology
Carbon dioxide is a kind of resource of preciousness, can be widely used in multiple fields: the industries such as chemical synthesis industry, mechanical protection welding, metal casting processing, agricultural fertilizer, fruit and vegetable using is fresh-keeping, beer beverage is filling, oil exploitation, fire-fighting fire extinguishing, medical and health all need great amount of carbon dioxide.The source of China's carbon dioxide is very abundant, but because the measure of recovery carbon dioxide is unfavorable, the carbon dioxide of annual recycling also not enough discharge capacity 2%, in world wide, be discharged into every year the nearly 20,000,000,000 tons of left and right of carbon dioxide in atmosphere, both caused the pollution of atmosphere, form fearful greenhouse effects, wasted again valuable resource.
In recent years along with the developing rapidly of industry, carbon dioxide consumption figure increase year after year and the production of carbon dioxide is often subject to resource limitation, therefore carbon dioxide product is always in the state that supply falls short of demand.
Ethylene is prepared a large amount of carbon dioxide of by-product in the production process of oxirane, makes full use of this part carbon resource, and carbon dioxide is refined to purification, has both reduced a large amount of pollutions, increases again the economic benefit of enterprise.
But ethylene is understood residual fraction ethene in carbon dioxide tail gas after preparing oxirane, causes carbon dioxide purification difficulty.
The separation of impurities in carbon dioxide gas in the past mainly adopts Production by Catalytic Combustion Process, under the effect of catalyst, the organic compound combustion in unstripped gas is generated to water and carbon dioxide.First Production by Catalytic Combustion Process will build the device of a set of cryogenic air separation method production liquid oxygen, pure oxygen is joined in the carbon dioxide that has 96% purity, mix with it, then all gas is heated to 350 ℃, enter in catalytic burner, by excessive oxygen effect, a small amount of organic impurities is burnt.The all gas generating cools to 20 ℃ of left and right again, enters supercharging in compressor after voltage stabilizing, through molecular sieve drying dehydration, and adsorption-edulcoration matter, then enter in rectifying column and remove the excessive oxygen adding after liquefaction, at the bottom of tower, can obtain liquid carbon dioxide product.
Production by Catalytic Combustion Process totally than absorption distillation fado a set of liquid oxygen production device and combustion heating cooling system, complicated one times than absorption distillation method of flow process, brings the operation of air liquefaction and catalysis intensification temperature-fall period to bother manyfold than absorption distillation.In addition, the absorbed portion of absorption distillation method operates under normal temperature condition, and the liquid oxygen production system of Production by Catalytic Combustion Process will be air liquefaction, consume mass energy, and the production cost of absorption distillation method is lower.
But the purifier of absorption distillation method adopted molecular sieve to carry out purifying to foreign gas in the past, and purifying is limited in one's ability.This patent is changed the structure of traditional purifier, adopts more effective purified material, has strengthened the adsorption capacity of ethene, and this purification system has good ethylene absorption performance, and purification degrees is high, and adsorbance is large, selectively good.
Summary of the invention
Goal of the invention of the present invention is the shortcoming in order to overcome above-mentioned background technology, provide a kind of synthetic method of solution of utilizing on substrate, to prepare zinc-oxide nano column array, and multiple substrates are arranged in to composition purification system in purifier, then remove the method for ethene in carbon dioxide.
Technical scheme of the present invention is: a kind of system is for the preparation of the method for removing the zinc-oxide nano column array purification system of ethene in carbon dioxide, the method is mainly divided into three steps, be respectively preparation, zinc-oxide nano column array preparation, substrate installation, concrete technology step is as follows:
Step 1, preparation:
First prepare various raw material, and prepare the solution of each proportioning.
Deionized water;
Absolute ethyl alcohol, purity is greater than 99.5%;
Zinc acetate, Zn (CH 3cOO) 22H 2o, the powder of content >99.8%;
Lithium hydroxide, LiOHH 2o, the powder of content >99.7%;
Zinc nitrate, Zn (NO 3) 26H 2o, the powder of content >99.5%;
Ammoniacal liquor, NH 3h 2o, NH 3the solution of content >25%;
Constant temperature water bath, temperature control scope room temperature～300 ℃, 0.1/0.01 ℃ of temperature-controlled precision;
Spin coater, 300-10000 revs/min of revolutions;
Sintering furnace, temperature control scope room temperature～1200 ℃;
Step 2, zinc-oxide nano column array preparation:
(1) by Zn (CH 3cOO) 22H 2o solution is added in appropriate absolute ethyl alcohol, then adds hot reflux 0.5h, naturally cooling;
(2) add again a certain amount of LiOHH 2o, ultrasonic reaction 1 h can obtain stable ZnO colloidal sol;
(3), after prepared by colloidal sol, utilize czochralski method, spin-coating method to prepare layer of ZnO membrana granulosa at substrate surface;
(4) by high temperature heat treatment 2h of ZnO membrana granulosa, standby;
(5) under normal temperature by Zn (NO 3) 26H 2o is dissolved in deionized water, then adds excessive ammonia, and on magnetic stirring apparatus, stir, and add appropriate copper, manganese, zinc, platinum, the slaine of the elements such as titanium carries out modification as active component to ZnO nano post array, and it is standby that this solution is made reactant liquor;
(6) substrate of above-mentioned deposited monolayers ZnO membrana granulosa is vertically put into the reactant liquor preparing;
(7) in water bath with thermostatic control, react 2 h and on substrate, prepared oldered array;
(8) at high temperature heat treatment of oldered array 2 h obtain ZnO nano post array;
(9) utilize above-mentioned steps making ZnO nano column array on multiple substrates;
Step 3, substrate is installed:
In purifier inside, substrate is arranged above and below, wherein first substrate right side connects purifying wall, vacancy is left in left side, and second substrate left side connects purifying wall, and vacancy is left on right side, arrange so successively until fill purifier inside, composition zinc-oxide nano column array purification system.
Zn (CH in described step 2 3cOO) 22H 2o and absolute ethyl alcohol mixed proportion are n (Zn (CH 3cOO) 22H 2o)/n (C 2h 5oH) between 0.001 to 0.003.
Zn (CH in described step 2 3cOO) 22H 2o and absolute ethyl alcohol add hot reflux minimum temperature after mixing is 60 ℃, and maximum temperature is 80 ℃.
LiOHH in described step 2 2the amount that O adds and Zn (CH 3cOO) 22H 2the ratio of O is n (Zn (CH 3cOO) 22H 2o)/n (LiOHH 2o) between 0.5 to 0.9.
Zn (NO in described step 2 3) 26H 2the mixed proportion that O joins ammonia neutralization ammoniacal liquor is n (NH 3h 2o)/n (Zn (NO 3) 26H 2o) between 2.5 to 5.
In described step 2 the water-bath temperature of zinc-oxide nano column array minimum be 65 ℃, be up to 95 ℃.
In described step 2 the heat treatment temperature of zinc-oxide nano column array minimum be 350 ℃, be up to 500 ℃.
The invention has the beneficial effects as follows: it is simple that this preparation method has technique, and reaction temperature is low, be not subject to size restrictions, cost is low, and purification system has good ethylene absorption performance, and purification degrees is high, and adsorbance is large, selectively good.
Accompanying drawing explanation
Fig. 1 is purifier internal base plate mounting structure schematic diagram of the present invention;
Wherein: 1, substrate, 2, air inlet, 3, gas outlet.
The specific embodiment
The present embodiment is a kind of method for the preparation of removing the zinc-oxide nano column array purification system of ethene in carbon dioxide, the method is mainly divided into three steps, be respectively preparation, zinc-oxide nano column array preparation, substrate installation, concrete technology step is as follows:
Step 1, preparation:
First prepare various raw material, and prepare the solution of each proportioning.
Deionized water;
Absolute ethyl alcohol, purity is greater than 99.5%;
Zinc acetate, Zn (CH 3cOO) 22H 2o, the powder of content >99.8%;
Lithium hydroxide, LiOHH 2o, the powder of content >99.7%;
Zinc nitrate, Zn (NO 3) 26H 2o, the powder of content >99.5%;
Ammoniacal liquor, NH 3h 2o, NH 3the solution of content >25%;
Constant temperature water bath, temperature control scope room temperature～300 ℃, 0.1/0.01 ℃ of temperature-controlled precision;
Spin coater, 300-10000 revs/min of revolutions;
Sintering furnace, temperature control scope room temperature～1200 ℃;
Step 2, zinc-oxide nano column array preparation:
(1) by Zn (CH 3cOO) 22H 2o solution is added in appropriate absolute ethyl alcohol, Zn (CH 3cOO) 22H 2o and absolute ethyl alcohol mixed proportion are n (Zn (CH 3cOO) 22H 2o)/n (C 2h 5oH) between 0.001 to 0.003, then add hot reflux 0.5h, the minimum temperature that adds hot reflux after mixing is 60 ℃, maximum temperature is 80 ℃, finally carries out nature cooling again;
(2) add again a certain amount of LiOHH 2o, LiOHH 2o and Zn (CH 3cOO) 22H 2the ratio of O is n (Zn (CH 3cOO) 22H 2o)/n (LiOHH 2o), between 0.5 to 0.9, ultrasonic reaction 1 h can obtain stable ZnO colloidal sol;
(3), after prepared by colloidal sol, utilize czochralski method, spin-coating method to prepare layer of ZnO membrana granulosa at substrate surface;
(4) by high temperature heat treatment 2h of ZnO membrana granulosa, standby;
(5) under normal temperature by Zn (NO 3) 26H 2o is dissolved in deionized water, then adds excessive ammonia, Zn (NO 3) 26H 2the mixed proportion that O joins ammonia neutralization ammoniacal liquor is n (NH 3h 2o)/n (Zn (NO 3) 26H 2o) between 2.5 to 5, on magnetic stirring apparatus, stir, and add appropriate copper, manganese, zinc, platinum, the slaine of the elements such as titanium carries out modification as active component to ZnO nano post array, and it is standby that this solution is made reactant liquor;
(6) substrate of above-mentioned deposited monolayers ZnO membrana granulosa is vertically put into the reactant liquor preparing;
(7) minimum be 65 ℃, be up to and in 95 ℃ of waters bath with thermostatic control, react 2 h and on substrate, prepared oldered array;
(8) oldered array minimum be 350 ℃, be up to heat treatment 2 h under 500 ℃ of high temperature and obtain ZnO nano post array;
(9) utilize above-mentioned steps making ZnO nano column array on multiple substrates;
Step 3, substrate is installed:
As shown in Figure 1, in purifier inside, substrate is arranged above and below, wherein first substrate right side connects purifying wall, vacancy is left in left side, and second substrate left side connects purifying wall, and vacancy is left on right side, arrange so successively until fill purifier inside, composition zinc-oxide nano column array purification system.
Enumerate two most preferred embodiment explanation the inventive method below:
Embodiment 1:
1) Zn (CH 3cOO) 22H 2o is added in appropriate absolute ethyl alcohol, n (Zn (CH 3cOO) 22H 2o)/n (C 2h 5oH) mixed proportion is 0.001, then at the temperature of 60-80 ℃, adds hot reflux 0.5h, naturally cooling;
2) add again a certain amount of LiOHH 2o, n (Zn (CH 3cOO) 22H 2o)/n (LiOHH 2o) mixed proportion is 0.6, and ultrasonic reaction 1 h can obtain the ZnO colloidal sol of stable homogeneous;
3), after prepared by colloidal sol, utilize czochralski method to prepare layer of ZnO membrana granulosa at substrate surface;
4) by high temperature heat treatment 2h of ZnO membrana granulosa, standby;
5) under normal temperature by Zn (NO 3) 26H 2o is dissolved in deionized water, then adds excessive ammonia, n (NH 3h 2o)/n (Zn (NO 3) 26H 2o) mixed proportion is 3, stirs, and add appropriate copper chloride, as active component, ZnO nano post array is carried out to modification on magnetic stirring apparatus, and it is standby that this solution is made reactant liquor;
6) substrate of above-mentioned deposited monolayers ZnO membrana granulosa is vertically put into the reactant liquor preparing;
7) in the water bath with thermostatic control of 70 ℃, react 2 h and on substrate, prepared oldered array;
8) oldered array heat treatment 2 h under the high temperature of 400 ℃ obtain ZnO nano post array;
9) utilize similar method making ZnO nano column array on multiple substrates;
10) then multiple substrates are arranged in and in purifier, form purification system according to the pattern shown in Fig. 1.
Embodiment 2:
1) by Zn (CH 3cOO) 22H 2o is added in appropriate absolute ethyl alcohol, n (Zn (CH 3cOO) 22H 2o)/n (C 2h 5oH) mixed proportion is 0.002, then at the temperature of 60-80 ℃, adds hot reflux 0.5h, naturally cooling;
2) add again a certain amount of LiOHH 2o, n (Zn (CH 3cOO) 22H 2o)/n (LiOHH 2o) mixed proportion is 0.7, and ultrasonic reaction 1 h can obtain the ZnO colloidal sol of stable homogeneous;
3), after prepared by colloidal sol, utilize spin-coating method to prepare layer of ZnO membrana granulosa at substrate surface;
4) by high temperature heat treatment 2h of ZnO membrana granulosa, standby;
5) under normal temperature by Zn (NO 3) 26H 2o is dissolved in deionized water, then adds excessive ammonia, n (NH 3h 2o)/n (Zn (NO 3) 26H 2o) mixed proportion is 4, stirs, and add appropriate copper chloride, as active component, ZnO nano post array is carried out to modification on magnetic stirring apparatus, and it is standby that this solution is made reactant liquor;
6) substrate of above-mentioned deposited monolayers ZnO membrana granulosa is vertically put into the reactant liquor preparing;
7) in the water bath with thermostatic control of 80 ℃, react 2 h and on substrate, prepared oldered array;
8) oldered array heat treatment 2 h under the high temperature of 500 ℃ obtain ZnO nano post array;
9) utilize similar method making ZnO nano column array on multiple substrates;
10) then multiple substrates are arranged in and in purifier, form purification system according to the pattern shown in Fig. 1.

Claims (7)

1. one kind is characterized in that for the preparation of the method for removing the zinc-oxide nano column array purification system of ethene in carbon dioxide the method is mainly divided into three steps, be respectively preparation, zinc-oxide nano column array preparation, substrate installation, concrete technology step is as follows:
Step 1, preparation:
First prepare various raw material, and prepare the solution of each proportioning;
Deionized water;
Absolute ethyl alcohol, purity is greater than 99.5%;
Zinc acetate, Zn (CH 3cOO) 22H 2o, the powder of content >99.8%;
Lithium hydroxide, LiOHH 2o, the powder of content >99.7%;
Zinc nitrate, Zn (NO 3) 26H 2o, the powder of content >99.5%;
Ammoniacal liquor, NH 3h 2o, NH 3the solution of content >25%;
Constant temperature water bath, temperature control scope room temperature～300 ℃, 0.1/0.01 ℃ of temperature-controlled precision;
Spin coater, 300-10000 revs/min of revolutions;
Sintering furnace, temperature control scope room temperature～1200 ℃;
Step 2, zinc-oxide nano column array preparation:
(1) by Zn (CH 3cOO) 22H 2o solution is added in appropriate absolute ethyl alcohol, then adds hot reflux 0.5h, naturally cooling;
(2) add again a certain amount of LiOHH 2o, ultrasonic reaction 1 h can obtain stable ZnO colloidal sol;
(3), after prepared by colloidal sol, utilize czochralski method, spin-coating method to prepare layer of ZnO membrana granulosa at substrate surface;
(4) by high temperature heat treatment 2h of ZnO membrana granulosa, standby;
(5) under normal temperature by Zn (NO 3) 26H 2o is dissolved in deionized water, then adds excessive ammonia, and on magnetic stirring apparatus, stir, and add appropriate copper, manganese, zinc, platinum, the slaine of the elements such as titanium carries out modification as active component to ZnO nano post array, and it is standby that this solution is made reactant liquor;
(6) substrate of above-mentioned deposited monolayers ZnO membrana granulosa is vertically put into the reactant liquor preparing;
(7) in water bath with thermostatic control, react 2 h and on substrate, prepared oldered array;
(8) at high temperature heat treatment of oldered array 2 h obtain ZnO nano post array;
(9) utilize above-mentioned steps making ZnO nano column array on multiple substrates;
Step 3, substrate is installed:
In purifier inside, substrate is arranged above and below, wherein first substrate right side connects purifying wall, vacancy is left in left side, and second substrate left side connects purifying wall, and vacancy is left on right side, arrange so successively until fill purifier inside, composition zinc-oxide nano column array purification system.
2. the method for the preparation of removing the zinc-oxide nano column array purification system of ethene in carbon dioxide according to claim 1, is characterized in that Zn (CH in described step 2 3cOO) 22H 2o and absolute ethyl alcohol mixed proportion are n (Zn (CH 3cOO) 22H 2o)/n (C 2h 5oH) between 0.001 to 0.003.
3. the method for the preparation of removing the zinc-oxide nano column array purification system of ethene in carbon dioxide according to claim 1, is characterized in that Zn (CH in described step 2 3cOO) 22H 2o and absolute ethyl alcohol add hot reflux minimum temperature after mixing is 60 ℃, and maximum temperature is 80 ℃.
4. the method for the preparation of removing the zinc-oxide nano column array purification system of ethene in carbon dioxide according to claim 1, is characterized in that LiOHH in described step 2 2the amount that O adds and Zn (CH 3cOO) 22H 2the ratio of O is n (Zn (CH 3cOO) 22H 2o)/n (LiOHH 2o) between 0.5 to 0.9.
5. the method for the preparation of removing the zinc-oxide nano column array purification system of ethene in carbon dioxide according to claim 1, is characterized in that Zn (NO in described step 2 3) 26H 2the mixed proportion that O joins ammonia neutralization ammoniacal liquor is n (NH 3h 2o)/n (Zn (NO 3) 26H 2o) between 2.5 to 5.
6. the method for the preparation of removing the zinc-oxide nano column array purification system of ethene in carbon dioxide according to claim 1, it is characterized in that the water-bath temperature of zinc-oxide nano column array in described step 2 minimum be 65 ℃, be up to 95 ℃.
7. according to claim 1 for the preparation of the method for removing the zinc-oxide nano column array purification system of ethene in carbon dioxide, it is characterized in that the heat treatment temperature of zinc-oxide nano column array in described step 2 minimum be 350 ℃, be up to 500 ℃.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102024637A (en) * 2009-09-17 2011-04-20 深圳华映显示科技有限公司 Method for preparing zinc oxide nano column array field emission component
KR20120042492A (en) * 2010-10-25 2012-05-03 엘지이노텍 주식회사 Light emitting diode
CN102531034A (en) * 2011-12-16 2012-07-04 天津大学 Method for preparing zinc oxide nano sheet array
CN103395823A (en) * 2013-07-22 2013-11-20 中国计量学院 Preparation method for nano-zinc oxide directional array

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102024637A (en) * 2009-09-17 2011-04-20 深圳华映显示科技有限公司 Method for preparing zinc oxide nano column array field emission component
KR20120042492A (en) * 2010-10-25 2012-05-03 엘지이노텍 주식회사 Light emitting diode
CN102531034A (en) * 2011-12-16 2012-07-04 天津大学 Method for preparing zinc oxide nano sheet array
CN103395823A (en) * 2013-07-22 2013-11-20 中国计量学院 Preparation method for nano-zinc oxide directional array

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Address after: 215152 Anmin Road, Panyang Industrial Park, Huangdai Town, Xiangcheng District, Suzhou City, Jiangsu Province

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