CN103736441B - Remove the method for the zinc-oxide nano column array purification system of ethene in carbon dioxide - Google Patents

Remove the method for the zinc-oxide nano column array purification system of ethene in carbon dioxide Download PDF

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CN103736441B
CN103736441B CN201310690940.3A CN201310690940A CN103736441B CN 103736441 B CN103736441 B CN 103736441B CN 201310690940 A CN201310690940 A CN 201310690940A CN 103736441 B CN103736441 B CN 103736441B
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zinc
column array
oxide nano
nano column
substrate
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CN103736441A (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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    • 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
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/151—Reduction of greenhouse gas [GHG] emissions, e.g. CO2

Abstract

The invention discloses a kind of method for the preparation of the zinc-oxide nano column array purification system of ethene in removal carbon dioxide, this preparation method is that the method for being synthesized by solution on substrate prepares zinc-oxide nano column array, this zinc-oxide nano column array and substrate combine firmly, and multiple substrate arrangement is formed purification system in purifier, it is simple that this preparation method has technique, reaction temperature is low, do not limit by size, cost is low, and purification system has good ethylene absorption performance, purification degrees is high, and adsorbance is large, selective 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, especially relate to the new method that a kind of purification system preparing the substrate composition of depositing zinc oxide nano column array can be used for removing in carbon dioxide recovery technique ethene.
Background technology
Carbon dioxide is a kind of resource of preciousness, can be widely used in multiple fields: the industry such as chemical synthesis industry, mechanical protection welding, metal casting processing, agricultural fertilizer, fruit and vegetable is fresh-keeping, beer beverage is filling, oil exploitation, fire-fighting fire extinguishing, medical and health all needs great amount of carbon dioxide.The source of China's carbon dioxide is very abundant, but because the measure of reclaiming carbon dioxide is unfavorable, the carbon dioxide of annual recycling also not enough discharge capacity 2%, nearly about 20,000,000,000 tons of carbon dioxide in air is discharged into every year in world wide, both the pollution of air had been caused, form fearful greenhouse effects, waste again valuable resource.
Developing rapidly in recent years along with industry, carbon dioxide consumption figure increases year by year and the production of carbon dioxide often limits by resource, and therefore carbon dioxide product is in the state that supply falls short of demand always.
Ethylene prepares the carbon dioxide that in the production process of oxirane, by-product is a large amount of, makes full use of this part carbon resource, carries out refining purification, both decreased a large amount of pollution, and increased again the economic benefit of enterprise carbon dioxide.
But ethylene understands residual fraction ethene in carbon dioxide tail gas after preparing oxirane, cause 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 water and carbon dioxide.First Production by Catalytic Combustion Process will build the device that a set of cryogenic air separation method produces liquid oxygen, pure oxygen is joined in the carbon dioxide having 96% purity, mixes with it, then all gas is heated to 350 DEG C, enter in catalytic burner, by excessive oxygen effect, a small amount of organic impurities is burnt.The all gas generated cools to about 20 DEG C again, enters supercharging in compressor after voltage stabilizing, through molecular sieve drying dehydration, and adsorption-edulcoration matter, then the excessive oxygen removing and add is entered in rectifying column through post liquefaction, can liquid carbon dioxide product be obtained at the bottom of tower.
Production by Catalytic Combustion Process is a set of liquid oxygen production device and combustion heating cooling system than absorption distillation fado totally, and more complicated than absorption distillation method one times of flow process, bring 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 air liquefaction, will will consume mass energy, and the production cost of absorption distillation method is lower.
But the purifier of absorption distillation method adopts molecular sieve to carry out purifying to foreign gas, and purification capacity is limited in the past.The structure of this patent to conventional purification device is changed, and adopts more effective purified material, enhances the adsorption capacity of ethene, and this purification system has good ethylene absorption performance, and purification degrees is high, and adsorbance is large, selective good.
Summary of the invention
Goal of the invention of the present invention is the shortcoming in order to overcome above-mentioned background technology, a kind of method utilizing solution to synthesize is provided to prepare zinc-oxide nano column array on substrate, and multiple substrate arrangement is formed 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 the zinc-oxide nano column array purification system of ethene in removal carbon dioxide, the method is mainly divided into three steps, be preparation, zinc-oxide nano column array preparation, substrate installation respectively, concrete technology step is as follows:
Step one, 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 DEG C, temperature-controlled precision 0.1/0.01 DEG C;
Spin coater, revolution 300-10000 rev/min;
Sintering furnace, temperature control scope room temperature ~ 1200 DEG C;
Step 2, prepared by zinc-oxide nano column array:
(1) by Zn (CH 3cOO) 22H 2o solution is added in appropriate absolute ethyl alcohol, then adds hot reflux 0.5h, naturally cools;
(2) a certain amount of LiOHH is added again 2o, ultrasonic reaction 1h can obtain stable ZnO colloidal sol;
(3), after prepared by colloidal sol, czochralski method, spin-coating method is utilized to prepare layer of ZnO membrana granulosa at substrate surface;
(4) by ZnO particle film at high temperature heat treatment 2h, for subsequent use;
(5) under normal temperature by Zn (NO 3) 26H 2o dissolves in deionized water, then adds excessive ammonia, magnetic stirring apparatus stirs, and adds appropriate copper, manganese, zinc, platinum, and the slaine of the elements such as titanium is used as active component and carries out modification to ZnO nano post array, and it is for subsequent use that this solution makes reactant liquor;
(6) substrate of above-mentioned deposited monolayers ZnO particle film is vertically put into the reactant liquor prepared;
(7) in water bath with thermostatic control, react 2h and namely on substrate, prepare oldered array;
(8) oldered array at high temperature heat treatment 2h obtain ZnO nano post array;
(9) above-mentioned steps making ZnO nano column array on multiple substrate is utilized;
Step 3, substrate is installed:
Inner at purifier, substrate is arranged above and below, wherein connects purifying wall on the right side of first substrate, vacancy is left in left side, and connect purifying wall on the left of second substrate, vacancy is left on right side, arrangement, until fill purifier inside, forms zinc-oxide nano column array purification system so successively.
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 2the minimum temperature adding hot reflux after O and absolute ethyl alcohol mix is 60 DEG C, and maximum temperature is 80 DEG C.
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 is minimum is 65 DEG C, is up to 95 DEG C.
In described step 2, the heat treatment temperature of zinc-oxide nano column array is minimum is 350 DEG C, is up to 500 DEG C.
The invention has the beneficial effects as follows: it is simple that this preparation method has technique, and reaction temperature is low, does not limit by size, and cost is low, and purification system has good ethylene absorption performance, and purification degrees is high, adsorbance is large, selective 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.
Detailed description of the invention
The present embodiment is a kind of method for the preparation of the zinc-oxide nano column array purification system of ethene in removal carbon dioxide, the method is mainly divided into three steps, be preparation, zinc-oxide nano column array preparation, substrate installation respectively, concrete technology step is as follows:
Step one, 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 DEG C, temperature-controlled precision 0.1/0.01 DEG C;
Spin coater, revolution 300-10000 rev/min;
Sintering furnace, temperature control scope room temperature ~ 1200 DEG C;
Step 2, prepared by zinc-oxide nano column array:
(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 adding hot reflux after mixing is 60 DEG C, and maximum temperature is 80 DEG C, finally carries out nature cooling again;
(2) a certain amount of LiOHH is added again 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 1h can obtain stable ZnO colloidal sol;
(3), after prepared by colloidal sol, czochralski method, spin-coating method is utilized to prepare layer of ZnO membrana granulosa at substrate surface;
(4) by ZnO particle film at high temperature heat treatment 2h, for subsequent use;
(5) under normal temperature by Zn (NO 3) 26H 2o dissolves 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, magnetic stirring apparatus stirs, and add appropriate copper, manganese, zinc, platinum, the slaine of the elements such as titanium is used as active component and carries out modification to ZnO nano post array, and it is for subsequent use that this solution makes reactant liquor;
(6) substrate of above-mentioned deposited monolayers ZnO particle film is vertically put into the reactant liquor prepared;
(7) minimum be 65 DEG C, be up to and react 2h in 95 DEG C of waters bath with thermostatic control and namely on substrate, prepared oldered array;
(8) oldered array minimum be 350 DEG C, under being up to 500 DEG C of high temperature, heat treatment 2h obtains ZnO nano post array;
(9) above-mentioned steps making ZnO nano column array on multiple substrate is utilized;
Step 3, substrate is installed:
As shown in Figure 1, inner at purifier, substrate is arranged above and below, wherein connect purifying wall on the right side of first substrate, vacancy is left in left side, and connect purifying wall on the left of second substrate, vacancy is left on right side, arrangement, until fill purifier inside, forms zinc-oxide nano column array purification system so successively.
Enumerate two most preferred embodiments below and the inventive method be described:
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 DEG C, adds hot reflux 0.5h, naturally cools;
2) a certain amount of LiOHH is added again 2o, n (Zn (CH 3cOO) 22H 2o)/n (LiOHH 2o) mixed proportion is 0.6, and ultrasonic reaction 1h can obtain the ZnO colloidal sol of stable homogeneous;
3), after prepared by colloidal sol, czochralski method is utilized to prepare layer of ZnO membrana granulosa at substrate surface;
4) by ZnO particle film at high temperature heat treatment 2h, for subsequent use;
5) under normal temperature by Zn (NO 3) 26H 2o dissolves in deionized water, then adds excessive ammonia, n (NH 3h 2o)/n (Zn (NO 3) 26H 2o) mixed proportion is 3, and magnetic stirring apparatus stirs, and adds appropriate copper chloride and carry out modification as active component to ZnO nano post array, and it is for subsequent use that this solution makes reactant liquor;
6) substrate of above-mentioned deposited monolayers ZnO particle film is vertically put into the reactant liquor prepared;
7) in the water bath with thermostatic control of 70 DEG C, react 2h and namely on substrate, prepare oldered array;
8) oldered array heat treatment 2h under the high temperature of 400 DEG C obtains ZnO nano post array;
9) similar method making ZnO nano column array on multiple substrate is utilized;
10) then multiple substrate is arranged in purifier according to the pattern shown in Fig. 1 and forms purification system.
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 DEG C, adds hot reflux 0.5h, naturally cools;
2) a certain amount of LiOHH is added again 2o, n (Zn (CH 3cOO) 22H 2o)/n (LiOHH 2o) mixed proportion is 0.7, and ultrasonic reaction 1h can obtain the ZnO colloidal sol of stable homogeneous;
3), after prepared by colloidal sol, spin-coating method is utilized to prepare layer of ZnO membrana granulosa at substrate surface;
4) by ZnO particle film at high temperature heat treatment 2h, for subsequent use;
5) under normal temperature by Zn (NO 3) 26H 2o dissolves in deionized water, then adds excessive ammonia, n (NH 3h 2o)/n (Zn (NO 3) 26H 2o) mixed proportion is 4, and magnetic stirring apparatus stirs, and adds appropriate copper chloride and carry out modification as active component to ZnO nano post array, and it is for subsequent use that this solution makes reactant liquor;
6) substrate of above-mentioned deposited monolayers ZnO particle film is vertically put into the reactant liquor prepared;
7) in the water bath with thermostatic control of 80 DEG C, react 2h and namely on substrate, prepare oldered array;
8) oldered array heat treatment 2h under the high temperature of 500 DEG C obtains ZnO nano post array;
9) similar method making ZnO nano column array on multiple substrate is utilized;
10) then multiple substrate is arranged in purifier according to the pattern shown in Fig. 1 and forms purification system.

Claims (7)

1. the method for the preparation of the zinc-oxide nano column array purification system of ethene in removal carbon dioxide, it is characterized in that the method is mainly divided into three steps, be preparation, zinc-oxide nano column array preparation, substrate installation respectively, concrete technology step is as follows:
Step one, 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 DEG C, temperature-controlled precision 0.1/0.01 DEG C;
Spin coater, revolution 300-10000 rev/min;
Sintering furnace, temperature control scope room temperature ~ 1200 DEG C;
Step 2, prepared by zinc-oxide nano column array:
(1) by Zn (CH 3cOO) 22H 2o solution is added in appropriate absolute ethyl alcohol, then adds hot reflux 0.5h, naturally cools;
(2) a certain amount of LiOHH is added again 2o, ultrasonic reaction 1h can obtain stable ZnO colloidal sol;
(3), after prepared by colloidal sol, czochralski method, spin-coating method is utilized to prepare layer of ZnO membrana granulosa at substrate surface;
(4) by ZnO particle film at high temperature heat treatment 2h, for subsequent use;
(5) under normal temperature by Zn (NO 3) 26H 2o dissolves in deionized water, then adds excessive ammonia, magnetic stirring apparatus stirs, and adds appropriate copper, manganese, zinc, platinum, and the slaine of titanium elements is used as active component and carries out modification to ZnO nano post array, and it is for subsequent use that this solution makes reactant liquor;
(6) substrate of above-mentioned deposited monolayers ZnO particle film is vertically put into the reactant liquor prepared;
(7) in water bath with thermostatic control, react 2h and namely on substrate, prepare oldered array;
(8) oldered array at high temperature heat treatment 2h obtain ZnO nano post array;
(9) above-mentioned steps making ZnO nano column array on multiple substrate is utilized;
Step 3, substrate is installed:
Inner at purifier, substrate is arranged above and below, wherein connects purifying wall on the right side of first substrate, vacancy is left in left side, and connect purifying wall on the left of second substrate, vacancy is left on right side, arrangement, until fill purifier inside, forms zinc-oxide nano column array purification system so successively.
2. the method for the preparation of the zinc-oxide nano column array purification system of ethene in removal 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 the zinc-oxide nano column array purification system of ethene in removal carbon dioxide according to claim 1, is characterized in that Zn (CH in described step 2 3cOO) 22H 2the minimum temperature adding hot reflux after O and absolute ethyl alcohol mix is 60 DEG C, and maximum temperature is 80 DEG C.
4. the method for the preparation of the zinc-oxide nano column array purification system of ethene in removal 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 the zinc-oxide nano column array purification system of ethene in removal 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 zinc-oxide nano column array purification system for the preparation of removing 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 DEG C, be up to 95 DEG C.
7. according to claim 1 for the preparation of the method for zinc-oxide nano column array purification system removing 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 DEG C, be up to 500 DEG C.
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Citations (3)

* 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
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

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101766715B1 (en) * 2010-10-25 2017-08-23 엘지이노텍 주식회사 Light emitting diode package

Patent Citations (3)

* 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
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

Patentee after: Jinhong Gas Co.,Ltd.

Address before: 215143 No. 6 Anmin Road, Panyang Industrial Park, Huangduo Town, Xiangcheng District, Suzhou City, Jiangsu Province

Patentee before: SUZHOU JINHONG GAS Co.,Ltd.