CN108704609A - Monolayer CuCl/ acticarbon preparation methods for CO adsorbing separations - Google Patents
Monolayer CuCl/ acticarbon preparation methods for CO adsorbing separations Download PDFInfo
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- CN108704609A CN108704609A CN201810535849.7A CN201810535849A CN108704609A CN 108704609 A CN108704609 A CN 108704609A CN 201810535849 A CN201810535849 A CN 201810535849A CN 108704609 A CN108704609 A CN 108704609A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0233—Compounds of Cu, Ag, Au
- B01J20/0237—Compounds of Cu
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0288—Halides of compounds other than those provided for in B01J20/046
Abstract
The invention discloses a kind of monolayer CuCl/ acticarbon preparation methods for CO adsorbing separations, belong to adsorbent preparation field in inorganic non-metallic material.This method is suitable for the preparation of the CO adsorbing separation adsorbents of industrialized production and application.The preparation process of the present invention is first by Cu2(OH)2CO3And CuCl2It is dissolved in acquisition cupric salt solution in formic acid, and is impregnated in activated carbon surface, obtains sorbent precursor body；Then under vacuum conditions or flowing inert atmosphere N2Or presoma is heated under Ar environment, you can monolayer CuCl/ acticarbons are prepared.The monolayer CuCl/ acticarbons prepared by the method for the invention have high CO adsorbances, selectivity and reproducibility, can be used for the separation and purification of the various gases containing CO.
Description
Technical field
The invention belongs to adsorbent preparation fields in inorganic non-metallic material, and in particular to a kind of for CO adsorbing separations
Monolayer CuCl/ acticarbon preparation methods.
Background technology
CO can synthesize many important chemical products, such as acetic acid, aceticanhydride, oxalic acid, grass as important basic chemical industry raw material
Acid esters, carbonic ester, makrolon, formic acid, formic acid esters, propionic acid, isocyanates, dimethylformamide, phosgene and metal-carbonyl
Compound etc..With the increase of these market demands for being referred to as carbonyl synthesis product, demand to basic material CO also with
Increase.China's CO resources are very abundant, and coal, oil, natural gas are through CO2Made from either water vapor portion is aoxidized or is converted
CO is all rich in synthesis gas, water-gas and semiwater gas；Industrial waste gas, such as make steel furnace exhaust gas, calcium carbide stove exhaust, blast furnace tail gas,
Also all being rich in yellow phosphoric tail gas has CO, however in these air sources, CO is often and CO2、CH4、N2、H2Etc. other gas coexistences, therefore
Obtain pure CO, it is necessary to which separating-purifying is carried out to mixed gas.
Currently, industrially the separation common methods of CO have cryogenic separation, solution absorption method and absorption method.With other technologies phase
Comparing absorption method has many advantages, such as that low energy consumption, degree of purification is high, equipment is simple and is easy to automation, therefore is solved in fact in commercial Application
Absorption method has sizable competitive advantage in the problem of border.For absorption method, adsorbent is its core, and obtaining has high inhale
The adsorbent of attached capacity and adsorptive selectivity is the basis for ensureing efficient absorption separation.But it is a large amount of the study found that conventional
CO physical absorbents, for example, zeolite molecular sieve and activated carbon etc., they are for the CO included in CO gaseous mixtures2、CH4、N2With
H2Equal gases have higher adsorption capacity, so as to cause its lower CO selectivity.Absorptive complex wave separating adsorbent is to be based on
The principle of π complex bonds can be formed between adsorption molecule and adsorbent activity site, to divide from mixture using its realization
From purification CO.π complexings belong to the scope of weak chemical bond, therefore, with traditional using Van der Waals force or the physics of electrostatic force
Absorption is compared, its active force is strong, there is higher adsorptive selectivity；And compared with general chemisorption, its weak chemical bond
Matter makes desorption process be easy to be achieved by way of reducing pressure or increasing temperature.In all d p-block element ps, compare
In other metals, Cu+π complexing powers it is strong, and cost is relatively low, and therefore, CO- π complexing adsorbents are focused primarily on CuCl at present
Complexing adsorbent.Meanwhile in order to make the utilization of CuCl reach maximization, the carrier with high-specific surface area need to be supported on
On, prepare load type adsorbing agent.
So far, it has been proposed that many is used for the Cu of CO separating-purifyings+ The preparation method of adsorbent.For example, Chinese
Patent CN1113828A and CN105749858A disclose Cu+/ Y sorbent preparation methods, United States Patent (USP) No3497462,
No4034065, No4019879 disclose Cu+/ X molecular sieve sorbent preparation method, Chinese patent CN101626831A, Japan
Tekiaki No. 60-156548 and No. 60-125250, special open 2003-311148, Unexamined Patent 9-122494 disclose Cu+/
ZSM5 sorbent preparation methods, these methods are by first using Cu2+Ion exchange is carried out with zeolite molecular sieve X, Y and ZSM-,
Then again by Cu2+It is reduced to Cu+, but the limitation due to molecular sieve exchange capacity and Cu2+To Cu+Reduction is difficult to control
Property, preparation-obtained adsorbent CO adsorption capacities are limited.Japanese Unexamined Patent Publication 11-226389, Chinese patent CN 86106219
Disclose and CuCl be dissolved in salt sour solvent or organic solvent preparation CO load type adsorbing agents, due to hydrochloric acid strong corrosive and
The toxicity of organic solvent and so that its industrialized production is restricted.Chinese patent CN 86102838, which is disclosed, passes through thermoplastic polymer
Principle prepares CuCl/ molecular sieves, and the specific steps are be to make CuCl thermoplastic polymers in molecular sieve CuCl and molecular sieve Hybrid Heating
Surface.However, due to the aerial unstability of CuCl, need to be mixed in the environment of stringent anhydrous and anaerobic in operation
Material, increases operation difficulty and cost.In order to solve this problem, Chinese patent CN 104525127A and CN 1683249 is
Copper formate and copper chloride are carried on using aqueous solution infusion process and are carried on the porous materials such as activated carbon and the organic bone of metal respectively
Frame MIL-100（Fe）As presoma, CO adsorbents are prepared by heating, but due to metal organic framework MIL-100
（Fe）Solubility low in water under the price of limitation and the copper formate costliness of carrier commercial Application and its room temperature, therefore
There are some problems in terms of practicability.
Invention content
The purpose of the present invention is to solve the deficiencies in the prior art, providing, a kind of production difficulty is small, easy to operate, cost
Monolayer CuCl/ acticarbon preparation methods cheap, suitable for industrialized production for CO adsorbing separations, by this
Monolayer CuCl/ acticarbons prepared by method have higher CO adsorbances and preferable selectivity and reproducibility.
To achieve the above object, the monolayer CuCl/ activated carbon adsorptions for CO adsorbing separations designed by the present invention
Agent preparation method, includes the following steps：
1）By Cu2(OH)2CO3And CuCl2It is 0.4 in molar ratio:1~0.8:After 1 weighs, it is added sequentially in deionized water,
Be stirred continuously down and add formic acid, continue stirring until mantoquita be completely dissolved, obtain cupric salt solution, wherein basic copper carbonate
Molar ratio with formic acid is 1:4~1:4.3；
2）By step 1）In solution obtained and activated carbon by liquid-solid ratio be 3ml:4g~5ml:4g is mixed, then will mixing
Object is added in cucurbit, and wherein addition must not exceed the 2/3 of cucurbit volume；
3）The dipping of mantoquita is carried out by the way of rotary evaporation, dipping temperature is 50 ~ 60 DEG C, and pressure is less than 10kPa；
4）Wait for step 3）After water evaporation in middle evaporative flask, takes out sample and be put into 110 ~ 120 DEG C of baking oven and continue fully
It is dry, obtain sorbent precursor body；
5）By step 4）In presoma obtained be placed in the reaction tube of tube furnace, under vacuum conditions or flowing indifferent gas
Under atmosphere environment, presoma is heated, specially heats 2 ~ 3h first at 120 ~ 130 DEG C, then again 180
Heat 4 ~ 8h at ~ 300 DEG C, you can monolayer CuCl/ acticarbons are prepared.
Preferably, the step 1）Cu2(OH)2CO3With CuCl2Molar ratio be 0.5:1~0.7:1, Cu2
(OH)2CO3Molar ratio with formic acid is 1:4.1~1:4.3.
Preferably, the step 2）In activated carbon be BET specific surfaces be 900 ~ 1400m2The granular active of/g
Charcoal or powdered activated carbon.
Preferably, Cu is 3 ~ 5mol/kg to the load capacity of activated carbon in the CuCl/ acticarbons.
Preferably, the step 5）In vacuum environment be that pressure in reaction tube is less than 10-1Pa；The inertia
Atmosphere is N2Or Ar, the air speed of the inert atmosphere is 2 ~ 10 mL/min/g.
Preferably, the step 1）Cu2(OH)2CO3And CuCl2Molar ratio be 1.3:2, the Cu2(OH)2CO3Molar ratio with formic acid is 1:4.3；The step 2）In activated carbon be BET specific surfaces be 1080m2The granular active of/g
Charcoal.
The beneficial effects of the invention are as follows：
First, the monolayer CuCl/ acticarbons that the present invention is prepared have CO adsorption capacity height, CO/CH4、CO/
CO2And CO/N2The good feature of adsorptive selectivity under 100kPa, can reach 52.8mL/g at 25 DEG C to CO adsorption capacities,
And adsorbent reactivation ability is strong, can Reusability and keep adsorbance almost unchanged, so as to applied to containing the various of CO
The separation and purification of gas；
Second, the monolayer CuCl/ acticarbons prepared by the method for the invention improve Cu+Utilization rate, this hair
The low in raw material price of bright use, and special protection equipment or organic solvent need not be used, pollution low with manufacturing cost
Small and simple for process feature is suitable for industrialized production and application.
Description of the drawings
Fig. 1 is the adsorption isotherm map of CuCl/ acticarbons prepared by the method for the present invention.
Fig. 2 is the XRD spectra of adsorbent described in the embodiment of the present invention 1.
Specific embodiment
Below by specific embodiment, the present invention is further illustrated：
Embodiment 1
28.9g Cu are weighed respectively2(OH)2CO3With 27.0g CuCl2, it is added in the deionized water of 100mL, under stiring again
The formic acid 24mL of 85wt%, density 1.22g/mL are added thereto, continues to stir, until mantoquita is completely dissolved, obtains cupric salt
Solution I；It is 1080 m to weigh specific surface area2The granular active carbon 20g of/g is put into rotary evaporation bottle, and it is molten to add above-mentioned mantoquita
I 25mL of liquid, less than 10kPa, temperature is that the dipping of mantoquita is carried out by the way of rotary evaporation at 50 DEG C, until water evaporation
It finishes；It takes out and continues fully drying in the baking oven for put it into 120 DEG C, obtain sorbent precursor body.Gained presoma is placed in
In tube furnace, less than 10-1Under the vacuum environment of Pa, heats 2h at 120 DEG C first, then heat at 220 DEG C of heating
4h is prepared monolayer CuCl/ acticarbons, is named as No1.
The XRD spectra of the adsorbent is shown in the diffraction maximum that CuCl is not observed in spectrogram, illustrates CuCl in activated carbon table
Face high dispersive；As shown in Fig. 1, CO, CH at 25 DEG C4、CO2And N2Adsorption isotherm on CuCl/ acticarbons can be with
Find out that the adsorbent has to the higher adsorption capacities of CO and preferable CO/CH4、CO/CO2And CO/N2Adsorptive selectivity, 25
DEG C, it is 52.8mL/g to CO adsorption capacities under 100kPa.
Embodiment 2
Cupric salt solution is obtained using proportioning and mode same as Example 1；And the granular active carbon for weighing same amount is put
Enter in rotary evaporation bottle, adds I 30mL of above-mentioned copper salt solution, then monolayer is prepared with identical process conditions
CuCl/ acticarbons No2.
The XRD spectra of the adsorbent is shown in the diffraction maximum that CuCl is not observed in spectrogram, illustrates CuCl in activated carbon table
Face high dispersive.The adsorbent is at 25 DEG C, is 52.1mL/g to CO adsorption capacities under 100kPa.
Embodiment 3
Cupric salt solution is obtained using proportioning and mode same as Example 1；And the granular active carbon for weighing same amount is put
Enter in rotary evaporation bottle, add I 19mL of above-mentioned copper salt solution, CuCl/ acticarbons No3 is prepared.
The XRD spectra of the adsorbent is shown in the diffraction maximum that CuCl is not observed in spectrogram, illustrates CuCl in activated carbon table
Face high dispersive.The adsorbent is at 25 DEG C, is 48.2mL/g to CO adsorption capacities under 100kPa.
Embodiment 4
Using adsorbent preparation method same as Example 1, only wherein the specific surface of activated carbon is 966m2/ g, is prepared into
To CuCl/ acticarbons No4.
The XRD spectra of the adsorbent is shown in the diffraction maximum that CuCl is not observed in spectrogram, illustrates CuCl in activated carbon table
Face high dispersive.The adsorbent is at 25 DEG C, is 51.0mL/g to CO adsorption capacities under 100kPa.
Embodiment 5
22.2g Cu are weighed respectively2(OH)2CO3With 27.0g CuCl2, it is added in the deionized water of 100mL, under stiring again
The formic acid 19mL of 85wt%, density 1.22g/mL are added thereto, continues to stir, until mantoquita is completely dissolved, obtains cupric salt
Solution II；Then adsorbent preparation method and proportioning same as Example 1 are used, it is molten only to change copper salt solution I into mantoquita
CuCl/ acticarbons No5 is prepared in liquid II.
The XRD spectra of the adsorbent is shown in the diffraction maximum that CuCl is not observed in spectrogram, illustrates CuCl in activated carbon table
Face high dispersive.The adsorbent is at 25 DEG C, is 50.9mL/g to CO adsorption capacities under 100kPa.
Embodiment 6
Cu in embodiment 12(OH)2CO3The amount of weighing be 26.6g, and the activated carbon chosen be specific surface area is 996m2/g
Powdered active carbon, it is in addition to this identical as 1 condition of embodiment, CuCl/ acticarbons No6 is prepared.
The XRD spectra of the adsorbent is shown in the diffraction maximum that CuCl is not observed in spectrogram, illustrates CuCl in activated carbon table
Face high dispersive.The adsorbent is at 25 DEG C, is 51.5mL/g to CO adsorption capacities under 100kPa.
Embodiment 7
Gained presoma is placed in tube furnace in embodiment 1, in the inert atmosphere N of flowing2Environment air speed is 5mL/min/g
Under, heat 2h at 120 DEG C first, then heats to 240 DEG C and heat 6h, it is in addition to this identical as 1 condition of embodiment,
Monolayer CuCl/ acticarbons No7 is prepared.
The XRD spectra of the adsorbent is shown in the diffraction maximum that CuCl is not observed in spectrogram, illustrates CuCl in activated carbon table
Face high dispersive.The adsorbent is at 25 DEG C, is 52.5mL/g to CO adsorption capacities under 100kPa.
Embodiment 8
Gained presoma is placed in tube furnace in embodiment 1, is 8mL/min/g in the inert atmosphere Ar environment air speeds of flowing
Under, heat 2h at 120 DEG C first, then heats to 240 DEG C and heat 6h, it is in addition to this identical as 1 condition of embodiment,
Monolayer CuCl/ acticarbons No9 is prepared.
The XRD spectra of the adsorbent is shown in the diffraction maximum that CuCl is not observed in spectrogram, illustrates CuCl in activated carbon table
Face high dispersive.The adsorbent is at 25 DEG C, is 52.4mL/g to CO adsorption capacities under 100kPa.
The specific implementation mode of present invention described above, is not intended to limit the scope of the present invention..Any basis
The various other corresponding changes and deformation that the technical concept of the present invention is made, should be included in the guarantor of the claims in the present invention
It protects in range.
Claims (6)
1. a kind of monolayer CuCl/ acticarbon preparation methods for CO adsorbing separations, it is characterised in that：Including such as
Lower step：
1）By Cu2(OH)2CO3And CuCl2It is 0.4 in molar ratio:1~0.8:After 1 weighs, it is added sequentially in deionized water, not
Add formic acid under disconnected stirring, continue stirring until mantoquita is completely dissolved, obtain cupric salt solution, wherein basic copper carbonate with
The molar ratio of formic acid is 1:4~1:4.3；
2）By step 1）In solution obtained and activated carbon by liquid-solid ratio be 3ml:4g~5ml:4g is mixed, then will mixing
Object is added in cucurbit, and wherein addition must not exceed the 2/3 of cucurbit volume；
3）The dipping of mantoquita is carried out by the way of rotary evaporation, dipping temperature is 50 ~ 60 DEG C, and pressure is less than 10kPa；
4）Wait for step 3）After water evaporation in middle evaporative flask, takes out sample and be put into 110 ~ 120 DEG C of baking oven and continue fully
It is dry, obtain sorbent precursor body；
5）By step 4）In presoma obtained be placed in the reaction tube of tube furnace, under vacuum conditions or flowing indifferent gas
Under atmosphere environment, presoma is heated, specially heats 2 ~ 3h first at 120 ~ 130 DEG C, then again 180
Heat 4 ~ 8h at ~ 300 DEG C, you can monolayer CuCl/ acticarbons are prepared.
2. the monolayer CuCl/ acticarbon preparation methods according to claim 1 for CO adsorbing separations,
It is characterized in that：The step 1）Cu2(OH)2CO3And CuCl2Molar ratio be 0.5:1~0.7:1, Cu2(OH)2CO3With formic acid
Molar ratio is 1:4.1~1:4.3.
3. the monolayer CuCl/ acticarbon preparation methods according to claim 2 for CO adsorbing separations,
It is characterized in that：The step 2）In activated carbon be BET specific surfaces be 900 ~ 1400m2The granular active carbon of/g is powdered activated
Charcoal.
4. the monolayer CuCl/ acticarbon preparation methods according to claim 3 for CO adsorbing separations,
It is characterized in that：Cu is 3 ~ 5mol/kg to the load capacity of activated carbon in the CuCl/ acticarbons.
5. the monolayer CuCl/ acticarbon preparation methods according to claim 4 for CO adsorbing separations,
It is characterized in that：The step 5）In vacuum environment be that pressure in reaction tube is less than 10-1Pa；The inert atmosphere is N2Or
The air speed of Ar, the inert atmosphere are 2 ~ 10mL/min/g.
6. the monolayer CuCl/ acticarbon preparation methods according to claim 5 for CO adsorbing separations,
It is characterized in that：The step 1）Cu2(OH)2CO3And CuCl2Molar ratio be 1.3:2, the Cu2(OH)2CO3With rubbing for formic acid
You are than being 1:4.3；The step 2）In activated carbon be BET specific surfaces be 1080m2The granular active carbon of/g.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110270303A (en) * | 2019-04-28 | 2019-09-24 | 大英达科特化工科技有限公司 | A kind of efficient CO adsorbent and preparation method thereof |
| CN111375374A (en) * | 2018-12-29 | 2020-07-07 | 中国石油化工股份有限公司 | Load type copper-based adsorbent and preparation method thereof |
| CN113351159A (en) * | 2020-03-04 | 2021-09-07 | 中国石油化工股份有限公司 | Adsorbent for deeply removing carbon monoxide in hydrogen, preparation method thereof and method for removing carbon monoxide in hydrogen by using adsorbent |
| CN114471441A (en) * | 2020-10-26 | 2022-05-13 | 中国石油化工股份有限公司 | CO adsorbent and preparation method and application thereof |
| CN115722187A (en) * | 2021-08-27 | 2023-03-03 | 北京北大先锋科技股份有限公司 | High-adsorption-capacity carbon monoxide complex adsorbent and preparation method and application thereof |
| CN116139666A (en) * | 2023-04-18 | 2023-05-23 | 大庆德斯曼环保设备有限公司 | Environmental protection exhaust emission treatment equipment |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111375374A (en) * | 2018-12-29 | 2020-07-07 | 中国石油化工股份有限公司 | Load type copper-based adsorbent and preparation method thereof |
| CN111375374B (en) * | 2018-12-29 | 2022-08-12 | 中国石油化工股份有限公司 | Load type copper-based adsorbent and preparation method thereof |
| CN110270303A (en) * | 2019-04-28 | 2019-09-24 | 大英达科特化工科技有限公司 | A kind of efficient CO adsorbent and preparation method thereof |
| CN113351159A (en) * | 2020-03-04 | 2021-09-07 | 中国石油化工股份有限公司 | Adsorbent for deeply removing carbon monoxide in hydrogen, preparation method thereof and method for removing carbon monoxide in hydrogen by using adsorbent |
| CN114471441A (en) * | 2020-10-26 | 2022-05-13 | 中国石油化工股份有限公司 | CO adsorbent and preparation method and application thereof |
| CN115722187A (en) * | 2021-08-27 | 2023-03-03 | 北京北大先锋科技股份有限公司 | High-adsorption-capacity carbon monoxide complex adsorbent and preparation method and application thereof |
| CN116139666A (en) * | 2023-04-18 | 2023-05-23 | 大庆德斯曼环保设备有限公司 | Environmental protection exhaust emission treatment equipment |
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Application publication date: 20181026 |