CN106807330A - The preparation and sorbing material and application of a kind of ordered structure sorbing material - Google Patents
The preparation and sorbing material and application of a kind of ordered structure sorbing material Download PDFInfo
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Abstract
Preparation method the present invention relates to be used for a class ordered structure sorbing material of gas absorption separation, the ordered structure sorbing material is made up of matrix, binding agent and metal-organic framework materials, by the way that the mixed processings such as metal-organic framework material powder, solvent and binding agent first are formed into slurry, then coating is formed by spraying, brushing or being immersed in matrix surface, matrix roll-forming prepares ordered structure sorbing material.The ordered structure sorbing material preparation process is simple, reproducible, sorbing material has abundant loose structure, and adsorption and desorption speed is fast when being separated for gas absorption, is particularly well-suited to the isolation of purified of atm number admixture of gas and concentrates the purification process such as purification.
Description
Technical field
The present invention relates to ordered structure sorbing material design preparation, mixed gas sorption separation technology field,
In particular to separatory monoblock type sorbing material of a class novel adsorption and preparation method thereof.
Background technology
PSA Gas Separation Technology is to grow up in the sixties in last century, by American Association carbon
Compound company (UCC) realizes the industrialization of the bed process technology of pressure-variable adsorption four first.The technology be according to
By the sorbing materials such as molecular sieve to the selective absorption of specific gas and with pressure change realize absorption and
Desorption and regeneration.The pressure-swing absorption process of gas because energy consumption is low, can at normal temperatures run, automate
Degree is high, flow is simple, be widely used in numerous areas, and with the hair of adsorber technologies
Exhibition develops very fast in recent years.
The sorbent used adsorption separation performance of PSA Technology directly determine separating effect and
Device operation energy consumption, it is therefore necessary to updating and developing the more preferable adsorbent of performance.Metal-organic
Framework material is that the polyporous materials for being formed are acted on by coordinate bond by metal ion and organic ligand.
In the past more than ten years, such material in gas due to the various fields such as storing, separate and being catalyzed
Potential application foreground gets more and more people's extensive concerning.
The adsorbent for being used on industry pressure-swing absorption apparatus at present is mostly granular adsorbent, absorption dress
Interior adsorbent is put generally using the limit for piling up type of feed, sorbent suspension adsorption capacity and adsorption desorption speed
System, adsorption tower volume is generally huger.In general, with the reduction of absorbent particles diameter, its
The diffusion rate of gas absorption and desorption will quickly increase, and can greatly improve pressure swing adsorption cycles speed,
So as to greatly reduce adsorption tower volume.But while formed absorbent particle diameter reduces, will also lead
Being significantly increased for bed pressure drop is caused, the desorption of easy adsorbed gas is hindered, so as to greatly increase separator
Operation power consumption.Therefore, using a kind of ordered structure sorbing material for being different from conventional particles adsorbent,
Not only can significantly reduce absorbent particles size, the problem of pressure drop of adsorbent bed can also be solved, to carrying
The adsorption efficiency of unit volume adsorbent high is significant.External many companies have used cellular
Molecular sieve adsorbent bed layer substitutes traditional granule adsorbent, have developed quick adsorption and separates hydrogen, sky
The adsorptive separation technologies such as gas.However, directly extruding the technique phase of overall structure adsorbent using molecular sieve
To complexity, while the later stage processability of metal-organic framework material sieves weaker than conventional molecular,
Ordered structure expressing technique is caused to be difficult to be directly used in the extrusion of metal-organic framework material.Therefore, open
Hair is applied to the metal organic frame ordered structure adsorbent technology of preparing of quick adsorption separation process,
Maintain on the basis of metal-organic framework material excellent properties, greatly improve gas on the adsorbent material
Adsorption desorption diffusion rate, the overall production capacity to improving potential device is significant.
The content of the invention
The purpose of the present invention is directed to that current pressure-swing absorption apparatus adsorbent bed is bulky, adsorbent filling
Amount is more, invest the series of problems such as high, low production efficiency and overall structure adsorbent-shaping complexity,
A kind of preparation method of the ordered structure adsorbent that can be used in quick adsorption separation process is proposed, should
Sorbing material preparation process is simple reliability involved by method, efficiency high, prepared ordered structure is inhaled
Attached dose can be used in the shorter rapid pressure swing adsorption separation process of cycle period, greatly improve unit volume
The disposal ability of device, is particularly well-suited to the isolation of purified of atm number admixture of gas and concentrates purification etc.
Purification process.
The invention provides the preparation method of a class ordered structure sorbing material, such sorbing material is by gold
Category organic framework materials, binding agent and support substrate are constituted.The general principle of its preparation method is will be big
The metal-organic framework materials powder of adsorption capacity is applied directly to support substrate by using binding agent
On, matrix and sorbing material powder are made by external diffusion distance by spraying, brushing or impregnating mode
Short ordered structure sorbing material.
Support substrate of the present invention is fiber cloth-like, according to sorbing material institute application field not
With the difference with the metal organic frame sorbing material for being supported.Support substrate master of the present invention
To be silicon dioxide fibre cloth, zirconium oxide fiber cloth, alumina fibre cloth, polyester fiber cloth, polypropylene fibre
Fiber cloth, aryl fiber cloth, polyester fiber cloth, vinylon fibre cloth, spandex fibre cloth, cotton and charcoal
One kind in fiber cloth.The matrix material for being used solvent selected when should be prepared insoluble in slurry.
The preparation method of a class ordered structure sorbing material involved in the present invention, used in preparation
Porous powder sorbing material is metal organic frame sorbing material.Such sorbing material is insoluble in slurry
Material prepares the powdery porous material of used solvent, its N2Specific surface area is more than 100m2/ g,
Particle size is between 10nm-100 μm.The preferential material specific surface area for using of the invention is between 200-2000
m2/ g, its powder granule size preferentially uses 0.2-30 μm of granular materials.Gold used in the present invention
Category organic frame sorbing material can select different metal ions, one or more material of different structure
Mixture, related engineers and technicians can within the above range enter according to the demand of application field
The appropriate adjustment of row.
Class ordered structure sorbing material involved in the present invention and preparation method thereof, the metal is organic
Frame material is by metal ion, the organic ligand porous structure material that ligand complex is constituted in a solvent.
The constituting portion of metal-organic framework material point includes：Metal ion or metal cluster compound node, have
Machine linking ligand and auxiliary common part and solvent molecule.Due to the topological structure master of metal organic frame
To be determined by the ligancy of node and geometric configuration, although the species of MOFs materials is very more,
The synthesis condition of most MOFs materials is harsher, while being limited by the property of its structure, there is a lot
MOFs materials are difficult to realize extensive synthesis application, so preferential recommendation, most work in the present invention
The porous metals organic framework materials of industry value.The preferential organic ligand selected is formic acid, acetic acid, pyrrole
Pyridine, succinic acid, tartaric acid, maleic acid, fumaric acid, isonicotinic acid, terephthalic acid (TPA), 2,5-
Dihydric para-phthalic acid, 1,3- phthalic acids, 4,4 '-bipyridyl, 2-methylimidazole, 2- nitroimidazoles,
One or more in imidazoles；Metal ion be selected from aluminium, iron, magnesium, cobalt, nickel, copper, zinc, zirconium,
One or more in lanthanum.The metal-organic framework material for being used is porous adsorbing material, N2Compare table
Area is between 20-2000m2/ g, between 0.4-2nm, preferential recommendation uses average hole to average pore size
Material of the footpath between 0.4-0.8nm.
The invention provides the preparation method of a class ordered structure sorbing material, its preparation method is included such as
Lower step：
(1) metal-organic framework material powder is added in solvent under agitation, stirs 0.5-5
Hour forms mixed slurry；
(2) binding agent is added in mixed slurry, stirs to form coating slurry；
(3) coating is passed through into spraying, brushing or dipping method in fiber cloth side or two side tables with slurry
Face forms coating；
(4) fiber cloth rolls into column, and ordered structure sorbing material is prepared with activation by drying.
The preparation method of ordered structure sorbing material involved in the present invention, needs during prepares coating slurry
Using a large amount of solvent scattered adsorption material powders, solvent for use is water, methyl alcohol, ethanol when preparing slurry
With the mixture of one or more in other low boiling point organic solvents.Preferential recommendation is used in the present invention
, used as dispersion solvent, water is cheap, it is easy to operate for water, environmental protection.Hold in aqueous solvent for some
The sorbent material that the destruction of sorbing material pore structure or possible adsorption separation performance decline is easily caused, then may be used
Can need using part organic solvent, above-mentioned organic solvent can be methyl alcohol, ethanol and other low boilings
One or more in organic solvent of mixture, preferential recommendation uses nontoxic, inexpensive ethanol conduct
Organic solvent.
The preparation method of a class ordered structure sorbing material involved in the present invention, prepares coating slurry
When need to use binding agent, for strengthening matrix and sorbing material powder binding ability each other, glue
Knot agent is the inorganic binder or organic bond that can be scattered in solvent.The inorganic binder can
Think the one kind or its mixed sols binding agent in Ludox, Alumina gel, zirconium colloidal sol and titanium colloidal sol；This
The described organic binder bond of invention for can in water or organic solvent scattered epoxy resin, phenolic resin,
One kind in acrylic resin, polyurethane, makrolon, polyvinyl alcohol, polyethylene glycol or two kinds with
On mixture.
The preparation method of a class ordered structure sorbing material involved in the present invention, prepares coating slurry
By using appropriate mechanical means certain thickness coating, the slurry must be formed in matrix surface
Coating method is mechanically spraying, brush or the various methods of impregnating in one kind, technical staff can be with
Adjustment coating paste concentration and coating time adjust coating layer thickness with coating number of times as needed.
The preparation method of a class ordered structure sorbing material involved in the present invention, when the slurry is coated,
Coating layer thickness typically can be controlled in 50~300 microns, and the preferable coating layer thickness that the present invention recommends is
100~200 microns, the coating layer thickness both can guarantee that larger adsorption capacity, can guarantee that again and inhale faster
Echo desorption rate.
The preparation method of a class ordered structure sorbing material involved in the present invention, in the coating slurry
The part by weight of metal-organic framework material, binding agent and solvent composition is：Metal-organic framework material
Powder 20-50%, binding agent 5-30%, solvent 40-75%.Metal organic frame in above-mentioned three kinds of materials
Material powder decides the adsorption capacity of ordered structure sorbing material, and consumption of binder controls absorption powder
Body material and ordered structure sorbing material matrix are firmly combined with degree, and solvent load determines that coating is starched
The viscosity of material and the coating layer thickness of single application.It should be noted that the binder component in slurry is in itself
Without absorption and separating property, its consumption may result in final ordered structure sorbing material absorption to be held
The reduction of amount, therefore recommend in the present invention under conditions of ordered structure firmness is permitted, subtract as far as possible
The usage amount of few binding agent.The correlation engineering technical staff in actual overall sorbing material preparation process
The usage amount of each component according to actual needs in above-mentioned amount ranges, can be adjusted.
Class ordered structure sorbing material involved in the present invention and preparation method thereof, it is characterised in that institute
The part by weight for stating metal-organic framework material powder, binding agent and matrix component in sorbing material is：
Metal-organic framework material powder 30-92%, binding agent 5-30%, matrix 3-40%.
Class ordered structure sorbing material involved in the present invention and preparation method thereof, matrix material after coating
Roll-forming by after expecting suitably to dry at room temperature, dries 0.1-4 small under present invention recommendation room temperature condition
When, preferably 0.5-2 hours.
Class ordered structure sorbing material involved in the present invention and preparation method thereof, it is characterised in that institute
Stating sorbing material has abundant pore structure, and uniform pore-size distribution is adsorbed and desorption rate faster；
Langmuir methods N2Specific surface area is more than 100m2/ g, pore-size distribution between 0.4-2nm, especially
The purification process such as isolation of purified and concentration purification suitable for atm number admixture of gas, can be preferentially used for
The gas absorption separation process of quick transformation or alternating temperature.
Ordered structure sorbing material of the present invention has compared with the sorbing material that existing adsorption technology is used
There is following significant advantage：
(1) sorbing material preparation process is simple is convenient, and repeatability is easily controlled, and preparation cost is low.
(2) sorbing material wide adaptation range, can need the variously-shaped overall structure of shaping according to application
Sorbing material component, material is easy to filling.
(3) the ordered structure sorbent assemblies bed resistance prepared by the present invention is low, and production efficiency is high,
Adsorption operations production cost is reduced, power consumption is saved.
(4) the ordered structure sorbent material prepared by the present invention, it is adaptable to atm number quick adsorption point
From and purification process, be suitable for the adsorption separation process that can complete multiple cycle period per minute,
It is particularly suited for the pressure-swing absorption process that switching frequency is up to more than scale for several times per minute, all
It is multi-field to have broad application prospects.
The ordered structure sorbing material preparation process is simple, reproducible, sorbing material has abundant
Loose structure, adsorption and desorption speed is fast when being separated for gas absorption, is particularly well-suited to air
Measure the isolation of purified of admixture of gas and concentrate the purification process such as purification.
Specific embodiment
The present invention is described further with reference to embodiment, but it is not thereby limiting the invention.
Embodiment 1：
Metal organic frame sorbing material ZIF-8：BET specific surface area 1350m2/ g, 2-5 μm of particle diameter,
Average pore size 0.9nm.
Measure 200ml water and make solvent, 100g metal organic frame sorbing material powders are weighed, by powder
It is dividedly in some parts in solvent under agitation, stirs 2 hours and form mixed slurry.In mixed slurry
Middle addition 30g adhesive for polyurethane, high-speed stirred forms uniform coating slurry for 3 hours.Slurry
Middle each component part by weight is：Sorbing material powder 30.3%, solvent 60.6%, adhesive 9.1%.
Make matrix from silicon dioxide fibre cloth, slurry is coated uniformly on by matrix table using mechanically spraying mode
Face, 140 μm of coating layer thickness.Coated matrix is spontaneously dried at room temperature, time 2 h,
Then cylindric entire normalization structure sorbing material is rolled into.
Embodiment 2：
Metal organic frame sorbing material CuBTC：BET specific surface area 1550m2/ g, average grain diameter 5
μm, average pore size 0.75nm.
Measure 200ml water and make solvent with 200mL ethanol, weigh 100g metal organic frame adsorption materials
Feed powder body, powder is dividedly in some parts in solvent under agitation, is stirred 1 hour and is formed mixing slurry
Material.Added in mixed slurry：70g Ludox, high-speed stirred forms uniform coating slurry for 1 hour
Material.Each component part by weight is in slurry：Sorbing material powder 23.8%, solvent 59.5%, adhesive
16.7%.Make matrix from silicon dioxide fibre cloth, slurry is coated uniformly on by matrix using brushing mode
Surface, 130 μm of coating layer thickness.Coated matrix is spontaneously dried at room temperature, the time 0.5 is small
When, then roll into cylindric entire normalization structure sorbing material.
Embodiment 3：
Metal organic frame sorbing material Al-BDC：BET specific surface area 1250m2/ g, particle diameter 2-5
μm, average pore size 0.75nm.
Measure 200ml ethanol and make solvent, weigh 100g metal organic frame sorbing material powders, will
Powder is dividedly in some parts in solvent under agitation, is stirred 0.5 hour and is formed mixed slurry.In mixing
Added in slurry：50g epoxy resin adhesives, high-speed stirred forms uniform coating slurry for 2 hours.
Each component part by weight is in slurry：Sorbing material powder 28.6%, solvent 57.1%, adhesive 14.3%.
Make matrix from zirconium oxide fiber cloth, slurry be coated uniformly on by matrix surface using mechanically spraying mode,
150 μm of coating layer thickness.Coated matrix is spontaneously dried at room temperature, 0.5 hour time, so
After roll into cylindric entire normalization structure sorbing material.
Above example is only used for being described in further detail the content of the invention of the invention, but should not
This scope for being interpreted as above-mentioned theme of the invention is only limitted to above-described embodiment.On the present invention is not departed from
State in the case of technological thought, according to this area common technological know-how and conventional means, that makes is various
Replace and change, all should be included in the range of the present invention should protect.
Claims (10)
1. a kind of preparation method of ordered structure sorbing material, it is characterised in that：The sorbing material by
Metal-organic framework material, binding agent and fiber cloth matrix are constituted, and its preparation method and step include：
(1) metal-organic framework material powder is added in solvent under agitation, stirs 0.5-5
Hour forms mixed slurry；
(2) binding agent is added in mixed slurry, stirs to form coating slurry；
(3) coating is passed through into spraying, brushing or dipping method in fiber cloth side or two side tables with slurry
Face forms coating；
(4) fiber cloth rolls into column, and ordered structure sorbing material is prepared with activation by drying.
2. preparation method according to claim 1, it is characterised in that：The metal organic frame
Material is by the suction with loose structure that ligand complex is formed in a solvent of metal ion, organic ligand
Enclosure material；Organic ligand can select to be formic acid, acetic acid, pyridine, succinic acid, tartaric acid, suitable fourth
Enedioic acid, fumaric acid, isonicotinic acid, terephthalic acid (TPA), 2,5- dihydric para-phthalic acids, 1,3- benzene two
One or two or more kinds in formic acid, 4,4 '-bipyridyl, 2-methylimidazole, 2- nitroimidazoles, imidazoles；
Metal ion can be selected from one kind or two kinds in aluminium, iron, magnesium, cobalt, nickel, copper, zinc, zirconium, lanthanum
More than.
3. preparation method according to claim 1, it is characterised in that：The coating paste is with molten
Agent is the mixture of one or two or more kinds in water, methyl alcohol, ethanol, ethyl acetate or butyl acetate.
4. preparation method according to claim 1, it is characterised in that：The slurry binding agent
It is Alumina gel, Ludox, epoxy resin, phenolic resin, acrylic resin, polyurethane, poly- carbonic acid
The mixture of one or two or more kinds in ester, polyvinyl alcohol, polyethylene glycol.
5. preparation method according to claim 1, it is characterised in that：The fiber cloth matrix material
Expect to be silicon dioxide fibre cloth, alumina fibre cloth, zirconium oxide fiber cloth, polyester fiber cloth, polypropylene fibre
Fiber cloth, aryl fiber cloth, polyester fiber cloth, vinylon fibre cloth, spandex fibre cloth, cotton and charcoal
One kind in fiber cloth.
6. preparation method according to claim 1, it is characterised in that：The painting of the slurry coating
Thickness degree is 50~300 microns；The preferable coating layer thickness of the slurry is 100~200 microns.
7. preparation method according to claim 1, it is characterised in that：The ordered structure absorption
The part by weight of metal-organic framework material powder, binding agent and fiber cloth matrix component is in material：
Metal-organic framework material powder 30-92%, binding agent 5-30%, matrix 3-40%.
8. preparation method according to claim 1, it is characterised in that：Gold in the coating slurry
Category organic framework materials, the part by weight of binding agent and solvent composition are：Metal-organic framework material powder
Body 20-50%, binding agent 5-30%, solvent 40-75%.
9. the ordered structure sorbing material that prepared by a kind of any preparation methods of claim 1-8.
10. the application of ordered structure sorbing material described in a kind of claim 9, it is characterised in that：Institute
Ordered structure sorbing material is stated suitable for the isolation of purified of admixture of gas or concentration purification process, can be excellent
First it is used for the gas absorption separation process of transformation or alternating temperature.
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| CN110982087B (en) * | 2019-12-18 | 2022-05-24 | 中国农业科学院农业质量标准与检测技术研究所 | Metal-organic framework material and preparation method and application thereof |
| CN113117647A (en) * | 2019-12-31 | 2021-07-16 | 中国石油化工股份有限公司 | Foam metal supporting adsorption material and preparation method thereof |
| CN113117647B (en) * | 2019-12-31 | 2023-07-28 | 中国石油化工股份有限公司 | Foam metal supporting adsorption material and preparation method thereof |
| CN115209986A (en) * | 2020-03-04 | 2022-10-18 | 埃克森美孚技术与工程公司 | Method for preparing metal-organic framework composite material |
| CN112755955A (en) * | 2020-12-24 | 2021-05-07 | 赣南师范大学 | Preparation method of light honeycomb molecular sieve purification module |
| CN113521880A (en) * | 2021-06-30 | 2021-10-22 | 武汉理工大学 | Photothermal regeneration mask core layer material and preparation method thereof |
| CN113521880B (en) * | 2021-06-30 | 2024-07-02 | 武汉理工大学 | Photothermal regeneration mask core layer material and preparation method thereof |
| CN114659701A (en) * | 2022-03-04 | 2022-06-24 | 武汉理工大学 | High-sensitivity gas pressure sensor for rapidly desorbing gas and preparation method thereof |
| CN114659701B (en) * | 2022-03-04 | 2023-09-26 | 武汉理工大学 | High-sensitivity air pressure sensor for rapidly desorbing gas and preparation method thereof |
| CN115193396A (en) * | 2022-05-12 | 2022-10-18 | 北京科技大学 | Integral adsorbent and preparation method thereof |
| CN115193396B (en) * | 2022-05-12 | 2023-06-09 | 北京科技大学 | Integral adsorbent and preparation method thereof |
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