CN105905893A - Ramie fiber carbon molecular sieve - Google Patents
Ramie fiber carbon molecular sieve Download PDFInfo
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- CN105905893A CN105905893A CN201610361490.7A CN201610361490A CN105905893A CN 105905893 A CN105905893 A CN 105905893A CN 201610361490 A CN201610361490 A CN 201610361490A CN 105905893 A CN105905893 A CN 105905893A
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- molecular sieve
- ramee
- carbon molecular
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- nitrogen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
Abstract
The invention discloses a preparation method of a ramie fiber carbon molecular sieve. The method comprises the following steps: (1) modifying ramie fiber; (2) bonding, namely, mixing the following raw materials in parts by mass: 52-58 parts of modified ramie fiber powder, 5-9 parts of walnut shell flour, 6 parts of mica powder, 25 parts of plant starch and 18-22 parts of water, and bonding for 35 minutes; (3) molding; (4) carbonizing and performing pore adjustment treatment; and (5) preparing a finished product, namely, rapidly cooling a certain amount of high-temperature samples in a vacuum state, rapidly evaluating the aperture distribution situation by using a specific surface area and pore structure distributor, detecting so as to obtain the carbon molecular sieve of which the aperture is 1.8-2.5 angstrom, and controlling the sealing temperature of a product to be 65-72 DEG C.
Description
Technical field
The invention belongs to macromolecule chemical industry technical field, be specifically related to a kind of ramee carbon molecular sieve.
Background technology
Carbon molecular sieve (Carbon Molecular Sieve, CMS) it is broadly the one nonpolar carbonaceous absorption material having nano level superfine micropore, it is the activated carbon of micropore distribution uniform in the narrow sense, because it is made up of with crystallization charcoal amorphous carbon, so the pore structure of carbon molecular sieve is the most flourishing, and there is the surface character of uniqueness.Because the wedge shape micropore of CMS is close with adsorbed molecular diameter size, major part is effective apearture, and has the advantages that to adjust CMS pore size according to molecular size, thus has the ability of screening molecule.Pore structure and stable chemical property that CMS is unique make it be widely used in chemical industry, additionally, be also widely used in fields such as the production of nitrogen hydrogen, waste water process, environmental conservation, military and national defense, canister respirators.
The raw material preparing carbon molecular sieve is a lot, originates the widest.The carbon molecular sieve that pore radiuses and distribution is different can be obtained in theory by different original materials through different preparation technologies.Experiment shows, the raw material of low ash content, high carbon content and high volatile is relatively suitable for preparing high performance carbon molecular sieve.
Prior art is disclosed the method preparing carbon molecular sieve by plurality of raw materials, but does not also have as the report of primary raw material with ramee, this is because ramee do not meet the requirement of low ash content, high carbon content and high volatile.Ramee is contained in ramie leaf, belongs to leaf fibre class.Ramee not yet obtains large-scale development application the most in the world, and Boehmeria is mainly in order to pulping and paper-making, water and soil conservation, making hand woven product.
It is desirable to provide a kind of ramee carbon molecular sieve and preparation technology thereof, by ramee modification, can prepare factor of created gase high, gas consumption ratio is low, energy-conserving and environment-protective, the carbon molecular sieve that oil resistance is good.
Summary of the invention
The technical problem existed based on background technology, the present invention is directed to the problem that background technology exists, the present invention provides a kind of ramee carbon molecular sieve and preparation technology thereof, by to ramee modification, factor of created gase can be prepared high, gas consumption ratio is low, energy-conserving and environment-protective, the carbon molecular sieve that oil resistance is good.
The topmost weakness of carbon molecular sieve is to fear greasy dirt dye, once it is polluted by the oil (oil poisoning), the adsorbance of carbon molecular sieve will be substantially reduced, have a strong impact on product nitrogen ability, regeneration method is i.e. used also to be difficult to recover its adsorbance, so compressed air pretreatment part must be equipped with the special grease trap of high-quality.In a word, carbon molecular sieve to compressed air quality require be: oil content want <
0.003mg/m3；Dirt granule content wants < 01001 μ (three grades of air filters can reach requirement)；Water content pressure leak source is at 0～10 °, and clean compressed air is also without preheating.The fundamental characteristics of carbon molecular sieve is: true density 1.9～2.0g/cm3；Grain density 0.9～1.1g/ cm3；Loading density 0.63～0.68g/ cm3；Porosity 0.35～0.41；Void content 0.5～0.6cm3/g；Specific surface area 450～550m2/g；Average pore size 0.4～0.7nm.
The purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method of ramee carbon molecular sieve, its step is as follows:
(1) ramee is modified:
Pretreatment: ramee puts into submergence in the hydrochloric acid solution of 0.3% concentration, constant temperature 20-25 DEG C processes 65min, clean by clean water；
Ferment treatment: the cellulase of preparation 0.6-0.9%, 0.1% Lactose enzyme, the solution of 0.2% pectase, pretreated ramee is put into wherein, then constant temperature 38 DEG C processes 3-5 hour, then beats sub-wire and obtains the ramee of modification, 80 DEG C of drying, grinds crosses 50 mesh sieves, obtains modified ramie powder；
(2) bonding: will be mixed by following raw material according to mass fraction: take modified ramie powder 52-58 part, walnut shell powder 5-9 part, 6 parts of mica powders, plant amylum 25 parts, 18-22 part water bond, and the bonding time is 35min；
(3) molding: the raw material bonded is carried out extruded moulding with twin screw band extrusion molding machine, by the material dry of forming；
(4) carbonization and tune hole process: carry out carbonization in the raw material dried well is imported converter and adjust hole; temperature rise rate 15 DEG C/min; carbonization is carried out under the conditions of 850 DEG C-900 DEG C; after reaching the highest temperature; at the protection borehole cooling of nitrogen to 700 DEG C of constant temperature, will be passed through the flow-control of nitrogen at 4 cubes ms/h, adjusting hole agent flux is that 18 ml/min carry out aperture adjustment; 90 minutes adjustment time, product maintains 780 DEG C of constant temperature with nitrogen protection in converter；
(5) finished product: take a certain amount of high temp samples, quickly cool down at vacuum state, by specific surface area and its pore-size distribution situation of pore size distribution$ instrument Fast Evaluation, obtains 1.8-2.5 angstrom of aperture carbon molecular sieve after testing, and the package temperature of product controls at 65 DEG C-72 DEG C.
The invention have benefit that:
Present invention process is simple, uses Boehmeria to limit as raw material, the raw material breaching carbon molecular sieve, and low price, the carbon molecular sieve excellent performance prepared, gas consumption ratio is low, and oil resistant pollutes, and energy-conserving and environment-protective have market potential very much.
Detailed description of the invention
Embodiment
1
:
A kind of preparation method of ramee carbon molecular sieve, its step is as follows:
(1) ramee is modified:
Pretreatment: ramee puts into submergence in the hydrochloric acid solution of 0.3% concentration, constant temperature 20 DEG C processes 65min, clean by clean water；
Ferment treatment: the cellulase of preparation 0.9%, 0.1% Lactose enzyme, the solution of 0.2% pectase, pretreated ramee is put into wherein, then constant temperature 38 DEG C processes 3 hours, then beats sub-wire and obtains the ramee of modification, 80 DEG C of drying, grinds crosses 50 mesh sieves, obtains modified ramie powder；
(2) bonding: will be mixed by following raw material according to mass fraction: take 58 parts of modified ramie powder, walnut shell powder 5 parts, 6 parts of mica powders, 25 parts, 22 parts water of plant amylum bond, and the bonding time is 35min；
(3) molding: the raw material bonded is carried out extruded moulding with twin screw band extrusion molding machine, by the material dry of forming；
(4) carbonization and tune hole process: carry out carbonization in the raw material dried well is imported converter and adjust hole; temperature rise rate 15 DEG C/min; carbonization is carried out under the conditions of 850 DEG C; after reaching the highest temperature; at the protection borehole cooling of nitrogen to 700 DEG C of constant temperature, will be passed through the flow-control of nitrogen at 4 cubes ms/h, adjusting hole agent flux is that 18 ml/min carry out aperture adjustment; 90 minutes adjustment time, product maintains 780 DEG C of constant temperature with nitrogen protection in converter；
(5) finished product: take a certain amount of high temp samples, quickly cool down at vacuum state, by specific surface area and its pore-size distribution situation of pore size distribution$ instrument Fast Evaluation, obtains 1.8-2.5 angstrom of aperture carbon molecular sieve after testing, and the package temperature of product controls at 65 DEG C-72 DEG C.
Result:
Gas consumption ratio: produce the ratio of the air capacity required for the nitrogen that 1 cube of purity is 99.99%, i.e. air and nitrogen,
After tested, cylindrical carbonaceous molecule sieve finished product gas consumption ratio under 0.8Mpa pressure, 99.99% nitrogen gas concn of the present embodiment is 3.8.
Oil content will be at 0.05mg/m3In the environment of, gas consumption ratio remains in that to be 3.9, the carbon molecular sieve lifting that oil resistance is the most traditional.
Embodiment
2
:
A kind of preparation method of ramee carbon molecular sieve, its step is as follows:
(1) ramee is modified:
Pretreatment: ramee puts into submergence in the hydrochloric acid solution of 0.3% concentration, constant temperature 25 DEG C processes 65min, clean by clean water；
Ferment treatment: the cellulase of preparation 0.6%, 0.1% Lactose enzyme, the solution of 0.2% pectase, pretreated ramee is put into wherein, then constant temperature 38 DEG C processes 5 hours, then beats sub-wire and obtains the ramee of modification, 80 DEG C of drying, grinds crosses 50 mesh sieves, obtains modified ramie powder；
(2) bonding: will be mixed by following raw material according to mass fraction: take 52 parts of modified ramie powder, walnut shell powder 9 parts, 6 parts of mica powders, 25 parts, 18 parts water of plant amylum bond, and the bonding time is 35min；
(3) molding: the raw material bonded is carried out extruded moulding with twin screw band extrusion molding machine, by the material dry of forming；
(4) carbonization and tune hole process: carry out carbonization in the raw material dried well is imported converter and adjust hole; temperature rise rate 15 DEG C/min; carbonization is carried out under the conditions of 900 DEG C; after reaching the highest temperature; at the protection borehole cooling of nitrogen to 700 DEG C of constant temperature, will be passed through the flow-control of nitrogen at 4 cubes ms/h, adjusting hole agent flux is that 18 ml/min carry out aperture adjustment; 90 minutes adjustment time, product maintains 780 DEG C of constant temperature with nitrogen protection in converter；
(5) finished product: take a certain amount of high temp samples, quickly cool down at vacuum state, by specific surface area and its pore-size distribution situation of pore size distribution$ instrument Fast Evaluation, obtains 1.8-2.5 angstrom of aperture carbon molecular sieve after testing, and the package temperature of product controls at 65 DEG C-72 DEG C.
Result:
Gas consumption ratio: produce the ratio of the air capacity required for the nitrogen that 1 cube of purity is 99.99%, i.e. air and nitrogen.
After tested, cylindrical carbonaceous molecule sieve finished product gas consumption ratio under 0.8Mpa pressure, 99.99% nitrogen gas concn of the present embodiment is 3.4.
Oil content will be at 0.05mg/m3In the environment of, gas consumption ratio remains in that to be 3.9, the carbon molecular sieve lifting that oil resistance is the most traditional.
Embodiment
3
:
A kind of preparation method of ramee carbon molecular sieve, its step is as follows:
(1) ramee is modified:
Pretreatment: ramee puts into submergence in the hydrochloric acid solution of 0.3% concentration, constant temperature 21 DEG C processes 65min, clean by clean water；
Ferment treatment: the cellulase of preparation 0.8%, 0.1% Lactose enzyme, the solution of 0.2% pectase, pretreated ramee is put into wherein, then constant temperature 38 DEG C processes 4 hours, then beats sub-wire and obtains the ramee of modification, 80 DEG C of drying, grinds crosses 50 mesh sieves, obtains modified ramie powder；
(2) bonding: will be mixed by following raw material according to mass fraction: take 56 parts of modified ramie powder, walnut shell powder 6 parts, 6 parts of mica powders, 25 parts, 20 parts water of plant amylum bond, and the bonding time is 35min；
(3) molding: the raw material bonded is carried out extruded moulding with twin screw band extrusion molding machine, by the material dry of forming；
(4) carbonization and tune hole process: carry out carbonization in the raw material dried well is imported converter and adjust hole; temperature rise rate 15 DEG C/min; carbonization is carried out under the conditions of 860 DEG C; after reaching the highest temperature; at the protection borehole cooling of nitrogen to 700 DEG C of constant temperature, will be passed through the flow-control of nitrogen at 4 cubes ms/h, adjusting hole agent flux is that 18 ml/min carry out aperture adjustment; 90 minutes adjustment time, product maintains 780 DEG C of constant temperature with nitrogen protection in converter；
(5) finished product: take a certain amount of high temp samples, quickly cool down at vacuum state, by specific surface area and its pore-size distribution situation of pore size distribution$ instrument Fast Evaluation, obtains 1.8-2.5 angstrom of aperture carbon molecular sieve after testing, and the package temperature of product controls at 65 DEG C-72 DEG C.
Result:
Gas consumption ratio: produce the ratio of the air capacity required for the nitrogen that 1 cube of purity is 99.99%, i.e. air and nitrogen,
After tested, cylindrical carbonaceous molecule sieve finished product gas consumption ratio under 0.8Mpa pressure, 99.99% nitrogen gas concn of the present embodiment is 3.7.
Oil content will be at 0.05mg/m3In the environment of, gas consumption ratio remains in that to be 3.9, the carbon molecular sieve lifting that oil resistance is the most traditional.
Embodiment
4
:
A kind of preparation method of ramee carbon molecular sieve, its step is as follows:
(1) ramee is modified:
Pretreatment: ramee puts into submergence in the hydrochloric acid solution of 0.3% concentration, constant temperature 24 DEG C processes 65min, clean by clean water；
Ferment treatment: the cellulase of preparation 0.7%, 0.1% Lactose enzyme, the solution of 0.2% pectase, pretreated ramee is put into wherein, then constant temperature 38 DEG C processes 3 hours, then beats sub-wire and obtains the ramee of modification, 80 DEG C of drying, grinds crosses 50 mesh sieves, obtains modified ramie powder；
(2) bonding: will be mixed by following raw material according to mass fraction: take 53 parts of modified ramie powder, walnut shell powder 8 parts, 6 parts of mica powders, 25 parts, 19 parts water of plant amylum bond, and the bonding time is 35min；
(3) molding: the raw material bonded is carried out extruded moulding with twin screw band extrusion molding machine, by the material dry of forming；
(4) carbonization and tune hole process: carry out carbonization in the raw material dried well is imported converter and adjust hole; temperature rise rate 15 DEG C/min; carbonization is carried out under the conditions of 890 DEG C; after reaching the highest temperature; at the protection borehole cooling of nitrogen to 700 DEG C of constant temperature, will be passed through the flow-control of nitrogen at 4 cubes ms/h, adjusting hole agent flux is that 18 ml/min carry out aperture adjustment; 90 minutes adjustment time, product maintains 780 DEG C of constant temperature with nitrogen protection in converter；
(5) finished product: take a certain amount of high temp samples, quickly cool down at vacuum state, by specific surface area and its pore-size distribution situation of pore size distribution$ instrument Fast Evaluation, obtains 1.8-2.5 angstrom of aperture carbon molecular sieve after testing, and the package temperature of product controls at 65 DEG C-72 DEG C.
Result:
Gas consumption ratio: produce the ratio of the air capacity required for the nitrogen that 1 cube of purity is 99.99%, i.e. air and nitrogen,
After tested, cylindrical carbonaceous molecule sieve finished product gas consumption ratio under 0.8Mpa pressure, 99.99% nitrogen gas concn of the present embodiment is 3.5.
Oil content will be at 0.05mg/m3In the environment of, gas consumption ratio remains in that to be 3.9, the carbon molecular sieve lifting that oil resistance is the most traditional.
Embodiment
5
Contrast test:
A kind of preparation method of ramee carbon molecular sieve, its step is as follows:
(1) ramee grinds is crossed 50 mesh sieves, obtain ramee powder；
(2) bonding: will be mixed by following raw material according to mass fraction: take 55 parts of ramee powder, walnut shell powder 7 parts, 6 parts of mica powders, 25 parts, 21 parts water of plant amylum bond, and the bonding time is 35min；
(3) molding: the raw material bonded is carried out extruded moulding with twin screw band extrusion molding machine, by the material dry of forming；
(4) carbonization and tune hole process: carry out carbonization in the raw material dried well is imported converter and adjust hole; temperature rise rate 15 DEG C/min; carbonization is carried out under the conditions of 870 DEG C; after reaching the highest temperature; at the protection borehole cooling of nitrogen to 700 DEG C of constant temperature, will be passed through the flow-control of nitrogen at 4 cubes ms/h, adjusting hole agent flux is that 18 ml/min carry out aperture adjustment; 90 minutes adjustment time, product maintains 780 DEG C of constant temperature with nitrogen protection in converter；
(5) finished product: take a certain amount of high temp samples, quickly cool down at vacuum state, by specific surface area and its pore-size distribution situation of pore size distribution$ instrument Fast Evaluation, obtains 1.8-2.5 angstrom of aperture carbon molecular sieve after testing, and the package temperature of product controls at 65 DEG C-72 DEG C.
Result:
Gas consumption ratio: produce the ratio of the air capacity required for the nitrogen that 1 cube of purity is 99.99%, i.e. air and nitrogen.
After tested, cylindrical carbonaceous molecule sieve finished product gas consumption ratio under 0.8Mpa pressure, 99.99% nitrogen gas concn of the present embodiment is 4.3.
Oil content will be at 0.05mg/m3In the environment of, carbon molecular sieve almost inactivates.
As can be seen here, the technique of the present invention is optimized in the control of raw material, especially the modified technique to ramee, the unexpected performance improving carbon molecular sieve.
The above; it is only the present invention preferably detailed description of the invention; but protection scope of the present invention is not limited thereto; any those familiar with the art is in the technical scope that the invention discloses; according to technical scheme and inventive concept equivalent or change in addition thereof, all should contain within protection scope of the present invention.
Claims (2)
1. a preparation method for ramee carbon molecular sieve, its step is as follows:
(1) ramee is modified:
Pretreatment: ramee puts into submergence in the hydrochloric acid solution of 0.3% concentration, constant temperature 20-25 DEG C processes 65min, clean by clean water；
Ferment treatment: the cellulase of preparation 0.6-0.9%, 0.1% Lactose enzyme, the solution of 0.2% pectase, pretreated ramee is put into wherein, then constant temperature 38 DEG C processes 3-5 hour, then beats sub-wire and obtains the ramee of modification, 80 DEG C of drying, grinds crosses 50 mesh sieves, obtains modified ramie powder；
(2) bonding: will be mixed by following raw material according to mass fraction: take modified ramie powder 52-58 part, walnut shell powder 5-9 part, 6 parts of mica powders, plant amylum 25 parts, 18-22 part water bond, and the bonding time is 35min；
(3) molding: the raw material bonded is carried out extruded moulding with twin screw band extrusion molding machine, by the material dry of forming；
(4) carbonization and tune hole process: carry out carbonization in the raw material dried well is imported converter and adjust hole; temperature rise rate 15 DEG C/min; carbonization is carried out under the conditions of 850 DEG C-900 DEG C; after reaching the highest temperature; at the protection borehole cooling of nitrogen to 700 DEG C of constant temperature, will be passed through the flow-control of nitrogen at 4 cubes ms/h, adjusting hole agent flux is that 18 ml/min carry out aperture adjustment; 90 minutes adjustment time, product maintains 780 DEG C of constant temperature with nitrogen protection in converter；
(5) finished product: take a certain amount of high temp samples, quickly cool down at vacuum state, by specific surface area and its pore-size distribution situation of pore size distribution$ instrument Fast Evaluation, obtains 1.8-2.5 angstrom of aperture carbon molecular sieve after testing, and the package temperature of product controls at 65 DEG C-72 DEG C.
2. the carbon molecular sieve that the preparation method of the ramee carbon molecular sieve described in claim 1 prepares.
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| CN111943196A (en) * | 2020-08-18 | 2020-11-17 | 湖州民强炭业有限公司 | Preparation method of high-performance methane carbon molecular sieve by taking gordon euryale seed shell as raw material |
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| CN105905893B (en) | 2018-10-02 |
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