CN103566911A - Method for manufacturing carbon molecular sieve capable of enlarging contact area between carbon molecular sieve and gas - Google Patents
Method for manufacturing carbon molecular sieve capable of enlarging contact area between carbon molecular sieve and gas Download PDFInfo
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- CN103566911A CN103566911A CN201210283218.3A CN201210283218A CN103566911A CN 103566911 A CN103566911 A CN 103566911A CN 201210283218 A CN201210283218 A CN 201210283218A CN 103566911 A CN103566911 A CN 103566911A
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- carbon molecular
- molecular sieve
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 79
- 239000002808 molecular sieve Substances 0.000 title claims abstract description 73
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 230000001788 irregular Effects 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract 3
- 238000001125 extrusion Methods 0.000 claims description 8
- 238000013467 fragmentation Methods 0.000 claims description 2
- 238000006062 fragmentation reaction Methods 0.000 claims description 2
- 238000007796 conventional method Methods 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 43
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 19
- 239000007789 gas Substances 0.000 abstract description 18
- 239000002245 particle Substances 0.000 abstract description 4
- 238000001179 sorption measurement Methods 0.000 abstract description 4
- 241000219793 Trifolium Species 0.000 abstract 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 18
- 239000000463 material Substances 0.000 description 18
- 238000003763 carbonization Methods 0.000 description 14
- 239000002994 raw material Substances 0.000 description 12
- 239000005011 phenolic resin Substances 0.000 description 8
- 229920001568 phenolic resin Polymers 0.000 description 8
- 238000000465 moulding Methods 0.000 description 7
- 239000000853 adhesive Substances 0.000 description 6
- 230000001070 adhesive effect Effects 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 6
- 239000011280 coal tar Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 230000001404 mediated effect Effects 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000004064 recycling Methods 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 238000010792 warming Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 229910001873 dinitrogen Inorganic materials 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- 239000003463 adsorbent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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Abstract
The invention relates to a method for manufacturing a carbon molecular sieve in a hollow cylinder shape, a clover shape or other irregular shapes so as to enlarge the contact area between the carbon molecular sieve and gas. The larger the outer surface area of the carbon molecular sieve is, the better the gas yield is improved. Existing carbon molecular sieves at home and abroad are commonly in solid cylinder shapes or spherical shapes, the outer surface areas of the carbon molecular sieves are enlarged by continuously reducing the particle sizes, and the current particle sizes reach about 1mm, so that the method is limited in the aspect of enlarging the outer surface area. By changing a banded extruder mould, in the method, the carbon molecular sieve can be extruded into the hollow cylinder shape, the clover shape or other irregular shapes or gaps or holes can be additionally formed in the outer surface of the existing solid cylinder shape under the condition of guaranteeing the same strength and quality. The method has the advantages of being easy to operate, high in production efficiency and relatively low in production cost, effectively enlarging the contact area between the carbon molecular sieve and gas, finally increasing the gas yield of a pressure swing adsorption (PSA) nitrogen making machine, relatively well saving energy, reducing the consumption, and the like.
Description
Technical field
The present invention relates to the carbon molecular sieve manufacture method of a kind of increase and gas contact area.
Background technology
Carbon molecular sieve is a kind of new adsorbent, is pressure-variable adsorption (being called for short P.S.A) the air separation nitrogen-enriching adsorbent of current engineering circles first-selection, is widely used in air separation to produce nitrogen-rich gas.Since carbon molecular sieve invention, people conduct in-depth research it, wherein the triumphant propaganda and education of the dell of Japan Nagoya university awards that (special permission publication number: the separated adsorption capacity that explicitly points out carbon molecular sieve 2003-1047204) not only depends on its inner ratio surface area (micropore surface is long-pending) and aperture homogeneity also depends on the contact area of itself and ambient atmos in its patent " carbon molecular sieve and the application in pressure-variable adsorption thereof ".Factor of created gase is the important performance indexes of carbon molecular sieve, and that the external surface area of carbon molecular sieve is the contact area of itself and gas is larger, and factor of created gase is higher, simultaneously more energy-saving and cost-reducing.Along with the development of forming machine and forming lubricant, kneading agent, the particle diameter of carbon molecular sieve is done less and less, thereby makes the ability of oxygen nitrogen in the separated air of carbon molecular sieve more and more stronger, and the purity of producing nitrogen is also more and more higher, can loss-rate constantly decline.Except fibrous, membranaceous and powdery carbon molecular sieve, the face shaping of nitrogen-preparing carbon molecular sieves both domestic and external generally adopts filled circles column type or ball-type at present, and this has just limited the contact area of itself and gas.Studies have shown that the irregularly shaped raising that is more conducive to external surface area, we find that by carbon molecular sieve, changing its face shaping is open circles column type, trifolium-shaped, irregularly shaped and increase seam ditch or hole at the outer surface of existing filled circles column type, can greatly improve the ability of its divided gas flow.
Summary of the invention
The object of the invention is in order to break through the limitation that conventional carbon molecular sieve column type or ball-type profile and gas contact area are less, provide a kind of technique simply, more effectively to improve the carbon molecular sieve preparation method with gas contact area.
The present invention solves the technical scheme that its technical problem is taked, become open circles column type or trifolium-shaped etc. irregularly shaped and increase seam ditch or hole at the outer surface of existing filled circles column type carbon molecular sieve extrusion, it is characterized in that: carbon molecular sieve raw material (phenolic resins insulating foam leftover pieces or flower mud leftover pieces) are pulverized, mediate with kneading agent, by changing the mould of banded extruder, to be extruded into open circles column type or trifolium-shaped etc. irregularly shaped, or the outer surface at existing column type increases seam ditch or hole, after moulding, deposit and adjust hole, carbonization, preparing qualified carbon molecular sieve encapsulates.
Its concrete preparation method (accompanying drawing 2) is as follows:
Pulverize and grind: the phenolic resins insulating foam leftover pieces of ash content≤10% or flower mud leftover pieces are tentatively pulverized by ball mill, then through oven for drying moisture wherein, then ground more than 20 hours through ultra-fine ball mill, grain size of micropowder is controlled at 5～20 microns.
Mediate: the adhesive of ground raw material and phenolic resins, coal tar and water composition is mediated in combinatorial introduction kneader by a certain percentage.
Extrusion: the column type banded extruder mould that transformation conventional carbon molecular sieve is used, adopt the various novel dies shown in accompanying drawing one, by carbon molecular sieve base material extruded moulding, be open circles column type or trifolium-shaped or the apertured filled circles column type of outer surface.
Carbonization, deposition are adjusted hole: the carbon molecular sieve base material of extruded moulding is heated to 300 ℃ of left and right in resistance furnace; pass into nitrogen protection; when being warming up to 800 ℃ of left and right, constant temperature is one hour; make base material carbonization and form hole; recycling nitrogen passes into reagent benzene or coconut wet goods organic matter in resistance furnace; make the substrate surface carbon deposit plug-hole of carbonization pore-forming, carbon molecular sieve is taken out after cooling.
Detect encapsulation: the sampling of carbon molecular sieve finished product, pack in miniature nitrogen analysis device processed, detect and qualifiedly encapsulate while carbon molecular sieve finished product being cooled to 60 ℃ of left and right, otherwise melt down, reproduce.
Accompanying drawing explanation
The die drawing that accompanying drawing 1 is erose banded extruder, left, center, right is respectively the elevation, front elevation of this mould and specific to the detail view in each hole.Wherein first row mould is for increasing by 6 ditches by traditional cylinder type carbon molecular sieve outer surface; Second row mould is for being extruded into hollow type by carbon molecular sieve; The 3rd row's mould is for being extruded into trifolium-shaped by carbon molecular sieve.
The basic production process chart that accompanying drawing 2 is carbon molecular sieve.
The specific embodiment
Below in conjunction with describing the present invention by embodiment and comparative example.
Comparative example 1:
Conventional carbon system with molecular sieve for preparing making method: the colored mud leftover pieces of ash content≤10% are tentatively pulverized by raw material ball grinding machine, then through oven for drying moisture wherein, then ground more than 20 hours through ultra-fine ball mill, grain size of micropowder is controlled at 5～20 microns; The adhesive of ground raw material and phenolic resins, coal tar and water composition is mediated in combinatorial introduction kneader by a certain percentage; The column type banded extruder mould that uses conventional carbon molecular sieve to use, it is 1mm that carbon molecular sieve base material extrusion is become to diameter, the filled circles column type that length is 2mm; The carbon molecular sieve base material of extruded moulding is heated to 300 ℃ of left and right in resistance furnace; pass into nitrogen protection; when being warming up to 800 ℃ of left and right, constant temperature is one hour; make base material carbonization and form hole; recycling nitrogen passes into reagent benzene in resistance furnace; make the substrate surface carbon deposit plug-hole of carbonization pore-forming, carbon molecular sieve is taken out after cooling.After tested, qualified carbon molecular sieve finished product factor of created gase under 0.8Mpa pressure, 99.99% nitrogen gas concn can reach 140L/h.Kg, gas consumption ratio is 4.5 (gas consumption ratios: produce the needed air capacity of nitrogen that 1 cube of purity is 99.99%, i.e. the ratio of air and nitrogen).
Embodiment 1:
There is the filled circles column type carbon molecular sieve manufacture method of 6 ditches on surface: the colored mud leftover pieces of ash content≤10% are tentatively pulverized by raw material ball grinding machine, then through oven for drying moisture wherein, through ultra-fine ball mill, grind more than 20 hours, grain size of micropowder is controlled at 5～20 microns again; The adhesive of ground raw material and phenolic resins, coal tar and water composition is mediated in combinatorial introduction kneader by a certain percentage; Use improved column type banded extruder mould, it is 1mm that carbon molecular sieve base material extrusion is become to diameter, the filled circles column type that length is 1mm, and there is the ditch of 6 rules in its outer surface; The carbon molecular sieve base material of extruded moulding is heated to 300 ℃ of left and right in resistance furnace; pass into nitrogen protection; when being warming up to 800 ℃ of left and right, constant temperature is one hour; make base material carbonization and form hole; recycling nitrogen passes into reagent benzene in resistance furnace; make the substrate surface carbon deposit plug-hole of carbonization pore-forming, carbon molecular sieve is taken out after cooling.After tested, qualified carbon molecular sieve finished product factor of created gase under 0.8Mpa pressure, 99.99% nitrogen gas concn can reach 180L/h.Kg, and gas consumption ratio is 4.15.
Embodiment 2:
Open circles column type carbon molecular sieve manufacture method: the colored mud leftover pieces of ash content≤10% are tentatively pulverized by raw material ball grinding machine, then through oven for drying moisture wherein, then ground more than 20 hours through ultra-fine ball mill, grain size of micropowder is controlled at 5～20 microns; The adhesive of ground raw material and phenolic resins, coal tar and water composition is mediated in combinatorial introduction kneader by a certain percentage; Use improved open circles column type banded extruder mould, it is 1mm that carbon molecular sieve base material extrusion is become to diameter, and length is 1mm, and there is the open circles column type of 0.06mm aperture centre; The carbon molecular sieve base material of extruded moulding is heated to 300 ℃ of left and right in resistance furnace; pass into nitrogen protection; when being warming up to 800 ℃ of left and right, constant temperature is one hour; make base material carbonization and form hole; recycling nitrogen passes into reagent benzene in resistance furnace; make the substrate surface carbon deposit plug-hole of carbonization pore-forming, carbon molecular sieve is taken out after cooling.After tested, qualified carbon molecular sieve finished product factor of created gase under 0.8Mpa pressure, 99.99% nitrogen gas concn can reach 200L/h.Kg, and gas consumption ratio is 3.9.
Embodiment 3:
Trifolium-shaped carbon molecular sieve manufacture method: the colored mud leftover pieces of ash content≤10% are tentatively pulverized by raw material ball grinding machine, then through oven for drying moisture wherein, then ground more than 20 hours through ultra-fine ball mill, grain size of micropowder is controlled at 5～20 microns; The adhesive of ground raw material and phenolic resins, coal tar and water composition is mediated in combinatorial introduction kneader by a certain percentage; Use improved trifolium-shaped banded extruder mould, it is 1mm that carbon molecular sieve base material extrusion is become to diameter, the trifolium-shaped that length is 1mm; The carbon molecular sieve base material of extruded moulding is heated to 300 ℃ of left and right in resistance furnace; pass into nitrogen protection; when being warming up to 800 ℃ of left and right, constant temperature is one hour; make base material carbonization and form hole; recycling nitrogen passes into reagent benzene in resistance furnace; make the substrate surface carbon deposit plug-hole of carbonization pore-forming, carbon molecular sieve is taken out after cooling.After tested, qualified carbon molecular sieve finished product factor of created gase under 0.8Mpa pressure, 99.99% nitrogen gas concn can reach 178L/h.Kg, and gas consumption ratio is 4.2.
Embodiment 4:
Difform carbon molecular sieve manufacture method: the colored mud leftover pieces of ash content≤10% are tentatively pulverized by raw material ball grinding machine, then ground more than 20 hours through ultra-fine ball mill, grain size of micropowder is controlled at 5～20 microns, the adhesive of ground raw material and phenolic resins, coal tar and water composition is mediated in combinatorial introduction kneader by a certain percentage, use conventional column type banded extruder mould, it is 1.3mm that carbon molecular sieve base material extrusion is become to diameter, length is the column type base material of 1.5mm, in resistance furnace, be heated to 300 ℃ of left and right, pass into nitrogen protection, when being warming up to 800 ℃ of left and right, constant temperature is one hour, make base material carbonization and form hole, recycling nitrogen passes into reagent benzene in resistance furnace, make the substrate surface carbon deposit plug-hole of carbonization pore-forming, after cooling, carbon molecular sieve is taken out, after slight fragmentation, become irregular shape carbon molecular sieve, finally by classifying screen, sieve, choose particle diameter at the irregular carbon molecular sieve of 14～25 object.After tested, qualified carbon molecular sieve finished product factor of created gase under 0.8Mpa pressure, 99.99% nitrogen gas concn can reach 185L/h.Kg, and gas consumption ratio is 4.0.
By above 4 embodiment, can be found out, trifolium-shaped, open circles column type, the improved filled circles column type of outer surface and through the irregular shape carbon molecular sieve of soft pulverizing, its properties of product are generally higher than traditional filled circles column type, in the situation that meeting same performance requirement, erose carbon molecular sieve has stronger economic benefit for PSA nitrogen making machine.
Claims (2)
1. the carbon molecular sieve manufacture method of an increase and gas contact area, it is characterized in that: the solid cylinder body profile or the ball-type profile that change conventional carbon molecular sieve, make open circles column type, trifolium-shaped, irregular shape, outer surface in existing filled circles column type increases gap, hole, thereby increases carbon molecular sieve and gas contact area.
2. prepare according to claim 1 the method for carbon molecular sieve, it is characterized in that: extrusion is that the carbon molecular sieve finished product of filled circles column type is sent into and in disintegrating machine, carried out slight fragmentation according to a conventional method, become irregular shape carbon molecular sieve, by classifying screen, sieve, choose the irregular shape carbon molecular sieve of 10～35 object as final qualified finished product.
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| CN201210283218.3A CN103566911A (en) | 2012-08-03 | 2012-08-03 | Method for manufacturing carbon molecular sieve capable of enlarging contact area between carbon molecular sieve and gas |
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| CN201210283218.3A CN103566911A (en) | 2012-08-03 | 2012-08-03 | Method for manufacturing carbon molecular sieve capable of enlarging contact area between carbon molecular sieve and gas |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6284021B1 (en) * | 1999-09-02 | 2001-09-04 | The Boc Group, Inc. | Composite adsorbent beads for adsorption process |
| CN101010257A (en) * | 2004-08-30 | 2007-08-01 | 可乐丽化学株式会社 | Method of separating nitrogen gas and molecular sieve carbon |
| CN101371979A (en) * | 2008-10-10 | 2009-02-25 | 天津大学 | A kind of adsorbent for adsorbing trace ethylene in carbon dioxide and preparation method thereof |
| CN101544362A (en) * | 2008-03-28 | 2009-09-30 | 胡耀明 | Method for manufacturing carbon molecular sieve by using phenolic resin waste |
| CN101642701A (en) * | 2009-08-14 | 2010-02-10 | 威海华泰分子筛有限公司 | Method for preparing carbon molecular sieve from flower mud leftover material |
| CN101711976B (en) * | 2009-10-27 | 2011-06-15 | 湖州强马分子筛有限公司 | Method for preparing nitrogen-producing carbon molecular sieve |
-
2012
- 2012-08-03 CN CN201210283218.3A patent/CN103566911A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6284021B1 (en) * | 1999-09-02 | 2001-09-04 | The Boc Group, Inc. | Composite adsorbent beads for adsorption process |
| CN101010257A (en) * | 2004-08-30 | 2007-08-01 | 可乐丽化学株式会社 | Method of separating nitrogen gas and molecular sieve carbon |
| CN101544362A (en) * | 2008-03-28 | 2009-09-30 | 胡耀明 | Method for manufacturing carbon molecular sieve by using phenolic resin waste |
| CN101371979A (en) * | 2008-10-10 | 2009-02-25 | 天津大学 | A kind of adsorbent for adsorbing trace ethylene in carbon dioxide and preparation method thereof |
| CN101642701A (en) * | 2009-08-14 | 2010-02-10 | 威海华泰分子筛有限公司 | Method for preparing carbon molecular sieve from flower mud leftover material |
| CN101711976B (en) * | 2009-10-27 | 2011-06-15 | 湖州强马分子筛有限公司 | Method for preparing nitrogen-producing carbon molecular sieve |
Non-Patent Citations (1)
| Title |
|---|
| 朱洪法，等: "《催化剂制备及应用技术》", 30 June 2011, article "异形催化剂的成型", pages: 350 - 2 * |
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Application publication date: 20140212 |