CN1089028C - Carbon and/or graphite board corrugated regular filler for packed column - Google Patents
Carbon and/or graphite board corrugated regular filler for packed column Download PDFInfo
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- CN1089028C CN1089028C CN97121089A CN97121089A CN1089028C CN 1089028 C CN1089028 C CN 1089028C CN 97121089 A CN97121089 A CN 97121089A CN 97121089 A CN97121089 A CN 97121089A CN 1089028 C CN1089028 C CN 1089028C
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Abstract
The present invention provides entity regular filler for a packed tower. An assembled unit of the entity regular filler is a simple or modified corrugated plate made of carbon and/or graphite and products thereof. Compared with regular filler made of the material of metal, ceramic, plastics or carbon fiber in the prior art, the present invention has the advantages of good corrosion resistance, high mass transfer efficiency, low resistance drop, high universality, etc. The entity regular filler for a packed tower solves the problems of gas-liquid and liquid-liquid mass transfer equipment with high efficiency, high flux and low resistance drop under corrosive environment.
Description
The invention belongs to gas-liquid in the chemical industry, liquid-liquid mass transfer apparatus field, especially a kind of packed tower is simple or the carbon of modification and/or the corrugated plating of graphite and goods thereof with carbon and/or graphite board corrugated entity structured packing, the assembled unit of this structured packing.
Because the scientific research and the technological development of tower packing have obtained huge progress, efficient height, the packed tower that pressure drop is low, liquid holdup is little replace the plate column that efficient is low, pressure drop is high, liquid holdup is big just gradually.Particularly structured packing is the outstanding person in the filler product as the device of low pressure drop, high mass transfer efficiency.It is the tower that gas-liquid, liquid-liquid mass transport process provide efficient, big flux, has promoted the technological progress of gas-liquid, liquid-liquid mass transport process.
Yet, because filler is generally metal (being mainly stainless steel) material in the tower, be difficult to be applicable to the corrosivity system, for example, the high-temperature and high concentration environment of acid, alkali etc.People attempt to solve efficient, the high flux under the corrosive environment, gas-liquid, the liquid-liquid mass transfer problem that lower resistance is fallen always, then New Type Material for example titanium alloy, pottery, and the efficient structured packing of plastics etc. come out one after another.
Though the efficient structured packing of above-mentioned material can remedy the deficiency of the efficient structured packing of stainless steel in some aspects, expose some new problems again simultaneously: for example, titanium and alloy thereof cost an arm and a leg, and not corrosion-resistant to some medium of high-temperature and high concentration; The ceramic packing wall thickness, voidage is low, and bulk density is big, and heat transfer coefficient is low, the crisp cracky of matter and not alkaline-resisting; The structured packing of plastic material is unsuitable for gas-liquid, the liquid-liquid mass transport process under the higher environment of temperature, and is not corrosion-resistant and surface wettability is poor to most of organic solvents.
Carbon and/or graphite product, corrosion-resistant wide ranges, the heat transfer coefficient height, linear expansion coefficient is low, and is high temperature resistant, and density is little, and the surface is less scaling, is both corrosion-resistant and tool thermal conductivity height, inertia nonmetallic materials that linear expansion coefficient is low.(" design of graphite inhibition and generation construction equipment " p.1～3, Science and Technology of Shanghai publishing house)
But it is well-known, carbon and/or graphite product are crisp, can't be processed into structured packing by present filler manufacturing process, so up to now, research report about the structured packing of carbon and/or graphite material is very few, it is 1994 that one piece of date is only arranged, 1,25 U.S. Pat 5,281,479A (denomination of invention: be used for the corrosion-resistant and heat-staple structured packing of mass transfer and heat exchanging process) has mentioned a kind of corrosion-resistant and heat-staple structured packing that is used for mass transfer and heat exchanging process, comprises prefabricated assembled unit, and assembled unit is made of the carbon fibre fabric of carbon fiber-strengthen with carbon fiber or carbon fiber line.
Tower packing is made material according to it can be divided into two classes: entity filler and dictyosome filler.(" the novel structured packing application manual of industrial tower ", p, 5, Liu Naipeng chief editor, 1993.12 printings)
Therefore, US 5,281, and the carbon fibre regular filler that 479A proposed belongs to the dictyosome structured packing.It is a base material with the polyacrylonitrile fibre fabric, resin impregnating, and molded curing, moulding, carbonization make the ripple section bar of carbon fibre fabric, are assembled into the carbon fibre regular filler again.This invention provides a kind of carbon fibre regular filler of dictyosome structured packing category, and it has corrosion-resistant, every meter advantage that number of theoretical plate is high, yet exists voidage low, the pressure drop height, and flux is little, deficiencies such as the easy obstruction of filler.
Purpose of the present invention, improve the above-mentioned deficiency of prior art exactly, with the carbon of simple or modification and/or graphite and goods thereof aggregate as assembled unit, treated base material, sheet material, the corrugated plating be processed into, and and then be processed into packed tower with carbon and/or the structured packing of graphite entity.With solve corrosive environment down efficiently, high flux, the lower resistance gas-liquid, the liquid-liquid mass transfer apparatus problem that fall.
The objective of the invention is to implement by following technical solution:
Manufacture and design the entity structured packing of a kind of packed tower, it is characterized in that assembled unit is simple or the carbon of modification and/or the corrugated plating of graphite and goods thereof.
Above-mentioned structured packing comprises vertical moire type, horizontal ripple type, plate-type and honeycomb type.
The assembled unit of this above-mentioned structured packing is the simple carbon and/or the corrugated plating of graphite and goods thereof, be meant the employing petroleum coke, pitch coke, native graphite is as the aggregate of carbon and/or graphite structured packing, can select suitable binding agent according to its shaping characteristic, as coal tar, coal tar pitch, bondings such as synthetic resin, also can add a small amount of corresponding curing agent, as benzene sulfonyl chloride, phthalic anhydride or dithyl sulfate solidify, become the ductility base material that is fit to the moulding requirement, or employing carbon, graphite and goods thereof, through mold pressing, extruding, punching press, the sheet material of base material or the corrugated plating of base material are processed in roll extrusion or cast, mechanical shearing strength characteristics according to the base material corrugated plating, shear earlier, bonding is assembled into the wave disc of the required shape of this structured packing, again through solidifying, carbonization and/or graphitization processing; Or with the base material corrugated plating, first curing, carbonization and/or graphitization processing are again through the wave disc of shearing, bonding is assembled into the required shape of this structured packing.
The assembled unit of this above-mentioned structured packing is the carbon and/or the graphite corrugated plating of modification, be meant the employing petroleum coke, pitch coke, native graphite adds pitch powder, calcium phosphate, glass dust or synthetic resin are modifier, as the carbon of modification and/or the aggregate of graphite structured packing, through bonding, be solidified into the ductility base material that is fit to the moulding requirement, or employing carbon, graphite and goods thereof, through mold pressing, extruding, punching press, the sheet material of base material or the corrugated plating of base material are processed in roll extrusion or cast, shear earlier, bonding is assembled into the wave disc of the required shape of this structured packing, again through solidifying, carbonization and/or graphitization processing; Perhaps with the base material corrugated plating, earlier through curing, carbonization and/or graphitization processing, again through the wave disc of shearing, bonding is assembled into the required shape of this structured packing.
The assembled unit of this above-mentioned structured packing is simple or the carbon of modification and/or the corrugated plating of graphite and goods thereof, is meant that aggregate or modification aggregate do not add binding agent, curing agent, directly it is shaped to the sheet material of base material or the corrugated plating of base material.
Adopting the extrusion modling of corrugated die orifice at the extrusion end in the above-mentioned extrusion process is the corrugated plating of base material.
Mechanical shearing strength characteristics according to the base material corrugated plating, can carry out even cloth hole, surface, roll decorative pattern or pit by certain percent opening, with it (for example according to the desired geometrical body of tower, cylindrical, rectangle, circle lack shape, ellipticity etc.) the dimensional requirement direct slicing, and direction is (for example in accordance with regulations, the opposite order of adjacent corrugations sheet ripple direction) become the wave disc of the required shape of tower through binding agent bonding assembling, again according to above-mentioned raw materials character through curing, carbonization or graphitization processing; Perhaps the base material corrugated plating is carried out surface treatment,, be assembled into the wave disc of the required shape of this structured packing again through bonding by the tower dimensional requirement earlier through curing, carbonization or graphitization processing.
The assembled unit of packed tower provided by the invention is simple or the entity structured packing of the corrugated plating of the carbon of modification and/or graphite and goods thereof, compare with the structured packing of metal, pottery, plastics or the carbon fiber material of prior art, has excellent corrosion resisting performance, high mass transfer efficiency, the clear superiority that organically combines with highly versatile etc. falls in lower resistance, solve efficient, the high flux under the corrosive environment, gas-liquid, the liquid-liquid mass transfer apparatus problem that lower resistance is fallen, reached the goal of the invention of expection.
Below in conjunction with embodiment the present invention is done into-goes on foot elaboration:
" embodiment one "
Adopt petroleum coke (volatile matter＜0.7%, ash content＜0.1%, sulfur content＜0.5%) powder (granularity 80～100 orders) is as aggregate, with mid temperature pitch and high temperature coal-tar as binding agent, proportioning is 100 parts of petroleum coke powders, add 30～40 parts of mid temperature pitches (70 ± 1 ℃ of softening points) and high temperature coal-tar (boiling point＞280 ℃, density 1.20 ± 0.5g/cm
3).
The compound of said ratio is pinched 130 ± 5 ℃ of abundant down mixing, obtain the ductility base material, in extruder under 20MPa pressure, be pressed in the corrugated die orifice and extrude by extrusion nozzle and (heat with propane flammable gas around the mould, outer wall is 300 ± 10 ℃, base material is 220 ± 10 ℃ in the mould, 100 ± 10 ℃ of outlet temperatures).Once extruding, use water cooling, obtain the petroleum coke corrugated plating.Then with it in gas roaster, under the condition of starvation, carry out carbonization treatment by certain temperature rise speed, the segmentation temperature rise speed is: (1) 0～350 ℃ of 5 ℃/h; (2) 350～450 ℃ of 2 ℃/h; (3) 450～600 ℃ of 2.5 ℃/h; (4) 600～800 ℃ of 4 ℃/h; (5) 800～1000 ℃ of 6 ℃/h; (6) 1000～1300 ℃ of 10 ℃/h; (7) 1300 ℃ keep 20h, obtain the carbon plate corrugated plate.Again with the carbon plate corrugated plate in graphitizing furnace, under the condition of starvation, carry out graphitization processing by certain temperature rise degree of stating, the segmentation temperature rise speed is: (1) 0～500 ℃ of 75 ℃/h; (2) 500～1000 ℃ of 70 ℃/h; (3) 1000～1500 ℃ of 60 ℃/h; (4) 1500～2000 ℃ of 40 ℃/h; (5) 2000～2300 ℃ of 20 ℃/h; (6) 2300～2500 ℃ of 0～10 ℃/h make graphite board corrugated.
With the section of carbon or graphite corrugated plating and be rightabout by adjacent two ripple inclination angles and make up, become the certain geometrical shape plate ripple arranged packing of (for example, cylindric, circle lacks shape, rectangle etc.).
" embodiment two " are aggregate with the graphous graphite powder, and phenolic resins is binding agent.
Phenolic resins (is added in the mixer after 1～3h) preheating of falling ball method viscosity, keeps 50～60 ℃, add graphous graphite powder (volatile matter≤3% of weighing in proportion, ash content≤1.6%, phosphorus content 〉=95%, moisture≤0.5%, granularity 80～100 orders), the weight ratio of graphous graphite powder and phenolic resins is 3: 1, mix, obtain the ductility base material, add in the identical forcing press of embodiment one, under 10MPa pressure, from ripple mouth mould, extrude (mold temperature is controlled at 90～100 ℃).Once extruding, enter curing area immediately and be cured, the temperature of curing area is 160～180 ℃, the length of curing area should adapt with extruded velocity, can curing molding to guarantee corrugated plating.Then the corrugated plating of extruding is carried out carbonization, graphitization processing by the method for embodiment one, cut into slices, be assembled into the Lamb wave line regular tower filler of certain geometrical shape.
" embodiment three " are aggregate with the graphous graphite powder, are binding agent with the hybrid resin.
With phenolic resins and epoxy resin 6101 is to add after the weighing in 6: 4 in the mixer by weight proportion, (the phenolic resins specification requirement is with implementing side two, epoxy resin is low viscosity), the dithyl sulfate that adds resin demand 2% is made curing agent, fully mix, in graphous graphite powder: the weight ratio of hybrid resin is 3: 1 a ratio, add graphous graphite powder (it requires with example two), method by embodiment two is carried out extrusion modling, carbonization, graphitization processing, cuts into slices, is assembled into the Lamb wave line regular tower filler of certain geometrical shape then.
" embodiment four " are aggregate with the graphous graphite powder, and phenolic resins is binding agent.
With phenolic resins is bonding agent (the phenolic resins specification requirement is with embodiment two), graphous graphite powder (it requires with example two) is an aggregate, in graphous graphite powder: the weight ratio of phenolic resins is that 4: 6 ratio adds, the benzene sulfonyl chloride that adds binding agent consumption 8% is a curing agent, stir 2～4h, its injection matched molds that stirs is undulatory mould, mould is cured by following temperature rise speed together with materials inside: (1) room temperature～60 ℃ 2 ℃/h; (2) 60～80 ℃ of 1 ℃/h; (3) 80～100 ℃ of 0.5 ℃/h; (4) 100～110 ℃ of 1 ℃/h; (5) 110～140 ℃ of 2 ℃/h; (6) 140～200 ℃ of 4 ℃/h.With the corrugated plate demoulding that is cured, carry out carbonization, graphitization processing by the method for embodiment one, cut into slices, be assembled into the Lamb wave line regular tower filler of certain geometrical shape then.
" embodiment five "
Adopting epoxy resin 6101 is binding agent, graphous graphite powder is an aggregate, in graphous graphite powder: the weight ratio of epoxy resin is 4: 6 a ratio batching, 13% the phthalic anhydride that adds the compound consumption is made curing agent, place fully mix in the mixer behind the ductility base material, make carbon, the graphite regular tower filler of definite shape by the method for embodiment four.
" embodiment six "
Use the native graphite particle, crystalline flake graphite particle (〉=60 orders for example, phosphorus content 〉=99%) makes aggregate, carry out oxidation processes 3～4h through nitration mixture (mixture of the concentrated sulfuric acid and nitric acid), so, be washed to PH6～7 with the sodium carbonate neutralization, centrifuge dripping, filter cake is after 50～100 ℃ of oven dry, and the propane flammable gas flame that places temperature to be about 1000 ℃ carries out high-temperature process, makes the pyrographite particle.In mould, add an amount of pyrographite particle, extrusion forming then, the graphite corrugated plate, be placed in the mould that the yin, yang mould forms, the yin, yang mould in conjunction with the plane be provided with longitudinal axis inclination angle at 45, the degree of depth be that 6.3mm, drift angle distance are the triangle groove milling of 10.2mm.The yin, yang mould all has electric heater unit, can keep mold temperature at 180～210 ℃.Can be coated with a small amount of industrial vaseline on the surface of yin, yang mould for the ease of the demoulding.
By the corresponding dimensional requirement of structured packing body, with the graphite board corrugated small pieces that cut into corresponding size, and small pieces are connect adjacent two opposite der group of ripple direction dress up dish, obtain graphite board corrugated filler.
" embodiment seven "
With the pyrographite particle that embodiment six described methods make, the stainless steel electrical heating of 6 couples of Φ 250 * 400mm of employing is rolled into row and is rolled step by step, makes it to become graphite sheet.This sheet material is placed punch forming on the peak mould, obtain graphite board corrugated filler band.This band is cut into slices, assembled, can obtain the graphite regular tower filler.
" embodiment eight "
The pitch powder (〉=200 order) that adds its weight 5% in the pyrographite particle that example six described methods are made places fully mixing of cylinder, obtains graphite-coal drop cream stuff and other stuff aggregate.Its method by embodiment six or example seven is made mellapak packing.It is carried out carbonization treatment under 1000 ℃, not only had certain elasticity but also had the graphitic carbon mellapak packing of the modification of higher mechanical strength.
" embodiment nine "
The high temperature oxidation resisting auxiliary agent calcium phosphate (〉=300 order) that adds its weight 8% in the pyrographite particle that example six described methods are made places fully mixing of cylinder, obtains the modified graphite particle aggregate of high temperature oxidation resisting.Its method by embodiment six or example seven is made the graphite board corrugated filler of the high temperature oxidation resisting of modification.
" embodiment ten "
The glass dust (〉=300 order) that adds its weight 22% in the pyrographite particle that example six described methods are made places fully mixing of cylinder as aggregate, makes mellapak packing by the method for embodiment six or embodiment seven.It is carried out high-temperature process under 950 ℃, obtain having the glass-modified graphitic carbon mellapak packing of higher mechanical strength.
" embodiment 11 "
The epoxy powder (〉=300 order) that adds its weight 10% in the pyrographite particle that example six described methods are made places fully mixing of cylinder as aggregate, makes mellapak packing by the method for embodiment six or embodiment seven.It is carried out carbonization treatment under 1000 ℃, obtain the graphitic carbon mellapak packing of epoxy resin modification; It is carried out graphitization processing under 2200 ℃, obtain the graphite board corrugated filler of epoxy resin modification.
" embodiment 12 "
The epoxy resin that adds its weight 10% in sheet material, plate corrugated ribbon and the mellapak packing that example seven described methods are made, carry out surface treatment, then adopt the method for embodiment four to be cured, the method carbonization treatment of embodiment one obtains carbon plate material, plate corrugated ribbon and the mellapak packing of epoxy resin modification; Press the method graphitization processing of embodiment one again, obtain graphite sheet, plate corrugated ribbon and the mellapak packing of epoxy resin modification.
Claims (5)
1. packed tower entity structured packing, the assembled unit that it is characterized in that this structured packing is carbon and/or graphite material corrugated plating.
2. according to the entity structured packing of the described packed tower of claim 1, it is characterized in that the assembled unit of this structured packing adopts petroleum coke, pitch coke or native graphite as aggregate, the treated sheet material that is processed into the ductility base material that is fit to the moulding requirement; The sheet material of aggregate or this ductility base material is processed into the corrugated plating of base material or base material through mold pressing, extruding, punching press, roll extrusion or cast, the wave disc that shear earlier, bonding is assembled into the required shape of this structured packing is again through curing, carbonization and/or graphitization processing; Perhaps that the base material corrugated plating is first through curing, carbonization and/or graphitization processing, again through the wave disc of shearing, bonding is assembled into the required shape of this structured packing.
3. according to the entity structured packing of the described packed tower of claim 2, it is characterized in that described aggregate is for to add pitch powder, calcium phosphate, glass dust or synthetic resin as modifier in petroleum coke, pitch coke or native graphite.
4. according to claim 1 or 3 described packed tower entity structured packings, it is characterized in that described structured packing comprises vertical moire type, horizontal ripple type, plate-type and honeycomb type.
5. according to the structured packing of the described packed tower entity of claim 2, it is characterized in that in the described extrusion process, in the extrusion modling of the terminal employing of extrusion corrugated die orifice.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97121089A CN1089028C (en) | 1997-12-24 | 1997-12-24 | Carbon and/or graphite board corrugated regular filler for packed column |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97121089A CN1089028C (en) | 1997-12-24 | 1997-12-24 | Carbon and/or graphite board corrugated regular filler for packed column |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1220911A CN1220911A (en) | 1999-06-30 |
| CN1089028C true CN1089028C (en) | 2002-08-14 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97121089A Expired - Fee Related CN1089028C (en) | 1997-12-24 | 1997-12-24 | Carbon and/or graphite board corrugated regular filler for packed column |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1895768B (en) * | 2006-06-15 | 2010-11-10 | 天津大学 | Production of carbon fibre regular corrugation filler |
| CN106861596B (en) * | 2017-04-27 | 2019-05-17 | 山东金城石墨烯科技有限公司 | A kind of preparation method and applications of grapheme foam rectifying tower packing |
| CN110118508A (en) * | 2019-03-12 | 2019-08-13 | 烟台大成塑业有限公司 | Cooling tower filler is without glue packaging technology |
| CN110526727B (en) * | 2019-08-29 | 2022-01-04 | 航天材料及工艺研究所 | Ceramic matrix composite structure and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2055584U (en) * | 1989-07-13 | 1990-04-04 | 浙江工学院 | Plate graphite heat exchanger |
-
1997
- 1997-12-24 CN CN97121089A patent/CN1089028C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2055584U (en) * | 1989-07-13 | 1990-04-04 | 浙江工学院 | Plate graphite heat exchanger |
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| CN1220911A (en) | 1999-06-30 |
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