CN103723729A - Preparation method of gradient activated carbon - Google Patents
Preparation method of gradient activated carbon Download PDFInfo
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- CN103723729A CN103723729A CN201310737982.8A CN201310737982A CN103723729A CN 103723729 A CN103723729 A CN 103723729A CN 201310737982 A CN201310737982 A CN 201310737982A CN 103723729 A CN103723729 A CN 103723729A
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Abstract
The invention discloses a preparation method of gradient activated carbon, relates to a preparation method of activated carbon, and aims at solving the problems that activated carbon pores prepared by the prior art form non-gradient continuous change, is low in separating efficiency and easily causes blocking. The preparation method disclosed by the invention comprises the following steps: 1, weighing; 2, preparing a first layer of polyurethane foam; 3, coating; and 4, activating and drying. The method has the advantages that the gradient activated carbon prepared by the method forms complete gradient distribution in structure, ingredient and performance, the separating efficiency can be up to 90%, and blocking is not easily generated; 2, the specific surface area (BET) of the gradient activated carbon prepared by the method is 100-700m<2>/g, and the density is 16-80kg/m<3>; 3, the gradient activated carbon prepared by the method comprises more than three layers of gradient material layers; 4, the mean pore size of the gradient activated carbon prepared by the method is 0.1-4mm, and the activated carbon is thick in grain and high in material strength. Therefore, the preparation method is applicable to the gradient activated carbon.
Description
Technical field
The present invention relates to a kind of preparation method of gac.
Background technology
Gac is widely used sorbent material and environmentfriendly products, to environment, is friendly.At present, since 2010, global gac consumption maintains sustained and rapid growth, and within 2012, global total quantity consumed reaches 1,200,000 tons, and market total value exceedes 1,500,000,000 dollars, and development potentiality is huge.Conventional requirement aspect, estimates that global wood activated charcoal total demand in 2015 is 600,000 tons of left and right, the output of the about half of domestic contribution; Potential demand aspect, the fields such as following global industry environmental protection (mercury emissions etc.), household/automobile environment-protection (formaldehyde, peculiar smell etc.), tap water purifying, food-drink are refining, may make the demand of wood activated charcoal occur explosive growth.Therefore, gac is an industry that has fine development prospect.
Gradient composites is according to service requirements, select the material of two kinds of different performances, adopt various compounding technologys, the Nomenclature Composition and Structure of Complexes of middle portion is changed continuously in gradient, there is not obvious interface in inside, thus a kind of advanced composite material that material property and function through-thickness are also changed in gradient.Its outstanding feature is the performance mismatch problem that has overcome bi-material combination, makes the both sides of material have different functions.This material can be widely used in Aeronautics and Astronautics industry, the engineering fields such as electronics, optics, chemistry, biomedicine and petrochemical complex.
People, when preparing Carbon Materials, usually pursue hole size homogeneous and certainly give no cause for much criticism, but performance is also single after all.
The porous material with tridimensional network that Carbon foam is comprised of the hole bubble wall of hole bubble and link mutually, the constitutional features of this uniqueness makes it have the features such as low density, high specific strength, is a kind of light porous property material.
But gac hole prepared by prior art is non-gradient to be changed continuously, separation efficiency is low and easily cause the problem of obstruction.
Summary of the invention
The object of the invention is to solve gac hole prepared by prior art and be non-gradient and change continuously, separation efficiency is low and easily cause the problem of obstruction, and a kind of preparation method of gradient active charcoal is provided.
A preparation method for gradient active charcoal, specifically completes according to the following steps:
One, take: take by weight 8 parts～12 parts polyether glycols, 10 parts～16 parts isocyanic ester, 0.05 part～0.25 part water, 2 parts～3.5 parts whipping agents, 0.05 part～0.2 part foam stabilizer and 0.04 part～0.08 part initiator;
Two, prepare the first layer polyurethane foam: under the condition that is first 1. 500r/min～1000r/min by 8 parts～12 parts polyether glycols that take, 0.05 part～0.25 part water, 2 parts～3.5 parts whipping agents, 0.05 part～0.2 part foam stabilizer and 0.04 part～0.08 part initiator low whipping speed, stir 0.5min～5min, then add 10 parts～16 parts isocyanic ester, low whipping speed is to stir 0.5min～5min under the condition of 800r/min～1500r/min, obtains the first layer polyurethane foam mixed solution; 2. the first layer polyurethane foam mixed solution being joined to temperature is in 15 ℃～30 ℃ moulds, is under the condition of 15 ℃～30 ℃, to solidify 5min～120min in temperature, and obtaining thickness is the first layer polyurethane foam of 0.5mm～10mm;
Three, apply: in the first layer polyurethane foam that is first 0.5mm～10mm at thickness, be coated with second layer polyurethane foam mixed solution, in temperature, be under the condition of 15 ℃～30 ℃, to solidify 5min～120min again, obtaining thickness is the composite foam of the first layer polyurethane foam and the second layer polyurethane foam of 1mm～15mm, on the composite foam of the first layer polyurethane foam that is then 1mm～15mm at thickness and second layer polyurethane foam, be coated with the 3rd layer of urethane foam mixing liquid, in temperature, be under the condition of 15 ℃～30 ℃, to solidify 5min～120min again, obtaining thickness is the gradient composite polyurethane foam of 2mm～20mm,
Second layer polyurethane foam mixed solution described in step 3 is to prepare according to the following steps: 1. take by weight 8 parts～12 parts polyether glycols, 10 parts～16 parts isocyanic ester, 0.05 part～0.25 part water, 2.1 parts～3.7 parts whipping agents, 0.05 part～0.21 part foam stabilizer and 0.04 part～0.08 part initiator; 2. under the condition that is 500r/min～1000r/min by 8 parts～12 parts polyether glycols that take, 0.05 part～0.25 part water, 2.1 parts～3.7 parts whipping agents, 0.05 part～0.21 part foam stabilizer and 0.04 part～0.08 part initiator low whipping speed, stir 0.5min～5min, then add 10 parts～16 parts isocyanic ester, under the condition that low whipping speed is 800r/min～1500r/min again, stir 0.5min～5min, obtain second layer polyurethane foam mixed solution; Wherein, the whipping agent described in is 1. one or more the mixture in pentane, pentamethylene, Skellysolve A, iso-pentane, methylene dichloride and trichloromethane; 1. the foam stabilizer described in is silicone oil; 1. the initiator described in is triethylenediamine, dibutyl tin laurate, stannous octoate, potassium oleate or potassium octanoate;
The 3rd layer of urethane foam mixing liquid described in step 3 is to prepare according to the following steps: 1. take by weight 8 parts～12 parts polyether glycols, 10 parts～16 parts isocyanic ester, 0.05 part～0.25 part water, 2.2 parts～3.85 parts whipping agents, 0.05 part～0.22 part foam stabilizer and 0.04 part～0.08 part initiator; 2. under the condition that is 500r/min～1000r/min by 8 parts～12 parts polyether glycols that take, 0.05 part～0.25 part water, 2.2 parts～3.85 parts whipping agents, 0.05 part～0.22 part foam stabilizer and 0.04 part～0.08 part initiator low whipping speed, stir 0.5min～5min, then add 10 parts～16 parts isocyanic ester, under the condition that low whipping speed is 800r/min～1500r/min again, stir 0.5min～5min, obtain the 3rd layer of urethane foam mixing liquid; Wherein, the whipping agent described in is 1. one or more the mixture in pentane, pentamethylene, Skellysolve A, iso-pentane, methylene dichloride and trichloromethane; 1. the foam stabilizer described in is silicone oil; 1. the initiator described in is triethylenediamine, dibutyl tin laurate, stannous octoate, potassium oleate or potassium octanoate;
Four, activation, dry: in the phosphoric acid that the gradient composite polyurethane foam impregnation that is 2mm～20mm by thickness is 20%～70% to massfraction, under normal temperature condition, react 0.5h～2h, then put into retort furnace, retort furnace is warming up to 400 ℃～1200 ℃ with the temperature rise rate of 1 ℃/min～5 ℃/min from room temperature, at inert gas atmosphere and temperature, be at 400 ℃～1200 ℃, priming reaction 0.5h～4h, naturally cool to room temperature, obtain activated material, then till activated material being washed to neutrality, in temperature, be 60 ℃～110 ℃ dry 1h～6h again, obtain gradient active charcoal.
Advantage of the present invention: structure, composition and the performance of the gradient active charcoal that, prepared by the present invention are complete Gradient distribution, and separation efficiency reaches 90%, is difficult for causing obstruction; The BET surface-area of the gradient active charcoal that two, prepared by the present invention is 100m
2/ g～700m
2/ g, density is 16kg/m
3～80kg/m
3; Three, the gradient active charcoal that prepared by the present invention has three layers of above gradient material layer; Four, the gradient active charcoal mean pore size that prepared by the present invention is 0.1mm～4mm, and channels and collaterals are thicker, and the intensity of material is high.
The present invention is applicable to the preparation method of gradient active charcoal.
Gradient active charcoal prepared by the present invention is a kind of novel Carbon Materials, because it has good physical and chemical performance, and the variation continuously in gradient of hole wherein, so be specially adapted to the separation that temperature is high, have the minuteness particle that contains multiple granularity in the fluids such as corrodibility.Compared with conventional filter material, gradient active charcoal filtration resistance prepared by the present invention is low, separation efficiency is high, be difficult for causing obstruction, and backwash is effective, its filtration procedure is: while containing micropartical in fluid, make these fluids by having the Carbon Materials of hole gradient, it is particles contained is filtered layer by layer by gradient Carbon Materials.This is the surface that is directly barred from Carbon Materials due to the particulate larger than Carbon Materials micropore size, and the little particulate in specific surface aperture enters while running into than its little aperture behind Carbon Materials inside, is again blocked in outside hole, thereby makes fluid fully by clarification filtration.
Accompanying drawing explanation
Fig. 1 is that test one step 3 obtains the SEM figure that thickness is the single foam of gradient composite polyurethane foam of 10mm;
Fig. 2 is the schematic diagram of the gradient active charcoal that obtains of test one step 4.
Embodiment
Embodiment one: present embodiment is a kind of preparation method of gradient active charcoal, specifically completes according to the following steps:
One, take: take by weight 8 parts～12 parts polyether glycols, 10 parts～16 parts isocyanic ester, 0.05 part～0.25 part water, 2 parts～3.5 parts whipping agents, 0.05 part～0.2 part foam stabilizer and 0.04 part～0.08 part initiator;
Two, prepare the first layer polyurethane foam: under the condition that is first 1. 500r/min～1000r/min by 8 parts～12 parts polyether glycols that take, 0.05 part～0.25 part water, 2 parts～3.5 parts whipping agents, 0.05 part～0.2 part foam stabilizer and 0.04 part～0.08 part initiator low whipping speed, stir 0.5min～5min, then add 10 parts～16 parts isocyanic ester, low whipping speed is to stir 0.5min～5min under the condition of 800r/min～1500r/min, obtains the first layer polyurethane foam mixed solution; 2. the first layer polyurethane foam mixed solution being joined to temperature is in 15 ℃～30 ℃ moulds, is under the condition of 15 ℃～30 ℃, to solidify 5min～120min in temperature, and obtaining thickness is the first layer polyurethane foam of 0.5mm～10mm;
Three, apply: in the first layer polyurethane foam that is first 0.5mm～10mm at thickness, be coated with second layer polyurethane foam mixed solution, in temperature, be under the condition of 15 ℃～30 ℃, to solidify 5min～120min again, obtaining thickness is the composite foam of the first layer polyurethane foam and the second layer polyurethane foam of 1mm～15mm, on the composite foam of the first layer polyurethane foam that is then 1mm～15mm at thickness and second layer polyurethane foam, be coated with the 3rd layer of urethane foam mixing liquid, in temperature, be under the condition of 15 ℃～30 ℃, to solidify 5min～120min again, obtaining thickness is the gradient composite polyurethane foam of 2mm～20mm,
Second layer polyurethane foam mixed solution described in step 3 is to prepare according to the following steps: 1. take by weight 8 parts～12 parts polyether glycols, 10 parts～16 parts isocyanic ester, 0.05 part～0.25 part water, 2.1 parts～3.7 parts whipping agents, 0.05 part～0.21 part foam stabilizer and 0.04 part～0.08 part initiator; 2. under the condition that is 500r/min～1000r/min by 8 parts～12 parts polyether glycols that take, 0.05 part～0.25 part water, 2.1 parts～3.7 parts whipping agents, 0.05 part～0.21 part foam stabilizer and 0.04 part～0.08 part initiator low whipping speed, stir 0.5min～5min, then add 10 parts～16 parts isocyanic ester, under the condition that low whipping speed is 800r/min～1500r/min again, stir 0.5min～5min, obtain second layer polyurethane foam mixed solution; Wherein, the whipping agent described in is 1. one or more the mixture in pentane, pentamethylene, Skellysolve A, iso-pentane, methylene dichloride and trichloromethane; 1. the foam stabilizer described in is silicone oil; 1. the initiator described in is triethylenediamine, dibutyl tin laurate, stannous octoate, potassium oleate or potassium octanoate;
The 3rd layer of urethane foam mixing liquid described in step 3 is to prepare according to the following steps: 1. take by weight 8 parts～12 parts polyether glycols, 10 parts～16 parts isocyanic ester, 0.05 part～0.25 part water, 2.2 parts～3.85 parts whipping agents, 0.05 part～0.22 part foam stabilizer and 0.04 part～0.08 part initiator; 2. under the condition that is 500r/min～1000r/min by 8 parts～12 parts polyether glycols that take, 0.05 part～0.25 part water, 2.2 parts～3.85 parts whipping agents, 0.05 part～0.22 part foam stabilizer and 0.04 part～0.08 part initiator low whipping speed, stir 0.5min～5min, then add 10 parts～16 parts isocyanic ester, under the condition that low whipping speed is 800r/min～1500r/min again, stir 0.5min～5min, obtain the 3rd layer of urethane foam mixing liquid; Wherein, the whipping agent described in is 1. one or more the mixture in pentane, pentamethylene, Skellysolve A, iso-pentane, methylene dichloride and trichloromethane; 1. the foam stabilizer described in is silicone oil; 1. the initiator described in is triethylenediamine, dibutyl tin laurate, stannous octoate, potassium oleate or potassium octanoate;
Four, activation, dry: in the phosphoric acid that the gradient composite polyurethane foam impregnation that is 2mm～20mm by thickness is 20%～70% to massfraction, under normal temperature condition, react 0.5h～2h, then put into retort furnace, retort furnace is warming up to 400 ℃～1200 ℃ with the temperature rise rate of 1 ℃/min～5 ℃/min from room temperature, at inert gas atmosphere and temperature, be at 400 ℃～1200 ℃, priming reaction 0.5h～4h, naturally cool to room temperature, obtain activated material, then till activated material being washed to neutrality, in temperature, be 60 ℃～110 ℃ dry 1h～6h again, obtain gradient active charcoal.
The advantage of present embodiment: structure, composition and the performance of the gradient active charcoal that, prepared by present embodiment are complete Gradient distribution, and separation efficiency reaches 90%, is difficult for causing obstruction; The BET surface-area of the gradient active charcoal that two, prepared by present embodiment is 100m
2/ g～700m
2/ g, density is 16kg/m
3～80kg/m
3; Three, the gradient active charcoal that prepared by present embodiment has three layers of above gradient material layer; Four, the gradient active charcoal mean pore size that prepared by present embodiment is 0.1mm～4mm, and channels and collaterals are thicker, and the intensity of material is high.
Present embodiment is applicable to the preparation method of gradient active charcoal.
Gradient active charcoal prepared by present embodiment is a kind of novel Carbon Materials, because it has good physical and chemical performance, and the variation continuously in gradient of hole wherein, so be specially adapted to the separation that temperature is high, have the minuteness particle that contains multiple granularity in the fluids such as corrodibility.Compared with conventional filter material, gradient active charcoal filtration resistance prepared by present embodiment is low, separation efficiency is high, be difficult for causing obstruction, and backwash is effective, its filtration procedure is: while containing micropartical in fluid, make these fluids by having the Carbon Materials of hole gradient, it is particles contained is filtered layer by layer by gradient Carbon Materials.This is the surface that is directly barred from Carbon Materials due to the particulate larger than Carbon Materials micropore size, and the little particulate in specific surface aperture enters while running into than its little aperture behind Carbon Materials inside, is again blocked in outside hole, thereby makes fluid fully by clarification filtration.
Embodiment two: present embodiment and embodiment one difference are: take by weight 8 parts～10 parts polyether glycols, 10 parts～14 parts isocyanic ester, 0.05 part～0.2 part water, 2 parts～3 parts whipping agents, 0.05 part～0.1 part foam stabilizer and 0.04 part～0.06 part initiator in step 1.Other steps are identical with embodiment one.
Embodiment three: one of present embodiment and embodiment one or two difference is: take by weight 10 parts～12 parts polyether glycols, 12 parts～16 parts isocyanic ester, 0.1 part～0.25 part water, 2.5 parts～3.5 parts whipping agents, 0.1～0.2 part of foam stabilizer and 0.06 part～0.08 part initiator in step 1.Other steps are identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three difference is: stir 2min～5min under the condition that first step 2 is 700r/min～1000r/min by 8 parts～10 parts polyether glycols that take, 0.05 part～0.2 part water, 2 parts～3 parts whipping agents, 0.05 part～0.1 part foam stabilizer and 0.04 part～0.06 part initiator low whipping speed in 1., then add 10 parts～14 parts isocyanic ester, low whipping speed is to stir 3min～5min under the condition of 1000r/min～1500r/min, obtains the first layer polyurethane foam mixed solution.Other steps are identical with embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four difference is: it is in 20 ℃～30 ℃ moulds that step 2 joins temperature by the first layer polyurethane foam mixed solution in 2., in temperature, be under the condition of 20 ℃～30 ℃, to solidify 10min～80min, obtaining thickness is the first layer polyurethane foam of 0.8mm～8mm.Other steps are identical with embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five difference is: be coated with second layer polyurethane foam mixed solution in the first layer polyurethane foam that is first 0.8mm～8mm at thickness in step 3, in temperature, be under the condition of 20 ℃～30 ℃, to solidify 10min～80min again, obtaining thickness is the composite foam of the first layer polyurethane foam and the second layer polyurethane foam of 1.5mm～13mm, on the composite foam of the first layer polyurethane foam that is then 1.5mm～13mm at thickness and second layer polyurethane foam, be coated with the 3rd layer of urethane foam mixing liquid, in temperature, be under the condition of 20 ℃～30 ℃, to solidify 10min～80min again, obtaining thickness is the gradient composite polyurethane foam of 2mm～20mm.Other steps are identical with embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six difference is: the second layer polyurethane foam mixed solution described in step 3 is to prepare according to the following steps: 1. take by weight 8 parts～10 parts polyether glycols, 10 parts～14 parts isocyanic ester, 0.05 part～0.2 part water, 2.3 parts～3.5 parts whipping agents, 0.05 part～0.2 part foam stabilizer and 0.04 part～0.06 part initiator; 2. under the condition that is 700r/min～1000r/min by 8 parts～10 parts polyether glycols that take, 0.05 part～0.2 part water, 2.3 parts～3.5 parts whipping agents, 0.05 part～0.2 part foam stabilizer and 0.04 part～0.06 part initiator low whipping speed, stir 2min～5min, then add 10 parts～14 parts isocyanic ester, under the condition that low whipping speed is 1000r/min～1500r/min again, stir 3min～5min, obtain second layer polyurethane foam mixed solution; Wherein, the whipping agent described in is 1. one or more the mixture in pentane, pentamethylene, Skellysolve A, iso-pentane, methylene dichloride and trichloromethane; 1. the foam stabilizer described in is silicone oil; 1. the initiator described in is triethylenediamine, dibutyl tin laurate, stannous octoate, potassium oleate or potassium octanoate.Other steps are identical with embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven difference is: the 3rd layer of urethane foam mixing liquid described in step 3 is to prepare according to the following steps: 1. take by weight 8 parts～10 parts polyether glycols, 10 parts～14 parts isocyanic ester, 0.05 part～0.2 part water, 2.3 parts～3.85 parts whipping agents, 0.05 part～0.21 part foam stabilizer and 0.04 part～0.06 part initiator; 2. under the condition that is 700r/min～1000r/min by 8 parts～10 parts polyether glycols that take, 0.05 part～0.2 part water, 2.3 parts～3.85 parts whipping agents, 0.05 part～0.2 part foam stabilizer and 0.04 part～0.06 part initiator low whipping speed, stir 2min～5min, then add 10 parts～14 parts isocyanic ester, under the condition that low whipping speed is 1000r/min～1500r/min again, stir 3min～5min, obtain the 3rd layer of urethane foam mixing liquid; Wherein, the whipping agent described in is 1. one or more the mixture in pentane, pentamethylene, Skellysolve A, iso-pentane, methylene dichloride and trichloromethane; 1. the foam stabilizer described in is silicone oil; 1. the initiator described in is triethylenediamine, dibutyl tin laurate, stannous octoate, potassium oleate or potassium octanoate.Other steps are identical with embodiment one to seven.
Embodiment nine: one of present embodiment and embodiment one to eight difference is: in the phosphoric acid that the gradient composite polyurethane foam impregnation that 1. step 4 is 2mm～20mm by thickness is 30%～60% to massfraction, under normal temperature condition, react 0.8h～2h, then put into retort furnace, retort furnace is warming up to 600 ℃～1100 ℃ with the temperature rise rate of 2 ℃/min～5 ℃/min from room temperature, at inert gas atmosphere and temperature, be at 600 ℃～1100 ℃, priming reaction 2h～4h, naturally cool to room temperature, use deionized water to be washed till neutrality, in temperature, be 80 ℃～110 ℃ dry 4h～6h again, obtain gradient active charcoal.Other steps are identical with embodiment one to eight.
Embodiment ten: one of present embodiment and embodiment one to nine difference is: the rare gas element described in step 4 is nitrogen, carbonic acid gas or argon gas.Other steps are identical with embodiment one to nine.
Embodiment 11: one of present embodiment and embodiment one to ten difference is: the whipping agent described in step 1 is one or more the mixture in pentane, pentamethylene, Skellysolve A, iso-pentane, methylene dichloride and trichloromethane.Other steps are identical with embodiment one to ten.
Embodiment 12: one of present embodiment and embodiment one to 11 difference is: the foam stabilizer described in step 1 is silicone oil.Other steps are identical with embodiment one to 11.
Embodiment 13: one of present embodiment and embodiment one to 12 difference is: the initiator described in step 1 is triethylenediamine, dibutyl tin laurate, stannous octoate, potassium oleate or potassium octanoate.Other steps are identical with embodiment one to 12.
Embodiment 14: one of present embodiment and embodiment one to 13 difference is: the isocyanic ester described in step 1 is one or both mixture of '-diphenylmethane diisocyanate and poly methylene poly phenyl poly isocyanate.Other steps are identical with embodiment one to 13.
Embodiment 15: one of present embodiment and embodiment one to 14 difference is: the hydroxyl value of the polyether glycol described in step 1 is 350～550mg KOH/g.Other steps are identical with embodiment one to 14.
Embodiment 16: one of present embodiment and embodiment one to 15 difference is: the rare gas element described in step 4 is one or more the mixed gas in nitrogen, carbonic acid gas and argon gas.Other steps are identical with embodiment one to 15.
Adopt following verification experimental verification effect of the present invention:
Test one: a kind of preparation method of gradient active charcoal, specifically completes according to the following steps:
One, take: take by weight 10 parts of polyether glycols, 12 parts of isocyanic ester, 0.15 part of water, 2.5 parts of whipping agents, 0.1 part of foam stabilizer and 0.06 part of initiator;
Two, prepare the first layer polyurethane foam: under the condition that is first 1. 800r/min by 10 parts of polyether glycols that take, 0.15 part of water, 2.5 parts of whipping agents, 0.1 part of foam stabilizer and 0.06 part of initiator low whipping speed, stir 2min, then add 12 parts of isocyanic ester, low whipping speed is to stir 2min under the condition of 1000r/min, obtains the first layer polyurethane foam mixed solution; 2. the first layer polyurethane foam mixed solution being joined to temperature is in 25 ℃ of moulds, is under the condition of 25 ℃, to solidify 30min in temperature, and obtaining thickness is the first layer polyurethane foam of 5mm;
Three, apply: in the first layer polyurethane foam that is first 5mm at thickness, be coated with second layer polyurethane foam mixed solution, in temperature, be under the condition of 25 ℃, to solidify 30min again, obtaining thickness is the composite foam of the first layer polyurethane foam and the second layer polyurethane foam of 8mm, on the composite foam of the first layer polyurethane foam that is then 10mm at thickness and second layer polyurethane foam, be coated with the 3rd layer of urethane foam mixing liquid, in temperature, be under the condition of 25 ℃, to solidify 30min again, obtaining thickness is the gradient composite polyurethane foam of 10mm;
Second layer polyurethane foam mixed solution described in step 3 is to prepare according to the following steps: 1. take by weight 10 parts of polyether glycols, 12 parts of isocyanic ester, 0.15 part of water, 2.6 parts of whipping agents, 0.1 part of foam stabilizer and 0.06 part of initiator; 2. under the condition that is 800r/min by 10 parts of polyether glycols that take, 0.15 part of water, 2.6 parts of whipping agents, 0.1 part of foam stabilizer and 0.06 part of initiator low whipping speed, stir 2min, then add 12 parts of isocyanic ester, under the condition that low whipping speed is 1000r/min again, stir 2min, obtain second layer polyurethane foam mixed solution; Wherein, the whipping agent described in is 1. trichloromethane; 1. the foam stabilizer described in is silicone oil; 1. the initiator described in is potassium oleate; 1. the polyether glycol described in is polyether glycol 4110; 1. the described isocyanic ester described in is '-diphenylmethane diisocyanate;
The 3rd layer of urethane foam mixing liquid described in step 3 is to prepare according to the following steps: 1. take by weight 10 parts of polyether glycols, 12 parts of isocyanic ester, 0.15 part of water, 2.75 parts of whipping agents, 0.15 part of foam stabilizer and 0.06 part of initiator; 2. under the condition that is 800r/min by 10 parts of polyether glycols that take, 0.15 part of water, 2.75 parts of whipping agents, 0.15 part of foam stabilizer and 0.06 part of initiator low whipping speed, stir 2min, then add 12 parts of isocyanic ester, under the condition that low whipping speed is 1000r/min again, stir 2min, obtain the 3rd layer of urethane foam mixing liquid; Wherein, the whipping agent trichloromethane described in 1.; 1. the foam stabilizer described in is silicone oil; 1. the initiator described in is potassium oleate; 1. the polyether glycol described in is polyether glycol 4110; 1. the described isocyanic ester described in is '-diphenylmethane diisocyanate;
Four, activation, dry: in the phosphoric acid that the gradient composite polyurethane foam impregnation that is 10mm by thickness is 40% to massfraction, under normal temperature condition, react 1h, then putting into retort furnace, retort furnace is warming up to 1000 ℃ with the temperature rise rate of 3 ℃/min from room temperature, is at 1000 ℃ at inert gas atmosphere and temperature, priming reaction 3h, naturally cool to room temperature, obtain activated material, till then activated material being washed to neutrality, in temperature, be 100 ℃ of dry 5h again, obtain gradient active charcoal;
Polyether glycol described in this testing sequence one is polyether glycol 4110;
Isocyanic ester described in this testing sequence one is '-diphenylmethane diisocyanate;
Whipping agent described in this testing sequence one is trichloromethane;
Foam stabilizer described in this testing sequence one is silicone oil;
Initiator described in this testing sequence one is potassium oleate;
Rare gas element described in this testing sequence four is nitrogen.
Use SEM to obtain the gradient composite polyurethane foam that thickness is 10mm and analyze testing a step 3, as shown in Figure 1, Fig. 1 is that test one step 3 obtains the SEM figure that thickness is the single foam of gradient composite polyurethane foam of 10mm.As can be seen from Figure 1, the similar football of whole foam shape, inside is a hollow structure, size is in 0.4mm left and right.Foam consists of three-dimensional cross-linked cancellated abscess chamber skeleton and irregular film.Three-dimensional cross-linked netted foam structure like this can demonstrate anisotropic character, and the membranaceous material of thin polyurethane covers skeleton surface.
Fig. 2 is the schematic diagram of the gradient active charcoal that obtains of test one step 4, as shown in Figure 2, test the feature that gradient active charcoal that a step 4 obtains has embodied hole gradient material, it is novel gradient Carbon Materials, compared with conventional filter material, the gradient active charcoal filtration resistance that test one step 4 obtains is low, and separation efficiency is high, be difficult for causing obstruction, and backwash is effective.
Claims (10)
1. a preparation method for gradient active charcoal, is characterized in that a kind of preparation method of gradient active charcoal specifically completes according to the following steps:
One, take: take by weight 8 parts～12 parts polyether glycols, 10 parts～16 parts isocyanic ester, 0.05 part～0.25 part water, 2 parts～3.5 parts whipping agents, 0.05 part～0.2 part foam stabilizer and 0.04 part～0.08 part initiator;
Two, prepare the first layer polyurethane foam: under the condition that is first 1. 500r/min～1000r/min by 8 parts～12 parts polyether glycols that take, 0.05 part～0.25 part water, 2 parts～3.5 parts whipping agents, 0.05 part～0.2 part foam stabilizer and 0.04 part～0.08 part initiator low whipping speed, stir 0.5min～5min, then add 10 parts～16 parts isocyanic ester, low whipping speed is to stir 0.5min～5min under the condition of 800r/min～1500r/min, obtains the first layer polyurethane foam mixed solution; 2. the first layer polyurethane foam mixed solution being joined to temperature is in 15 ℃～30 ℃ moulds, is under the condition of 15 ℃～30 ℃, to solidify 5min～120min in temperature, and obtaining thickness is the first layer polyurethane foam of 0.5mm～10mm;
Three, apply: in the first layer polyurethane foam that is first 0.5mm～10mm at thickness, be coated with second layer polyurethane foam mixed solution, in temperature, be under the condition of 15 ℃～30 ℃, to solidify 5min～120min again, obtaining thickness is the composite foam of the first layer polyurethane foam and the second layer polyurethane foam of 1mm～15mm, on the composite foam of the first layer polyurethane foam that is then 1mm～15mm at thickness and second layer polyurethane foam, be coated with the 3rd layer of urethane foam mixing liquid, in temperature, be under the condition of 15 ℃～30 ℃, to solidify 5min～120min again, obtaining thickness is the gradient composite polyurethane foam of 2mm～20mm,
Second layer polyurethane foam mixed solution described in step 3 is to prepare according to the following steps: 1. take by weight 8 parts～12 parts polyether glycols, 10 parts～16 parts isocyanic ester, 0.05 part～0.25 part water, 2.1 parts～3.7 parts whipping agents, 0.05 part～0.21 part foam stabilizer and 0.04 part～0.08 part initiator; 2. under the condition that is 500r/min～1000r/min by 8 parts～12 parts polyether glycols that take, 0.05 part～0.25 part water, 2.1 parts～3.7 parts whipping agents, 0.05 part～0.21 part foam stabilizer and 0.04 part～0.08 part initiator low whipping speed, stir 0.5min～5min, then add 10 parts～16 parts isocyanic ester, under the condition that low whipping speed is 800r/min～1500r/min again, stir 0.5min～5min, obtain second layer polyurethane foam mixed solution; Wherein, the whipping agent described in is 1. one or more the mixture in pentane, pentamethylene, Skellysolve A, iso-pentane, methylene dichloride and trichloromethane; 1. the foam stabilizer described in is silicone oil; 1. the initiator described in is triethylenediamine, dibutyl tin laurate, stannous octoate, potassium oleate or potassium octanoate;
The 3rd layer of urethane foam mixing liquid described in step 3 is to prepare according to the following steps: 1. take by weight 8 parts～12 parts polyether glycols, 10 parts～16 parts isocyanic ester, 0.05 part～0.25 part water, 2.2 parts～3.85 parts whipping agents, 0.05 part～0.22 part foam stabilizer and 0.04 part～0.08 part initiator; 2. under the condition that is 500r/min～1000r/min by 8 parts～12 parts polyether glycols that take, 0.05 part～0.25 part water, 2.2 parts～3.85 parts whipping agents, 0.05 part～0.22 part foam stabilizer and 0.04 part～0.08 part initiator low whipping speed, stir 0.5min～5min, then add 10 parts～16 parts isocyanic ester, under the condition that low whipping speed is 800r/min～1500r/min again, stir 0.5min～5min, obtain the 3rd layer of urethane foam mixing liquid; Wherein, the whipping agent described in is 1. one or more the mixture in pentane, pentamethylene, Skellysolve A, iso-pentane, methylene dichloride and trichloromethane; 1. the foam stabilizer described in is silicone oil; 1. the initiator described in is triethylenediamine, dibutyl tin laurate, stannous octoate, potassium oleate or potassium octanoate;
Four, activation, dry: in the phosphoric acid that the gradient composite polyurethane foam impregnation that is 2mm～20mm by thickness is 20%～70% to massfraction, under normal temperature condition, react 0.5h～2h, then put into retort furnace, retort furnace is warming up to 400 ℃～1200 ℃ with the temperature rise rate of 1 ℃/min～5 ℃/min from room temperature, at inert gas atmosphere and temperature, be at 400 ℃～1200 ℃, priming reaction 0.5h～4h, naturally cool to room temperature, obtain activated material, then till activated material being washed to neutrality, in temperature, be 60 ℃～110 ℃ dry 1h～6h again, obtain gradient active charcoal.
2. the preparation method of a kind of gradient active charcoal according to claim 1, is characterized in that the whipping agent described in step 1 is one or more the mixture in pentane, pentamethylene, Skellysolve A, iso-pentane, methylene dichloride and trichloromethane.
3. the preparation method of a kind of gradient active charcoal according to claim 1, is characterized in that the foam stabilizer described in step 1 is silicone oil.
4. the preparation method of a kind of gradient active charcoal according to claim 1, is characterized in that the initiator described in step 1 is triethylenediamine, dibutyl tin laurate, stannous octoate, potassium oleate or potassium octanoate.
5. the preparation method of a kind of gradient active charcoal according to claim 1, is characterized in that the isocyanic ester described in step 1 is one or both mixture of '-diphenylmethane diisocyanate and poly methylene poly phenyl poly isocyanate.
6. the preparation method of a kind of gradient active charcoal according to claim 1, the hydroxyl value that it is characterized in that the polyether glycol described in step 1 is 350～550mg KOH/g.
7. the preparation method of a kind of gradient active charcoal according to claim 1, under the condition that to it is characterized in that during step 2 1. first 8 parts～10 parts polyether glycols that take, 0.05 part～0.2 part water, 2 parts～3 parts whipping agents, 0.05 part～0.1 part foam stabilizer and 0.04 part～0.06 part initiator low whipping speed be 700r/min～1000r/min, stir 2min～5min, then add 10 parts～14 parts isocyanic ester, low whipping speed is to stir 3min～5min under the condition of 1000r/min～1500r/min, obtains the first layer polyurethane foam mixed solution.
8. the preparation method of a kind of gradient active charcoal according to claim 1, it is characterized in that the first layer polyurethane foam mixed solution being joined to temperature during step 2 is 2. in 20 ℃～30 ℃ moulds, in temperature, be under the condition of 20 ℃～30 ℃, to solidify 10min～80min, obtaining thickness is the first layer polyurethane foam of 0.8mm～8mm.
9. the preparation method of a kind of gradient active charcoal according to claim 1, it is characterized in that in phosphoric acid that gradient composite polyurethane foam impregnation that 1. step 4 is 2mm～20mm by thickness is 30%～60% to massfraction, under normal temperature condition, react 0.8h～2h, then put into retort furnace, retort furnace is warming up to 600 ℃～1100 ℃ with the temperature rise rate of 2 ℃/min～5 ℃/min from room temperature, at inert gas atmosphere and temperature, be at 600 ℃～1100 ℃, priming reaction 2h～4h, naturally cool to room temperature, use deionized water to be washed till neutrality, in temperature, be 80 ℃～110 ℃ dry 4h～6h again, obtain gradient active charcoal.
10. the preparation method of a kind of gradient active charcoal according to claim 1, is characterized in that the rare gas element described in step 4 is one or more the mixed gas in nitrogen, carbonic acid gas and argon gas.
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