CN103723729B - Preparation method of gradient activated carbon - Google Patents
Preparation method of gradient activated carbon Download PDFInfo
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- CN103723729B CN103723729B CN201310737982.8A CN201310737982A CN103723729B CN 103723729 B CN103723729 B CN 103723729B CN 201310737982 A CN201310737982 A CN 201310737982A CN 103723729 B CN103723729 B CN 103723729B
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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, is friendly to environment.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 total market is more than 1,500,000,000 dollars, and development potentiality is huge.Conventional requirement aspect, estimates that global wood activated charcoal total demand in 2015 is at about 600,000 tons, the output of domestic contribution about half; 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 having fine development prospect.
Gradient composites is according to service requirements, select the material of two kinds of different performances, adopt various compounding technology, the Nomenclature Composition and Structure of Complexes of middle portion is changed continuously in gradient, there is not obvious interface in inside, thus makes a kind of advanced composite material that material property and function through-thickness also change in gradient.Its outstanding feature is the performance mismatch problem overcoming 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 that hole size is homogeneous certainly gives no cause for much criticism, but performance is also single after all.
The porous material with tridimensional network that Carbon foam is steeped by hole and interconnected hole bubble wall forms, the constitutional features of this uniqueness makes it have the feature 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 consecutive variations, separation efficiency is low and easily cause the problem of blocking.
Summary of the invention
The object of the invention is to solve gac hole prepared by prior art is non-gradient consecutive variations, and separation efficiency is low and easily cause the problem of blocking, and provides a kind of preparation method of gradient active charcoal.
A preparation method for gradient active charcoal, specifically completes according to the following steps:
One, take: take 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 initiators by weight;
Two, the first layer polyurethane foam is prepared: be 1. first stir 0.5min ~ 5min under the condition of 500r/min ~ 1000r/min by take 8 parts ~ 12 parts polyether glycols, 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 speeds, then 10 parts ~ 16 parts isocyanic ester are added, low whipping speed is 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 temperature is in 15 DEG C ~ 30 DEG C moulds, is to solidify 5min ~ 120min under the condition of 15 DEG C ~ 30 DEG C in temperature, obtains the first layer polyurethane foam that thickness is 0.5mm ~ 10mm;
Three, coating: first at thickness be 0.5mm ~ 10mm the first layer polyurethane foam on be coated with second layer polyurethane foam mixed solution, be solidify 5min ~ 120min under the condition of 15 DEG C ~ 30 DEG C again in temperature, obtaining thickness is the first layer polyurethane foam of 1mm ~ 15mm and the composite foam of second layer polyurethane foam, then be that the first layer polyurethane foam of 1mm ~ 15mm and the composite foam of second layer polyurethane foam are coated with third layer polyurethane foam mixed solution at thickness, be solidify 5min ~ 120min under the condition of 15 DEG C ~ 30 DEG C again in temperature, obtain the graded composite polyurethane foam that thickness is 2mm ~ 20mm,
Second layer polyurethane foam mixed solution described in step 3 prepares according to the following steps: 1. take 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 initiators by weight; 2. be stir 0.5min ~ 5min under the condition of 500r/min ~ 1000r/min by take 8 parts ~ 12 parts polyether glycols, 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 speeds, then 10 parts ~ 16 parts isocyanic ester are added, low whipping speed is stir 0.5min ~ 5min under the condition of 800r/min ~ 1500r/min again, obtains second layer polyurethane foam mixed solution; Wherein, 1. described in whipping agent be the mixture of one or more 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;
Third layer polyurethane foam mixed solution described in step 3 prepares according to the following steps: 1. take 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 initiators by weight; 2. be stir 0.5min ~ 5min under the condition of 500r/min ~ 1000r/min by take 8 parts ~ 12 parts polyether glycols, 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 speeds, then 10 parts ~ 16 parts isocyanic ester are added, low whipping speed is stir 0.5min ~ 5min under the condition of 800r/min ~ 1500r/min again, obtains third layer polyurethane foam mixed solution; Wherein, 1. described in whipping agent be the mixture of one or more 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: to be that to be impregnated into massfraction be in the phosphoric acid of 20% ~ 70% for the graded composite polyurethane foam of 2mm ~ 20mm by thickness, 0.5h ~ 2h is reacted under normal temperature condition, then retort furnace is put into, by retort furnace with the temperature rise rate of 1 DEG C/min ~ 5 DEG C/min from room temperature to 400 DEG C ~ 1200 DEG C, at inert gas atmosphere and temperature are 400 DEG C ~ 1200 DEG C, priming reaction 0.5h ~ 4h, naturally cool to room temperature, obtain activated material, then till activated material being washed to neutrality, be 60 DEG C ~ 110 DEG C dry 1h ~ 6h in temperature again, obtain gradient active charcoal.
Advantage of the present invention: one, the structure of the gradient active charcoal prepared of the present invention, composition and performance are complete Gradient distribution, and separation efficiency reaches 90%, not easily causes blocking; Two, the BET surface-area of gradient active charcoal that 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 the gradient material layer of more than three layers; Four, the gradient active charcoal mean pore size that prepared by the present invention is 0.1mm ~ 4mm, and channels and collaterals are comparatively thick, 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 excellent physical and chemical performance, and hole consecutive variations in gradient wherein, so be specially adapted to the separation that temperature is high, have the minuteness particle containing 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, not easily cause blocking, and backwash is effective, its filtration procedure is: time in fluid containing micropartical, make these fluids by having the Carbon Materials of gradient pores, and namely it is particles contained is filtered layer by layer by gradient Carbon Materials.This is because the particulate larger than Carbon Materials micropore size is directly barred from the surface of Carbon Materials, and when the little particulate in specific surface aperture runs into the aperture less than it after entering Carbon Materials inside, is again blocked in outside hole, thus makes fluid fully by clarification filtration.
Accompanying drawing explanation
Fig. 1 is the SEM figure that test one step 3 obtains that thickness is the single foam of graded composite polyurethane foam of 10mm;
Fig. 2 is the schematic diagram of the gradient active charcoal that test one step 4 obtains.
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 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 initiators by weight;
Two, the first layer polyurethane foam is prepared: be 1. first stir 0.5min ~ 5min under the condition of 500r/min ~ 1000r/min by take 8 parts ~ 12 parts polyether glycols, 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 speeds, then 10 parts ~ 16 parts isocyanic ester are added, low whipping speed is 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 temperature is in 15 DEG C ~ 30 DEG C moulds, is to solidify 5min ~ 120min under the condition of 15 DEG C ~ 30 DEG C in temperature, obtains the first layer polyurethane foam that thickness is 0.5mm ~ 10mm;
Three, coating: first at thickness be 0.5mm ~ 10mm the first layer polyurethane foam on be coated with second layer polyurethane foam mixed solution, be solidify 5min ~ 120min under the condition of 15 DEG C ~ 30 DEG C again in temperature, obtaining thickness is the first layer polyurethane foam of 1mm ~ 15mm and the composite foam of second layer polyurethane foam, then be that the first layer polyurethane foam of 1mm ~ 15mm and the composite foam of second layer polyurethane foam are coated with third layer polyurethane foam mixed solution at thickness, be solidify 5min ~ 120min under the condition of 15 DEG C ~ 30 DEG C again in temperature, obtain the graded composite polyurethane foam that thickness is 2mm ~ 20mm,
Second layer polyurethane foam mixed solution described in step 3 prepares according to the following steps: 1. take 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 initiators by weight; 2. be stir 0.5min ~ 5min under the condition of 500r/min ~ 1000r/min by take 8 parts ~ 12 parts polyether glycols, 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 speeds, then 10 parts ~ 16 parts isocyanic ester are added, low whipping speed is stir 0.5min ~ 5min under the condition of 800r/min ~ 1500r/min again, obtains second layer polyurethane foam mixed solution; Wherein, 1. described in whipping agent be the mixture of one or more 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;
Third layer polyurethane foam mixed solution described in step 3 prepares according to the following steps: 1. take 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 initiators by weight; 2. be stir 0.5min ~ 5min under the condition of 500r/min ~ 1000r/min by take 8 parts ~ 12 parts polyether glycols, 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 speeds, then 10 parts ~ 16 parts isocyanic ester are added, low whipping speed is stir 0.5min ~ 5min under the condition of 800r/min ~ 1500r/min again, obtains third layer polyurethane foam mixed solution; Wherein, 1. described in whipping agent be the mixture of one or more 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: to be that to be impregnated into massfraction be in the phosphoric acid of 20% ~ 70% for the graded composite polyurethane foam of 2mm ~ 20mm by thickness, 0.5h ~ 2h is reacted under normal temperature condition, then retort furnace is put into, by retort furnace with the temperature rise rate of 1 DEG C/min ~ 5 DEG C/min from room temperature to 400 DEG C ~ 1200 DEG C, at inert gas atmosphere and temperature are 400 DEG C ~ 1200 DEG C, priming reaction 0.5h ~ 4h, naturally cool to room temperature, obtain activated material, then till activated material being washed to neutrality, be 60 DEG C ~ 110 DEG C dry 1h ~ 6h in temperature again, obtain gradient active charcoal.
The advantage of present embodiment: one, the structure of the gradient active charcoal prepared of present embodiment, composition and performance are complete Gradient distribution, and separation efficiency reaches 90%, not easily causes blocking; Two, the BET surface-area of gradient active charcoal that 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 the gradient material layer of more than three layers; Four, the gradient active charcoal mean pore size that prepared by present embodiment is 0.1mm ~ 4mm, and channels and collaterals are comparatively thick, 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 excellent physical and chemical performance, and hole consecutive variations in gradient wherein, so be specially adapted to the separation that temperature is high, have the minuteness particle containing 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, not easily cause blocking, and backwash is effective, its filtration procedure is: time in fluid containing micropartical, make these fluids by having the Carbon Materials of gradient pores, and namely it is particles contained is filtered layer by layer by gradient Carbon Materials.This is because the particulate larger than Carbon Materials micropore size is directly barred from the surface of Carbon Materials, and when the little particulate in specific surface aperture runs into the aperture less than it after entering Carbon Materials inside, is again blocked in outside hole, thus makes fluid fully by clarification filtration.
Embodiment two: present embodiment and embodiment one difference are: take 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 initiators in step one by weight.Other steps are identical with embodiment one.
Embodiment three: one of present embodiment and embodiment one or two difference is: take 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 one by weight.Other steps are identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three difference is: step 2 1. in be first stir 2min ~ 5min under the condition of 700r/min ~ 1000r/min by take 8 parts ~ 10 parts polyether glycols, 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 speeds, then 10 parts ~ 14 parts isocyanic ester are added, low whipping speed is 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: step 2 2. in the first layer polyurethane foam mixed solution is joined temperature is in 20 DEG C ~ 30 DEG C moulds, be solidify 10min ~ 80min under the condition of 20 DEG C ~ 30 DEG C in temperature, obtain the first layer polyurethane foam that thickness is 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 first coated with second layer polyurethane foam mixed solution in the first layer polyurethane foam that thickness is 0.8mm ~ 8mm in step 3, be solidify 10min ~ 80min under the condition of 20 DEG C ~ 30 DEG C again in temperature, obtaining thickness is the first layer polyurethane foam of 1.5mm ~ 13mm and the composite foam of second layer polyurethane foam, then be that the first layer polyurethane foam of 1.5mm ~ 13mm and the composite foam of second layer polyurethane foam are coated with third layer polyurethane foam mixed solution at thickness, be solidify 10min ~ 80min under the condition of 20 DEG C ~ 30 DEG C again in temperature, obtain the graded composite polyurethane foam that thickness is 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 prepares according to the following steps: 1. take 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 initiators by weight; 2. be stir 2min ~ 5min under the condition of 700r/min ~ 1000r/min by take 8 parts ~ 10 parts polyether glycols, 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 speeds, then 10 parts ~ 14 parts isocyanic ester are added, low whipping speed is stir 3min ~ 5min under the condition of 1000r/min ~ 1500r/min again, obtains second layer polyurethane foam mixed solution; Wherein, 1. described in whipping agent be the mixture of one or more 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 third layer polyurethane foam mixed solution described in step 3 prepares according to the following steps: 1. take 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 initiators by weight; 2. be stir 2min ~ 5min under the condition of 700r/min ~ 1000r/min by take 8 parts ~ 10 parts polyether glycols, 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 speeds, then 10 parts ~ 14 parts isocyanic ester are added, low whipping speed is stir 3min ~ 5min under the condition of 1000r/min ~ 1500r/min again, obtains third layer polyurethane foam mixed solution; Wherein, 1. described in whipping agent be the mixture of one or more 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: 1. thickness be that to be impregnated into massfraction be in the phosphoric acid of 30% ~ 60% to the graded composite polyurethane foam of 2mm ~ 20mm by step 4, 0.8h ~ 2h is reacted under normal temperature condition, then retort furnace is put into, by retort furnace with the temperature rise rate of 2 DEG C/min ~ 5 DEG C/min from room temperature to 600 DEG C ~ 1100 DEG C, at inert gas atmosphere and temperature are 600 DEG C ~ 1100 DEG C, priming reaction 2h ~ 4h, naturally cool to room temperature, deionized water is used to be washed till neutrality, be 80 DEG C ~ 110 DEG C dry 4h ~ 6h in temperature 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 one is the mixture of one or more 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 ten one difference is: the foam stabilizer described in step one is silicone oil.Other steps are identical with embodiment one to ten one.
Embodiment 13: one of present embodiment and embodiment one to ten two difference is: the initiator described in step one is triethylenediamine, dibutyl tin laurate, stannous octoate, potassium oleate or potassium octanoate.Other steps are identical with embodiment one to ten two.
Embodiment 14: one of present embodiment and embodiment one to ten three difference is: the isocyanic ester described in step one is one or both mixture of '-diphenylmethane diisocyanate and poly methylene poly phenyl poly isocyanate.Other steps are identical with embodiment one to ten three.
Embodiment 15: one of present embodiment and embodiment one to ten four difference is: the hydroxyl value of the polyether glycol described in step one is 350 ~ 550mg KOH/g.Other steps are identical with embodiment one to ten four.
Embodiment 16: one of present embodiment and embodiment one to ten five difference is: the rare gas element described in step 4 is the mixed gas of one or more in nitrogen, carbonic acid gas and argon gas.Other steps are identical with embodiment one to ten five.
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 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 by weight;
Two, the first layer polyurethane foam is prepared: be 1. first stir 2min under the condition of 800r/min by take 10 parts of polyether glycols, 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, then 12 parts of isocyanic ester are added, low whipping speed is 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 temperature is in 25 DEG C of moulds, is to solidify 30min under the condition of 25 DEG C in temperature, obtains the first layer polyurethane foam that thickness is 5mm;
Three, apply: first at thickness be 5mm the first layer polyurethane foam on be coated with second layer polyurethane foam mixed solution, be solidify 30min under the condition of 25 DEG C again in temperature, obtaining thickness is the first layer polyurethane foam of 8mm and the composite foam of second layer polyurethane foam, then be that the first layer polyurethane foam of 10mm and the composite foam of second layer polyurethane foam are coated with third layer polyurethane foam mixed solution at thickness, be solidify 30min under the condition of 25 DEG C again in temperature, obtain the graded composite polyurethane foam that thickness is 10mm;
Second layer polyurethane foam mixed solution described in step 3 prepares according to the following steps: 1. take 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 by weight; 2. be stir 2min under the condition of 800r/min by take 10 parts of polyether glycols, 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, then 12 parts of isocyanic ester are added, low whipping speed is stir 2min under the condition of 1000r/min again, obtains second layer polyurethane foam mixed solution; Wherein, 1. described in whipping agent be 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;
Third layer polyurethane foam mixed solution described in step 3 prepares according to the following steps: 1. take 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 by weight; 2. be stir 2min under the condition of 800r/min by take 10 parts of polyether glycols, 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, then 12 parts of isocyanic ester are added, low whipping speed is stir 2min under the condition of 1000r/min again, obtains third layer polyurethane foam mixed solution; Wherein, 1. described in whipping agent 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;
Four, activate, dry: be that to be impregnated into massfraction be in the phosphoric acid of 40% for the graded composite polyurethane foam of 10mm by thickness, 1h is reacted under normal temperature condition, then put into retort furnace, by retort furnace with the temperature rise rate of 3 DEG C/min from room temperature to 1000 DEG C, at inert gas atmosphere and temperature are 1000 DEG C, priming reaction 3h, naturally cool to room temperature, obtain activated material, till then activated material being washed to neutrality, be 100 DEG C of dry 5h in temperature 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 to test one step 3 the graded composite polyurethane foam that thickness is 10mm to analyze, as shown in Figure 1, Fig. 1 is the SEM figure that test one step 3 obtains that thickness is the single foam of graded composite polyurethane foam of 10mm.As can be seen from Figure 1, the similar football of whole foam shape, inside is a hollow structure, and size is at about 0.4mm.Foam is made up of three-dimensional cross-linked cancellated abscess room 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 test one step 4 obtains, as shown in Figure 2, test the feature that gradient active charcoal that a step 4 obtains embodies gradient pores material, it is novel gradient Carbon Materials, compared with conventional filter material, test the gradient active charcoal filtration resistance that a step 4 obtains low, separation efficiency is high, not easily cause blocking, and backwash is effective.
Claims (7)
1. a preparation method for gradient active charcoal, is characterized in that what a kind of preparation method of gradient active charcoal specifically completed according to the following steps:
One, take: take 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 initiators by weight;
Whipping agent described in step one is the mixture of one or more in pentane, pentamethylene, Skellysolve A, iso-pentane, methylene dichloride and trichloromethane;
Foam stabilizer described in step one is silicone oil;
Initiator described in step one is triethylenediamine, dibutyl tin laurate, stannous octoate, potassium oleate or potassium octanoate;
Two, the first layer polyurethane foam is prepared: be 1. first stir 0.5min ~ 5min under the condition of 500r/min ~ 1000r/min by take 8 parts ~ 12 parts polyether glycols, 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 speeds, then 10 parts ~ 16 parts isocyanic ester are added, low whipping speed is 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 temperature is in 15 DEG C ~ 30 DEG C moulds, is to solidify 5min ~ 120min under the condition of 15 DEG C ~ 30 DEG C in temperature, obtains the first layer polyurethane foam that thickness is 0.5mm ~ 10mm;
Three, coating: first at thickness be 0.5mm ~ 10mm the first layer polyurethane foam on be coated with second layer polyurethane foam mixed solution, be solidify 5min ~ 120min under the condition of 15 DEG C ~ 30 DEG C again in temperature, obtaining thickness is the first layer polyurethane foam of 1mm ~ 15mm and the composite foam of second layer polyurethane foam, then be that the first layer polyurethane foam of 1mm ~ 15mm and the composite foam of second layer polyurethane foam are coated with third layer polyurethane foam mixed solution at thickness, be solidify 5min ~ 120min under the condition of 15 DEG C ~ 30 DEG C again in temperature, obtain the graded composite polyurethane foam that thickness is 2mm ~ 20mm,
Second layer polyurethane foam mixed solution described in step 3 prepares according to the following steps: 1. take 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 initiators by weight; 2. be stir 0.5min ~ 5min under the condition of 500r/min ~ 1000r/min by take 8 parts ~ 12 parts polyether glycols, 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 speeds, then 10 parts ~ 16 parts isocyanic ester are added, low whipping speed is stir 0.5min ~ 5min under the condition of 800r/min ~ 1500r/min again, obtains second layer polyurethane foam mixed solution; Wherein, 1. described in whipping agent be the mixture of one or more 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;
Third layer polyurethane foam mixed solution described in step 3 prepares according to the following steps: 1. take 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 initiators by weight; 2. be stir 0.5min ~ 5min under the condition of 500r/min ~ 1000r/min by take 8 parts ~ 12 parts polyether glycols, 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 speeds, then 10 parts ~ 16 parts isocyanic ester are added, low whipping speed is stir 0.5min ~ 5min under the condition of 800r/min ~ 1500r/min again, obtains third layer polyurethane foam mixed solution; Wherein, 1. described in whipping agent be the mixture of one or more 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: to be that to be impregnated into massfraction be in the phosphoric acid of 20% ~ 70% for the graded composite polyurethane foam of 2mm ~ 20mm by thickness, 0.5h ~ 2h is reacted under normal temperature condition, then retort furnace is put into, by retort furnace with the temperature rise rate of 1 DEG C/min ~ 5 DEG C/min from room temperature to 400 DEG C ~ 1200 DEG C, at inert gas atmosphere and temperature are 400 DEG C ~ 1200 DEG C, priming reaction 0.5h ~ 4h, naturally cool to room temperature, obtain activated material, then till activated material being washed to neutrality, be 60 DEG C ~ 110 DEG C dry 1h ~ 6h in temperature 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 isocyanic ester described in step one is one or both mixture of '-diphenylmethane diisocyanate and poly methylene poly phenyl poly isocyanate.
3. the preparation method of a kind of gradient active charcoal according to claim 1, is characterized in that the hydroxyl value of the polyether glycol described in step one is 350 ~ 550mg KOH/g.
4. the preparation method of a kind of gradient active charcoal according to claim 1, to it is characterized in that during step 2 being 1. first stir 2min ~ 5min under the condition of 700r/min ~ 1000r/min by take 8 parts ~ 10 parts polyether glycols, 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 speeds, then 10 parts ~ 14 parts isocyanic ester are added, low whipping speed is stir 3min ~ 5min under the condition of 1000r/min ~ 1500r/min, obtains the first layer polyurethane foam mixed solution.
5. the preparation method of a kind of gradient active charcoal according to claim 1, it is characterized in that during step 2 2., the first layer polyurethane foam mixed solution being joined temperature is in 20 DEG C ~ 30 DEG C moulds, be solidify 10min ~ 80min under the condition of 20 DEG C ~ 30 DEG C in temperature, obtain the first layer polyurethane foam that thickness is 0.8mm ~ 8mm.
6. the preparation method of a kind of gradient active charcoal according to claim 1, it is characterized in that 1. thickness be that to be impregnated into massfraction be in the phosphoric acid of 30% ~ 60% for the graded composite polyurethane foam of 2mm ~ 20mm by step 4, 0.8h ~ 2h is reacted under normal temperature condition, then retort furnace is put into, by retort furnace with the temperature rise rate of 2 DEG C/min ~ 5 DEG C/min from room temperature to 600 DEG C ~ 1100 DEG C, at inert gas atmosphere and temperature are 600 DEG C ~ 1100 DEG C, priming reaction 2h ~ 4h, naturally cool to room temperature, deionized water is used to be washed till neutrality, be 80 DEG C ~ 110 DEG C dry 4h ~ 6h in temperature again, obtain gradient active charcoal.
7. 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 a kind of in nitrogen and argon gas or the wherein mixed gas of two kinds.
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| CN104368325B (en) * | 2014-12-04 | 2016-11-02 | 东北林业大学 | A kind of preparation method of light degradation formaldehyde cellular activated carbon |
| CN104984745A (en) * | 2015-07-06 | 2015-10-21 | 安徽成方新材料科技有限公司 | Bactericidal composite spherical activated carbon and preparation method thereof |
| CN104984727A (en) * | 2015-07-06 | 2015-10-21 | 安徽成方新材料科技有限公司 | Asphalt resin composite-based spherical activated carbon with fast absorption effect enhanced and preparation method thereof |
| CN105013441A (en) * | 2015-07-06 | 2015-11-04 | 安徽成方新材料科技有限公司 | High-temperature resistant corrosion resistant composite spherical activated carbon and preparation method therefor |
| CN104998617A (en) * | 2015-07-13 | 2015-10-28 | 安徽成方新材料科技有限公司 | Composite based spherical active carbon added with hard polyurethane foam wastes and preparation method for spherical active carbon |
| CN104984729A (en) * | 2015-07-13 | 2015-10-21 | 安徽成方新材料科技有限公司 | Fire proofed magnetic asphalt resin composite spherical activated carbon and preparation method thereof |
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