CN106000305A - High-molecular modified carbon powder and preparation method thereof - Google Patents
High-molecular modified carbon powder and preparation method thereof Download PDFInfo
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- CN106000305A CN106000305A CN201610398292.8A CN201610398292A CN106000305A CN 106000305 A CN106000305 A CN 106000305A CN 201610398292 A CN201610398292 A CN 201610398292A CN 106000305 A CN106000305 A CN 106000305A
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Abstract
The invention discloses a high-molecular modified carbon powder. The high-molecular modified carbon powder comprises the following raw materials by weight: 0.1 to 0.18 part of sodium hydroxide, 2 to 3 parts of ammonium polyphosphate, 0.3 to 1 part of manganese sulfate, 100 to 120 parts of eucalyptus powder, 50 to 60 parts of phenol, 0.6 to 1 part of phosphoric acid, 0.03 to 0.05 part of urotropine, 17 to 20 parts of a formaldehyde solution with a concentration of 15 to 17%, 2 to 3 parts of lignin, 20 to 30 parts of dimethyl formamide, 0.7 to 1 part of calcium acetylacetone, 0.1 to 0.2 part of glyceryl tristearate, 0.7 to 1 part of beta-hydroxyalkylamide, 2.5 to 3 parts of polyacrylamide, 0.8 to 1 part of polylactic acid, 2 to 3 parts of pentaerythritol and 0.1 to 0.2 part of hydroxyquinoline. According to the invention, a high-molecular solution is added into the carbon powder, so stability of lignin phenolic resin can be improved; and thus, compactness of holes in the carbon powder is further improved.
Description
Technical field
The present invention relates to nano-sized carbon technical field, particularly relate to a kind of macromolecule modified carbon dust and preparation method thereof.
Background technology
Activated carbon fiber has diameter pore distribution concentration tiny, micro-, quick adsorption and desorption, is provided that the features such as bigger adsorption capacity and high-specific surface area, and its pore structure and surface chemical structure are the main structure parameters determining its adsorption and desorption performance.Carbon fiber is after activation processing, original fibre structure is destroyed, it is partially formed class graphite microcrystal, carbon atom exists owing to each parallel layers of crystallite lamella is piled up irregular with the class graphite microcrystal sheet form that random layer stack is folded, lacking three-dimensional order arrangement, in Turbostratic, average-size is the least, plus the various defects caused in carbonization process, poling processing technique process, jointly construct the void network structure that activated carbon fiber is cross-linked with each other；Activated carbon fiber has the features such as intensity efflorescence higher, high temperature resistant, unsuitable, processing forming are good; can be made into the character that cloth, paper etc. are different; and resistance to bronsted lowry acids and bases bronsted lowry corruption candle, characteristic renewable, environment amenable; since coming out, the various fields such as chemical industry, electronics production, health care, environmental conservation it are widely used in.
Activated carbon fiber is with high polymer as raw material, " the difference according to raw material that a kind of threadiness efficient absorption made through high temperature cabonization and activation separates material, activated carbon fiber is divided into viscose glue base by people, polyacrylonitrile-radical, asphaltic base, phenolic aldehyde base isoreactivity carbon fiber, they are respectively arranged with unique distinction, and " viscose rayon is the primary raw material being prepared to activated carbon fiber the earliest, owing to it is cheap, aboundresources, make excellent product performance, it is relatively big " under identical carbonization-soak time that production cost reduces potentiality, activated carbon fiber is readily available bigger specific surface area and adsorption capacity than the activated carbon fiber of other raw material, the ratio of performance to price is high " so, viscose base activated carbon fiber be also the most studied at most, one of most widely used activated carbon fiber；
The activated carbon fiber of report is mostly pore type and mesothyrid activated carbon fiber the most both at home and abroad, seldom there is the progress of research worker report macroscopic void activated carbon fiber, it is blank that this has been filled up by carbon fiber prepared by the present invention, this macroscopic void activated carbon fiber is applied to medical domain through the most modified, leavens dough have good value at viral adsorption protein, kreatinin, the bioprotein etc. of VB12.
Summary of the invention
The object of the invention is contemplated to make up the defect of prior art, it is provided that a kind of macromolecule modified carbon dust and preparation method thereof.
The present invention is achieved by the following technical solutions:
A kind of macromolecule modified carbon dust, it is made up of the raw material of following weight parts:
Sodium hydroxide 0.1-0.18, APP 2-3, manganese sulfate 0.3-1, Eucalyptus wood powder 100-120, phenol 50-60, phosphoric acid 0.6-1, formalin 17-20 of hexamethylenamine 0.03-0.05,15-17%, lignin 2-3, dimethylformamide 20-30, calcium acetylacetonate 0.7-1, glyceryl tristearate 0.1-0.2, beta-hydroxy alkylamide 0.7-1, polyacrylamide 2.5-3, polylactic acid 0.8-1, tetramethylolmethane 2-3,8-hydroxyquinoline 0.1-0.2.
The preparation method of a kind of described macromolecule modified carbon dust, comprises the following steps:
(1) 85-90% of above-mentioned phenol weight is taken, mix with above-mentioned Eucalyptus wood powder, stir, send in oil bath, add phosphoric acid, slowly raising oil bath temperature under stirring condition, temperature reaches to stop heating, insulated and stirred 2-3 hour when 160-165 DEG C, discharging, it is cooled to room temperature, is filtered to remove filtrate, obtain liquefaction products；
(2) being joined by above-mentioned APP in the deionized water of its weight 5-8 times, stir, add beta-hydroxy alkylamide, insulated and stirred 3-6 minute at 40-50 DEG C, secure satisfactory grades sub-solution；
(3) above-mentioned 8-hydroxyquinoline is joined in the dehydrated alcohol of its weight 17-20 times, stir, add tetramethylolmethane, calcium acetylacetonate, insulated and stirred 4-5 minute at 60-67 DEG C, obtain compound alcoholic solution；
(4) being joined by above-mentioned polyacrylamide in the deionized water of its weight 3-4 times, add lignin, stir, secure satisfactory grades sub-lignin liquor；
(5) formalin of remaining phenol with above-mentioned 15-17% being mixed, stir, add macromolecule lignin liquor, sodium hydroxide, at 90-95 DEG C, stirring reaction 110-120 minute, obtains lignin phenol formaldehyde resin；
(6) above-mentioned lignin phenol formaldehyde resin is joined in dimethylformamide, add compound alcoholic solution, stir, for lignin phenol formaldehyde resin solution；
(7) above-mentioned liquefaction products is mixed with hexamethylenamine, add lignin phenol formaldehyde resin solution, stir, it is sent in heating tank, gradually rises temperature with the speed of 3-4 DEG C/min, be 165-170 DEG C to temperature, insulated and stirred 16-20 minute, add above-mentioned macromolecular solution, stir, obtain spinning liquid；Reduce spinning liquid temperature, carry out spinning, obtain initial fiber；
(8) preparation impregnation liquid: described impregnation liquid by the concentration that mass ratio is 1:3-4 be the formaldehyde of 18-19%, concentration be that the mixed in hydrochloric acid of 15-16% forms；Above-mentioned initial fiber is joined in impregnation liquid, slowly rises high-temperature and be 86-90 DEG C, be incubated 120-130 minute, take out, wash, be dried, obtain carbon fibre precursor；
(9) above-mentioned carbon fibre precursor is mixed with remaining each raw material, put in retort, under nitrogen protection with 3-4 DEG C/min liter high-temperature for 770-800 DEG C, carbonization 70-80 minute, take out cooling, wear into fine powder, to obtain final product.
The invention have the advantage that
The reaction principle of the present invention is: Eucalyptus wood powder carries out acidic catalyst liquefaction reaction in the presence of phenol, polymer substance degraded in timber, phenol reacts with partial intermediate and generates aldehydes matter, glucose unit in cellulose is by after open loop, the reactions such as the cracking of saccharic composition, deoxidation and phenolate can occur, create multiple aldehydes matter, and generate substantial amounts of aldehydes matter after lignin generation degradation reaction.These aldehydes matters that liquefaction reaction generates can be prepared as thermoplastic phenolic resin, this wooden base phenolic resin is after spinning under molten, in the mixing liquid of formaldehyde and hydrochloric acid, carry out cross-linking and curing reaction again, finally carry out charring process process, timber liquefied matter carbon fiber can be prepared.
nullWood liquefied carbon fiber high-temperature activation in the environment of steam of the present invention，C-0 easy fracture,Destroy the netted random layer graphite-like structure of carbon fiber aromatic ring two dimensional surface，Form oxygen-containing functional group such as hydroxyl、Ether etc.,Making activated carbon fiber generate more pore structure makes activated carbon fiber absorbability improve，The present invention is also added into lignin，With phenol、Formaldehyde hybrid reaction，Molecule segment activeness is made to properly increase，Be conducive to the formation of macromole hole，Its network structure divides, the bigger micro-molecular gas ball cutting formed, the less bead becoming evenly sized,Limit excessive hole formation，Play the effect being evenly distributed hole diameter，Can play a protective role in resin system，Thus improve the thermal stability of resin，Make the hole homogenization within Lignin phenolic carbon fiber、Densification.The carbon dust of the present invention adds macromolecular solution, can effectively improve the stability of lignin phenol formaldehyde resin, improve the compactness of carbon dust hole further.
Detailed description of the invention
A kind of macromolecule modified carbon dust, it is made up of the raw material of following weight parts:
Sodium hydroxide 0.1, APP 2, manganese sulfate 0.3, Eucalyptus wood powder 100, phenol 50, phosphoric acid 0.6, the formalin 17 of hexamethylenamine 0.03,15%, lignin 2, dimethylformamide 20, calcium acetylacetonate 0.7, glyceryl tristearate 0.1, β hydroxyalkyl amide 0.7, polyacrylamide 2.5, polylactic acid 0.8, tetramethylolmethane 2,8 hydroxyquinoline 0.1.
The preparation method of a kind of described macromolecule modified carbon dust, comprises the following steps:
(1) take the 85% of above-mentioned phenol weight, mix with above-mentioned Eucalyptus wood powder, stir, send in oil bath, adding phosphoric acid, slowly raise oil bath temperature under stirring condition, temperature reaches to stop heating, insulated and stirred 2 hours when 160 DEG C, discharging, is cooled to room temperature, is filtered to remove filtrate, obtains liquefaction products；
(2) being joined by above-mentioned APP in the deionized water of its weight 5 times, stir, add β hydroxyalkyl amide, insulated and stirred 3 minutes at 40 DEG C, secure satisfactory grades sub-solution；
(3) above-mentioned 8 hydroxyquinoline are joined in the dehydrated alcohol of its weight 17 times, stir, add tetramethylolmethane, calcium acetylacetonate, insulated and stirred 4 minutes at 60 DEG C, obtain compound alcoholic solution；
(4) being joined by above-mentioned polyacrylamide in the deionized water of its weight 3 times, add lignin, stir, secure satisfactory grades sub-lignin liquor；
(5) formalin of remaining phenol with above-mentioned 15% being mixed, stir, add macromolecule lignin liquor, sodium hydroxide, at 90 DEG C, stirring reaction 110 minutes, obtain lignin phenol formaldehyde resin；
(6) above-mentioned lignin phenol formaldehyde resin is joined in dimethylformamide, add compound alcoholic solution, stir, for lignin phenol formaldehyde resin solution；
(7) above-mentioned liquefaction products is mixed with hexamethylenamine, add lignin phenol formaldehyde resin solution, stir, be sent in heating tank, gradually rise temperature with the speed of 3 DEG C/min, be 165 DEG C to temperature, insulated and stirred 16 minutes, add above-mentioned macromolecular solution, stir, obtain spinning liquid；Reduce spinning liquid temperature, carry out spinning, obtain initial fiber；
(8) preparation impregnation liquid: described impregnation liquid is made up of the mixed in hydrochloric acid that the formaldehyde that the concentration that mass ratio is 1:3 is 18%, concentration are 15%；Joining in impregnation liquid by above-mentioned initial fiber, slowly rising high-temperature is 86 DEG C, is incubated 120 minutes, takes out, washes, and is dried, obtains carbon fibre precursor；
(9) being mixed with remaining each raw material by above-mentioned carbon fibre precursor, put in retort, rising high-temperature with 3 DEG C/min under nitrogen protection is 770 DEG C, and carbonization 70 minutes is taken out cooling, worn into fine powder, to obtain final product.
Performance test:
Specific surface area is 1177m2/ g, average pore volume is 0.868cm3/ g, average pore size is 18-20nm.
Claims (2)
1. a macromolecule modified carbon dust, it is characterised in that it is made up of the raw material of following weight parts:
Sodium hydroxide 0.1-0.18, APP 2-3, manganese sulfate 0.3-1, Eucalyptus wood powder 100-120, phenol 50-60, phosphoric acid 0.6-1, formalin 17-20 of hexamethylenamine 0.03-0.05,15-17%, lignin 2-3, dimethylformamide 20-30, calcium acetylacetonate 0.7-1, glyceryl tristearate 0.1-0.2, beta-hydroxy alkylamide 0.7-1, polyacrylamide 2.5-3, polylactic acid 0.8-1, tetramethylolmethane 2-3,8-hydroxyquinoline 0.1-0.2.
2. the preparation method of a macromolecule modified carbon dust as claimed in claim 1, it is characterised in that comprise the following steps:
(1) 85-90% of above-mentioned phenol weight is taken, mix with above-mentioned Eucalyptus wood powder, stir, send in oil bath, add phosphoric acid, slowly raising oil bath temperature under stirring condition, temperature reaches to stop heating, insulated and stirred 2-3 hour when 160-165 DEG C, discharging, it is cooled to room temperature, is filtered to remove filtrate, obtain liquefaction products；
(2) being joined by above-mentioned APP in the deionized water of its weight 5-8 times, stir, add beta-hydroxy alkylamide, insulated and stirred 3-6 minute at 40-50 DEG C, secure satisfactory grades sub-solution；
(3) above-mentioned 8-hydroxyquinoline is joined in the dehydrated alcohol of its weight 17-20 times, stir, add tetramethylolmethane, calcium acetylacetonate, insulated and stirred 4-5 minute at 60-67 DEG C, obtain compound alcoholic solution；
(4) being joined by above-mentioned polyacrylamide in the deionized water of its weight 3-4 times, add lignin, stir, secure satisfactory grades sub-lignin liquor；
(5) formalin of remaining phenol with above-mentioned 15-17% being mixed, stir, add macromolecule lignin liquor, sodium hydroxide, at 90-95 DEG C, stirring reaction 110-120 minute, obtains lignin phenol formaldehyde resin；
(6) above-mentioned lignin phenol formaldehyde resin is joined in dimethylformamide, add compound alcoholic solution, stir, for lignin phenol formaldehyde resin solution；
(7) above-mentioned liquefaction products is mixed with hexamethylenamine, add lignin phenol formaldehyde resin solution, stir, it is sent in heating tank, gradually rises temperature with the speed of 3-4 DEG C/min, be 165-170 DEG C to temperature, insulated and stirred 16-20 minute, add above-mentioned macromolecular solution, stir, obtain spinning liquid；Reduce spinning liquid temperature, carry out spinning, obtain initial fiber；
(8) preparation impregnation liquid: described impregnation liquid by the concentration that mass ratio is 1:3-4 be the formaldehyde of 18-19%, concentration be that the mixed in hydrochloric acid of 15-16% forms；Above-mentioned initial fiber is joined in impregnation liquid, slowly rises high-temperature and be 86-90 DEG C, be incubated 120-130 minute, take out, wash, be dried, obtain carbon fibre precursor；
(9) above-mentioned carbon fibre precursor is mixed with remaining each raw material, put in retort, under nitrogen protection with 3-4 DEG C/min liter high-temperature for 770-800 DEG C, carbonization 70-80 minute, take out cooling, wear into fine powder, to obtain final product.
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| CN201610398292.8A CN106000305A (en) | 2016-06-07 | 2016-06-07 | High-molecular modified carbon powder and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101135075A (en) * | 2007-10-11 | 2008-03-05 | 北京林业大学 | Wood liquefied carbide fiber, protofilament and preparation method thereof |
| CN101323445A (en) * | 2008-06-13 | 2008-12-17 | 东华大学 | Method for preparing porous carbon material based on alkali lignose |
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- 2016-06-07 CN CN201610398292.8A patent/CN106000305A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101135075A (en) * | 2007-10-11 | 2008-03-05 | 北京林业大学 | Wood liquefied carbide fiber, protofilament and preparation method thereof |
| CN101323445A (en) * | 2008-06-13 | 2008-12-17 | 东华大学 | Method for preparing porous carbon material based on alkali lignose |
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Application publication date: 20161012 |