CN100526258C - Method for preparing wood ceramics from tobacco straw castoff - Google Patents
Method for preparing wood ceramics from tobacco straw castoff Download PDFInfo
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- CN100526258C CN100526258C CNB2007100661589A CN200710066158A CN100526258C CN 100526258 C CN100526258 C CN 100526258C CN B2007100661589 A CNB2007100661589 A CN B2007100661589A CN 200710066158 A CN200710066158 A CN 200710066158A CN 100526258 C CN100526258 C CN 100526258C
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- Prior art keywords
- temperature
- tobacco rod
- resol
- under
- tobacco stem
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- 241000208125 Nicotiana Species 0.000 title claims abstract description 42
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 42
- 239000000919 ceramic Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000002023 wood Substances 0.000 title claims description 40
- 239000010902 straw Substances 0.000 title claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 6
- 229920003987 resole Polymers 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 18
- 238000002360 preparation method Methods 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000003610 charcoal Substances 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 5
- 230000000630 rising effect Effects 0.000 claims description 5
- 238000007605 air drying Methods 0.000 claims description 2
- 238000000748 compression moulding Methods 0.000 claims 1
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 abstract description 7
- 229920001568 phenolic resin Polymers 0.000 abstract description 7
- 239000005011 phenolic resin Substances 0.000 abstract description 7
- 239000002131 composite material Substances 0.000 abstract description 5
- 239000000843 powder Substances 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 10
- 238000003763 carbonization Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000012467 final product Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000010815 organic waste Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to a method of producing a wooden ceramic by applying tobacco stem wastes. After being fully mixed with phenolic resin and ethanol solution with 20 wt percent ethanol content, tobacco stem powder as a material with a particle diameter less than 150 Mu m, which is produced after tobacco stems are carbonized under the temperature of 400 DEG C and then smashed, is dried under the temperature of 80 DEG C for half an hour, so that part of ethanol and water is removed, and then the tobacco stem powder is pressed under the pressure of 8 to 12 MPa for ten minutes to shape a tobacco stem carbon and phenolic resin composite; subsequently, at the temperature-increasing speed rate of 20 DEG C per minute, the temperature is increased to 500 DEG C, under which the tobacco stem carbon and phenolic resin composite is precarbonized for thirty minutes, the tobacco stem carbon and phenolic resin composite is finally put into a single mode cavity microwave reactor with a microwave frequency of 2.54 GHz, and under the condiction of a microwave output power of 600 to 800 W, the product is produced after the tobacco stem carbon and phenolic resin composite is prheated for 60 to 80 minutes.
Description
One, technical field
The present invention relates to a kind of method of wood ceramics preparation, affiliated field is a raw material of wood-charcoal material preparing technical field.
Two, background technology
Wood ceramics is a kind of novel amorphous carbon/glass carbon composite, light weight, hardness height, be difficult for embrittlement, have good mechanical characteristic, thermal property, electromagnetic property and tribological property, alternative traditional ceramics after processing, can be used as electrode, heating element, motor carbon, brake lining, corrosion resistant material, thermal insulation material, filtering material etc., having the wide development application prospect, is the ideal substitute of some non-renewable material.
At present, the general technology of preparation wood ceramics be the wood materials with impreg material such as resol or pulverizing directly mixes with resol carry out moulding after, through high temperature carbonization (generally temperature is 800～1600 ℃), is incubated 1～6h and obtains wood ceramics.Four kinds of diverse ways are specifically arranged: (1) solid wood timber or medium density fibre board (MDF) through resin impregnating under the ultrasonic wave, are cured processing earlier afterwards, and the wood ceramics finished product then is processed in charing under inert atmosphere again; (2) solid wood timber or medium density fibre board (MDF) behind the ultrasonic wave impregnated phenolic resin, are cured processing afterwards earlier through the machining moulding, and charing becomes wood ceramics under inert atmosphere then, is finish-machined to the wood ceramics finished product at last again; (3) wood materials of wood chip and other pulverizing mixes with resol earlier, is pressed into predetermined shape after Procuring is handled, and carries out deeply-curing then, and high temperature carbonization obtains the wood ceramics finished product under inert atmosphere at last; (4) earlier with a certain amount of wood powder, after adding an amount of phenol, the vitriol oil with 98% carries out catalysis, make liquefaction timber after reacting for some time at a certain temperature, wood materials with solid wood, wood chip and other pulverizing mixes subsequently, be pressed into predetermined shape after Procuring is handled, carry out deeply-curing then, high temperature carbonization obtains the wood ceramics finished product under inert atmosphere at last.
Take a broad view of the prior art of these preparation wood ceramics, all exist some problems: in method (1) and (2), because the raw material that is adopted is timber and medium density fibre board (MDF), structure is closely knit, thereby when carrying out resin impregnating, need to adopt special impregnation technology, flood as ultrasonic wave, otherwise prepared wood ceramics structure is inhomogeneous and inner and surface tissue is widely different, thereby cause performance to differ, influenced the application of wood ceramics, adopt special impregnation technology also will increase manufacturing facilities simultaneously, cause cost up, and can't be from solving the uneven problem of structure in essence; In method (3), directly pulverize wood materials and resol mixing during preparation with wood chip and other, because the wood materials rate of weight loss is bigger during charing, thereby cause big quantitative response to generate gas and volatile matter effusion, make product ftracture, mechanical property declines to a great extent, and is to improve mechanical property, must strengthen the consumption of resol, cause cost to increase; In method (4), for soaker/binding agent,, certainly will in the wood ceramics preparation process, introduce sulphur, thereby cause producing in the carbonization process pollution of sulfurous gas as adopting liquefaction timber, therefore should not use.
In above-mentioned 4 kinds of methods, all adopt the method for high temperature carbonization.These heating means make that sample is inside and outside and produce bigger thermograde, have caused problems such as product cracking and performance be inhomogeneous.Simultaneously, this method preparation time is long, energy consumption is big, has seriously limited the wood ceramics application.
Three, summary of the invention
1 purpose of the present invention is exactly the problem that exists among the above-mentioned wood ceramics preparation technology in order to overcome, provide a kind of technological process simple, easy and simple to handle and product performance are good, can enough tobacco rods etc. agriculture and forestry organic waste materials prepare the method for wood ceramics fast.
2 methods from preparing wood ceramics from tobacco straw castoff, its technical scheme may further comprise the steps and operational path: the first step, tobacco rod after being 400 ℃ of following charings, temperature pulverized to obtain the tobacco rod powdered carbon that particle diameter is not more than 150 μ m be raw material, with the ethanolic soln thorough mixing that the resol and the composition of certainweight is 20wt%, the weight of material ratio is: tobacco rod charcoal: resol=100:30～30:100; Tobacco rod charcoal: ethanolic soln=30:70; Second step was 80 ℃ in temperature and dries 0.5h down to remove part ethanol and moisture, was compacting 10min moulding under 8～12MPa at pressure then, had formed tobacco rod charcoal/resol mixture; The 3rd step, mixture is carried out pre-charing, promptly rising to temperature with the temperature rise rate of 20 ℃/min is 500 ℃, insulation 30min; The 4th step: fast mixture is taken out, putting into the microwave frequency that is connected with nitrogen protection is the monofilm chamber microwave reactor of 2.45GHz, is under the condition of 600～800W at microwave output power, heating 60～80s, and the cooling back is taken out and is got final product.
3 the present invention compared with prior art, have following advantage: the tobacco rod that (1) selects one of huge agriculture and forestry organic waste material of Yunnan Province's output for use is as one of preparation raw material of wood ceramics, not only utilized the abundant tobacco rod resource of our province, improved the added value of tobacco industry, can replace simultaneously needed timber in the existing wood ceramics manufacturing process, protect ecotope; (2) adopt elder generation that tobacco rod is carried out charing, method with the resol mixing moulding prepares wood ceramics then, adopt this method to prepare wood ceramics, not only solve the uneven problem of resin impregnating in the existing method, saved the operation that utility appliance such as ultrasonic wave are carried out resin impregnating simultaneously.Simultaneously, enhance product performance effectively, saved the consumption of resol, reduced cost; (3) adopting microwave as the energy, the preparation time of wood ceramics is shortened to 60～80s, is 0.8～2.2% of prior art, has shortened preparation time significantly.
Four, embodiment
Used tobacco rod is taken from the Yunnan Yuxi in the following example, and behind the natural air drying, its chemical constitution sees Table 1; The 2130 resol system that adopts by phenol and formaldehyde in the presence of sodium carbonate catalyst, the heat-reactive phenolic resin that after polycondensation, makes.Its outward appearance is the reddish-brown thick liquid.Quality index is as shown in table 2; Ethanol, analytical pure (CH
3CH
2OH content is no less than 99.7wt%), subsequently with an amount of distilled water mixed diluting to 20wt%.
The chemical constitution of table 1 tobacco rod
The quality standard of table 2 2130 resol
Embodiment one:
The first step: tobacco rod pulverized after temperature is 400 ℃ of following charings to obtain the tobacco rod powdered carbon that particle diameter is not more than 150 μ m be raw material, get tobacco rod powdered carbon 80g, with resol and the 186.67g ethanolic soln thorough mixing of 56g;
Second step: in temperature is 80 ℃ of oven dry 0.5h removal part ethanol and moisture down, is compacting 10min moulding under 8～12Mpa at pressure then, has formed tobacco rod charcoal/resol mixture;
The 3rd step: mixture is carried out pre-charing, and promptly rising to temperature with the temperature rise rate of 20 ℃/min is under 500 ℃, insulation 30min;
The 4th step: fast mixture is taken out, putting into the microwave frequency that is connected with nitrogen protection is the monofilm chamber microwave reactor of 2.45GHz, is under the condition of 800W at microwave output power, heating 80s, and taking-up gets final product behind the furnace cooling.
Embodiment two:
The first step: tobacco rod pulverized after temperature is 400 ℃ of following charings to obtain the tobacco rod powdered carbon that particle diameter is not more than 150 μ m be raw material, get tobacco rod powdered carbon 50g, with resol and the 116.67g ethanolic soln thorough mixing of 50g;
Second step: in temperature is 80 ℃ of oven dry 0.5h removal part ethanol and moisture down, is compacting 10min moulding under 8～12Mpa at pressure then, has formed tobacco rod charcoal/resol mixture;
The 3rd step: mixture is carried out pre-charing, and promptly rising to temperature with the temperature rise rate of 20 ℃/min is under 500 ℃, insulation 30min;
The 4th step: fast mixture is taken out, putting into the microwave frequency that is connected with nitrogen protection is the monofilm chamber microwave reactor of 2.45GHz, is under the condition of 720W at microwave output power, heating 80s, and taking-up gets final product behind the furnace cooling.
Embodiment three:
The first step: tobacco rod pulverized after temperature is 400 ℃ of following charings to obtain the tobacco rod powdered carbon that particle diameter is not more than 150 μ m be raw material, get tobacco rod powdered carbon 35g, with resol and the 81.67g ethanolic soln thorough mixing of 35g;
Second step: in temperature is g0 ℃ of oven dry 0.5h removal part ethanol and moisture down, is compacting 10min moulding under 8～12Mpa at pressure then, has formed tobacco rod charcoal/resol mixture;
The 3rd step: mixture is carried out pre-charing, and promptly rising to temperature with the temperature rise rate of 20 ℃/min is under 500 ℃, insulation 30min;
The 4th step: fast mixture is taken out, putting into the microwave frequency that is connected with nitrogen protection is the monofilm chamber microwave reactor of 2.45GHz, is under the condition of 800W at microwave output power, heating 70s, and taking-up gets final product behind the furnace cooling.
The product of above-mentioned three embodiment takes out the back and measures its performance, and performance data is as shown in table 3.
Every performance tabulation of table 3 embodiment product
Claims (1)
1. the method with preparing wood ceramics from tobacco straw castoff comprises tobacco rod charing, pulverizing, mix with resol and ethanolic soln, and oven dry, compression moulding, pre-charing, microwave heating is prepared into wood ceramics product several steps, it is characterized in that:
Do raw material 1.1 adopt the tobacco rod of natural air drying, in temperature is 400 ℃ of following charings, be crushed to particle diameter subsequently and be not more than 150 μ m, raw material as the preparation wood ceramics, tobacco rod powdered carbon after the pulverizing and certainweight resol and composition are the ethanolic soln thorough mixing of 20wt%, and the weight of material ratio is: tobacco rod charcoal: resol=100:30～30:100; Tobacco rod charcoal: ethanolic soln=30:70;
1.2 is 80 ℃ of oven dry 0.5h removal part ethanol and moisture down with mixed material in temperature, is compacting 10min moulding under 8～12MPa at pressure then, has formed tobacco rod charcoal/resol mixture;
1.3 mixture is carried out pre-charing, and promptly rising to temperature with the temperature rise rate of 20 ℃/min is 500 ℃, insulation 30min;
1.4 the monofilm chamber microwave reactor that the microwave frequency that is connected with nitrogen protection is 2.45GHz is put in the taking-up of the mixture after the pre-charing, be under the condition of 600～800W at microwave output power, heating 60～80s, the cooling back is taken out and is obtained the wood ceramics product.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100661589A CN100526258C (en) | 2007-09-03 | 2007-09-03 | Method for preparing wood ceramics from tobacco straw castoff |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100661589A CN100526258C (en) | 2007-09-03 | 2007-09-03 | Method for preparing wood ceramics from tobacco straw castoff |
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| CN101143788A CN101143788A (en) | 2008-03-19 |
| CN100526258C true CN100526258C (en) | 2009-08-12 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351564B (en) * | 2011-07-20 | 2012-11-21 | 福州大学 | Method for preparing wood ceramics by sintering coal tar pitch and biomass materials |
| CN104261869B (en) * | 2014-09-28 | 2015-12-30 | 齐齐哈尔大学 | A kind of preparation method of resin base wood ceramics matrix material |
| CN105060894B (en) * | 2015-08-05 | 2017-10-31 | 西北农林科技大学 | A kind of method for preparing zirconium carbide wood ceramics |
| CN107056250A (en) * | 2017-05-31 | 2017-08-18 | 合肥创沃科技有限公司 | A kind of preparation method for the wood ceramics material that attapulgite is combined with stalk |
| CN110304921A (en) * | 2019-06-12 | 2019-10-08 | 魏炎梅 | A kind of wood Ceramic Composite anticracking material |
| NO346974B1 (en) * | 2021-05-14 | 2023-03-20 | Procarbon Bio Ab | Charcoal products made with cardanol |
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2007
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| CN101143788A (en) | 2008-03-19 |
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