CN103721999A - Liquefaction method of forest litter - Google Patents
Liquefaction method of forest litter Download PDFInfo
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- CN103721999A CN103721999A CN201310725526.1A CN201310725526A CN103721999A CN 103721999 A CN103721999 A CN 103721999A CN 201310725526 A CN201310725526 A CN 201310725526A CN 103721999 A CN103721999 A CN 103721999A
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Abstract
The invention discloses a liquefaction method of forest litter, and belongs to the technical field of bioengineering. The liquefaction method is characterized by comprising the following steps: 1) collecting outdoor naturally withering leaves as materials, baking and then crushing, and baking again at the same temperature so as to obtain litter powder; (2) putting phenol into a water bath at 50-80 DEG C to heat for 10-21 minutes; rapidly pouring into a reaction kettle when the phenol is completely fused into liquid, controlling the temperature of the reaction kettle at 85-110 DEG C, and then adding the litter powder; slowly dropwise adding concentrated nitric acid and hydrogen peroxide after evenly stirring and mixing, stirring for 50-75 minutes until the liquid becomes dark red liquid, adding sodium dodecyl benzene sulfonate, stirring, mixing and dissolving uniformly, and stopping heating until the liquid becomes clear black liquid; 3) cooling the liquid to room temperature, so as to obtain litter liquefied liquid. The liquefaction method of the forest litter is low in liquefaction cost, simple and feasible, accurate and reliable, and the forest litter can be effectively liquefied.
Description
Technical field
The invention belongs to technical field of bioengineering, be specially a kind of liquifying method of Forest Litter.
Background technology
Forest Litter refers in the ecosystem that biological components produces and be returned to surface, forest land, originates, so as to maintaining the general name of all organic substances of ecosystem function as analyst's matter and energy.Forest Litter is metabolic product in forest plants growth and development process, in forest ecosystem Nutrient Cycling, plays an important role.At present, how to accelerate the decomposition of Litter-fall, or improve the utilization rate of Litter-fall, more and more cause silviculturist, ecologist and orest management worker's attention.
An effective way of natural material potential value is fully excavated in the liquefaction of biomaterial just, has obtained the attention of various countries He Ge scientific research departments, has also obtained a series of fruitful achievements.Briefly, biomaterial liquefaction refers to the existence at some organic matter or catalyst, and under pressurization or condition of normal pressure, biomaterial is converted into the thermochemical process of liquid.At present, liquifying method can be divided into hot method, thermochemical method, chemical hydrolysis and bioanalysis substantially.By liquefaction, can make Woody Biomass be converted into alcohols, flammable oil or other compound with particular functional group, thereby provide relevant raw material for the exploitation of new product.People have just considered to produce fuel and industrial chemicals with lignocellulose raw material as far back as the 1950's, but only limit to use pure by the use of thermal means.To during 20 century 70 oil crisis; people are increased to unprecedented degree to the interest of plant energy; the report of relevant lignocellulose raw material liquefaction occurs in a large number; some have even also been built up experimental with the raw petroliferous factory of plant material; but because production cost is higher, all fail large-scale production.At present, the liquifying method of Woody Biomass mainly contains following a few class substantially: phenol as liquefied reagent, polyalcohol as liquefied reagent, ring carbonate as liquefier.It is reported, Japanese forest comprehensive study starts the quick growing species of trees to carry out solubilization in 1991, the research of development functionality resin, through the liquefaction reaction thing of phenol, add formalin and make it wooden esterified, add curing agent, filler etc. again and make adhesive, its performance can meet or exceed Japanese JIS standard.But at present due to each side, Wood liquefied product is not also fully used, and its commercialization and industrialization also exist a lot of problems.
Liquefaction can be converted into energy and material, industrial chemicals etc. by Woody Biomass such as agriculture and forestry organic waste material, wood machining residues, thereby turns waste into wealth, and improves value, is also an effective way of these comprehensive utilizations of resources.But at present, due to the diversity of Woody Biomass chemical constituent, the complexity of liquefaction reaction process, and the liquefaction products arduousness that separates, characterize, at aspects such as the character of the control of the liquefaction mechanism of different biomaterial chemical compositions, liquefaction intermediate product, liquifying method, liquefaction products and utilizations, also need further further investigation.
Summary of the invention
In view of problems of the prior art, the object of the invention is to design provides a kind of technical scheme of liquifying method of Forest Litter, and its liquefaction cost is low, simple and easy to do, accurately and reliably and can efficient liquefaction Forest Litter.
The liquifying method of described a kind of Forest Litter, is characterized in that comprising the following steps:
1) collecting the leaf that naturally withers and falls of field is material, dries at 41-57 ℃ in baking oven, is then placed on and in pulverizer, is crushed to 200-450 order, again dries 35-56min under synthermal to obtain Litter-fall powder, standby;
2) phenol is placed in the water-bath of 50-80 ℃ and heats 10-21min, until it, be melted into completely when liquid and pour into rapidly in reactor, temperature of reaction kettle is controlled at 85-110 ℃, then add the Litter-fall powder in step 1), be uniformly mixed rear slow dropping red fuming nitric acid (RFNA) and hydrogen peroxide, stir 50-75min until liquid becomes kermesinus liquid, add again neopelex, be uniformly mixed and be uniformly dissolved, to it, become limpid black liquor and stop heating, wherein, Litter-fall: phenol: red fuming nitric acid (RFNA): hydrogen peroxide: the weight ratio of neopelex is 3-5:8-12:0.1-0.3:0.1-0.3:0.3-0.5,
3) by step 2) in liquid cools to room temperature, sealing preserve, obtain Litter-fall liquefier.
The liquifying method of described a kind of Forest Litter, is characterized in that rapid 1) in: bake out temperature is 45-50 ℃, is crushed to 300-400 order, again dries 40-50min under synthermal.
The liquifying method of described a kind of Forest Litter, is characterized in that step 2) in: bath temperature is 55-75 ℃, preferably 60-70 ℃; Water-bath time 15-18min, stirs 60-70min after dropping red fuming nitric acid (RFNA) and hydrogen peroxide.
The liquifying method of described a kind of Forest Litter, is characterized in that step 2) in: temperature of reaction kettle is preferably 89-100 ℃, preferably 92-95 ℃.
The liquifying method of described a kind of Forest Litter, is characterized in that step 2) in: phenol: red fuming nitric acid (RFNA): hydrogen peroxide: the weight ratio of neopelex is 4:9-10:0.2:0.2:0.4.
The liquifying method of above-mentioned a kind of Forest Litter, naturally the plant leaves dropping with nature, the Litter-falls such as bark carry out biomass liquefying and performance transformation, by liquefaction, Litter-fall is turned waste into wealth, solved the difficult problem that Litter-fall liquefies in production and application process, technical support is provided for developing new product, has naturally rotted with traditional Litter-fall, compared with discarded situation, expanded its range of application and function.The method applied in the present invention is more simple and easy to do, and accurately and reliably, liquefaction cost is low, accuracy is higher, can make Litter-fall well be liquefied
.
In present specification, apart from outside specified otherwise, percentage composition is the weight percentage of pure material.
The specific embodiment
Now, in conjunction with specific embodiments of the invention, further illustrate beneficial effect of the present invention.
Embodiment 1
The leaf being withered and fallen naturally in field is put into baking oven at 42 ℃ dries, after oven dry, with pulverizer, be crushed to 400 orders, under synthermal, again dry 39min and obtain Litter-fall powder, then getting 100kg phenol is placed in the water-bath of 65 ℃ and heats 12min, until it, be melted into completely when liquid and pour into rapidly in reactor, temperature of reaction kettle is controlled at 95 ℃, add 40kg Litter-fall powder, be uniformly mixed rear slow dropping 2kg red fuming nitric acid (RFNA) and 2kg hydrogen peroxide, stir 50min until liquid becomes kermesinus liquid, add again 4kg neopelex, be uniformly mixed and be uniformly dissolved, to it, become limpid black liquor and stop heating, finally be cooled to room temperature, sealing is preserved, obtain Litter-fall liquefier.
Embodiment 2
The leaf being withered and fallen naturally in field is put into baking oven at 51 ℃ dries, after oven dry, with pulverizer, be crushed to 350 orders, under synthermal, again dry 50min and obtain Litter-fall powder, then getting 100kg phenol is placed in the water-bath of 75 ℃ and heats 18min, until it, be melted into completely when liquid and pour into rapidly in reactor, temperature of reaction kettle is controlled at 93 ℃, add 40kg Litter-fall powder, be uniformly mixed rear slow dropping 2kg red fuming nitric acid (RFNA) and 2kg hydrogen peroxide, stir 75min until liquid becomes kermesinus liquid, add again 4kg neopelex, be uniformly mixed and be uniformly dissolved, to it, become limpid black liquor and stop heating, finally be cooled to room temperature, sealing is preserved, obtain Litter-fall liquefier.
Embodiment 3
The leaf being withered and fallen naturally in field is put into baking oven at 44 ℃ dries, after oven dry, with pulverizer, be crushed to 300 orders, under synthermal, again dry 41min and obtain Litter-fall powder, then getting 100kg phenol is placed in the water-bath of 70 ℃ and heats 14min, until it, be melted into completely when liquid and pour into rapidly in reactor, temperature of reaction kettle is controlled at 91 ℃, add 40kg Litter-fall powder, be uniformly mixed rear slow dropping 2kg red fuming nitric acid (RFNA) and 2kg hydrogen peroxide, stir 55min until liquid becomes kermesinus liquid, add again 4kg neopelex, be uniformly mixed and be uniformly dissolved, to it, become limpid black liquor and stop heating, finally be cooled to room temperature, sealing is preserved, obtain Litter-fall liquefier.
Embodiment 4
The leaf being withered and fallen naturally in field is put into baking oven at 46 ℃ dries, after oven dry, with pulverizer, be crushed to 250 orders, under synthermal, again dry 44min and obtain Litter-fall powder, then getting 100kg phenol is placed in the water-bath of 60 ℃ and heats 15min, until it, be melted into completely when liquid and pour into rapidly in reactor, temperature of reaction kettle is controlled at 90 ℃, add 40kg Litter-fall powder, be uniformly mixed rear slow dropping 2kg red fuming nitric acid (RFNA) and 2kg hydrogen peroxide, stir 60min until liquid becomes kermesinus liquid, add again 4kg neopelex, be uniformly mixed and be uniformly dissolved, to it, become limpid black liquor and stop heating, finally be cooled to room temperature, sealing is preserved, obtain Litter-fall liquefier.
Embodiment 5
The leaf being withered and fallen naturally in field is put into baking oven at 48 ℃ dries, after oven dry, with pulverizer, be crushed to 450 orders, under synthermal, again dry 47min and obtain Litter-fall powder, then getting 100kg phenol is placed in the water-bath of 80 ℃ and heats 16min, until it, be melted into completely when liquid and pour into rapidly in reactor, temperature of reaction kettle is controlled at 96 ℃, add 40kg Litter-fall powder, be uniformly mixed rear slow dropping 2kg red fuming nitric acid (RFNA) and 2kg hydrogen peroxide, stir 65min until liquid becomes kermesinus liquid, add again 4kg neopelex, be uniformly mixed and be uniformly dissolved, to it, become limpid black liquor and stop heating, finally be cooled to room temperature, sealing is preserved, obtain Litter-fall liquefier.
Embodiment 6
The leaf being withered and fallen naturally in field is put into baking oven at 50 ℃ dries, after oven dry, with pulverizer, be crushed to 200 orders, under synthermal, again dry 49min and obtain Litter-fall powder, then getting 100kg phenol is placed in the water-bath of 50 ℃ and heats 17min, until it, be melted into completely when liquid and pour into rapidly in reactor, temperature of reaction kettle is controlled at 89 ℃, add 40kg Litter-fall powder, be uniformly mixed rear slow dropping 2kg red fuming nitric acid (RFNA) and 2kg hydrogen peroxide, stir 70min until liquid becomes kermesinus liquid, add again 4kg neopelex, be uniformly mixed and be uniformly dissolved, to it, become limpid black liquor and stop heating, finally be cooled to room temperature, sealing is preserved, obtain Litter-fall liquefier.
By test, further illustrate beneficial effect of the present invention below.
Table 1 shows the embodiment 1-6 Litter-fall that all can effectively liquefy, and wherein, embodiment 1 is better than embodiment 2, and embodiment 3 is better than embodiment 4, and embodiment 5 is better than embodiment 6.
Claims (5)
1. a liquifying method for Forest Litter, is characterized in that comprising the following steps:
1) collecting the leaf that naturally withers and falls of field is material, dries at 41-57 ℃ in baking oven, is then placed on and in pulverizer, is crushed to 200-450 order, again dries 35-56min under synthermal to obtain Litter-fall powder, standby;
2) phenol is placed in the water-bath of 50-80 ℃ and heats 10-21min, until it, be melted into completely when liquid and pour into rapidly in reactor, temperature of reaction kettle is controlled at 85-110 ℃, then add the Litter-fall powder in step 1), be uniformly mixed rear slow dropping red fuming nitric acid (RFNA) and hydrogen peroxide, stir 50-75min until liquid becomes kermesinus liquid, add again neopelex, be uniformly mixed and be uniformly dissolved, to it, become limpid black liquor and stop heating, wherein, Litter-fall: phenol: red fuming nitric acid (RFNA): hydrogen peroxide: the weight ratio of neopelex is 3-5:8-12:0.1-0.3:0.1-0.3:0.3-0.5,
3) by step 2) in liquid cools to room temperature, sealing preserve, obtain Litter-fall liquefier.
2. the liquifying method of a kind of Forest Litter as claimed in claim 1, is characterized in that rapid 1) in: bake out temperature is 45-50 ℃, is crushed to 300-400 order, again dries 40-50min under synthermal.
3. the liquifying method of a kind of Forest Litter as claimed in claim 1, is characterized in that step 2) in: bath temperature is 55-75 ℃, preferably 60-70 ℃; Water-bath time 15-18min, stirs 60-70min after dropping red fuming nitric acid (RFNA) and hydrogen peroxide.
4. the liquifying method of a kind of Forest Litter as claimed in claim 1, is characterized in that step 2) in: temperature of reaction kettle is preferably 89-100 ℃, preferably 92-95 ℃.
5. the liquifying method of a kind of Forest Litter as claimed in claim 1, is characterized in that step 2) in: phenol: red fuming nitric acid (RFNA): hydrogen peroxide: the weight ratio of neopelex is 4:9-10:0.2:0.2:0.4.
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| CN201310725526.1A CN103721999B (en) | 2013-12-25 | 2013-12-25 | A kind of liquifying method of Forest Litter |
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| CN201310725526.1A CN103721999B (en) | 2013-12-25 | 2013-12-25 | A kind of liquifying method of Forest Litter |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04357002A (en) * | 1991-02-01 | 1992-12-10 | Nippon Mokuzai Boufu Kogyo Kumiai | Method of treating rot-proof and insect-proof lumber waste material |
| US5364475A (en) * | 1993-07-30 | 1994-11-15 | State Of Oregon Acting By And Through The State Board Of Higher Education On Behalf Of Oregon State University | Process for removing chemical preservatives from wood using supercritical fluid extraction |
| JP2004255362A (en) * | 2003-02-26 | 2004-09-16 | Yasunobu Yoshida | Method of producing fuel for burning cement by drying construction and demolition waste and its device |
| JP2005297250A (en) * | 2004-04-07 | 2005-10-27 | Komiya Kazuhiro | Method and apparatus for solidifying wood chip and solidified wood chip |
| JP2008049691A (en) * | 2006-07-27 | 2008-03-06 | Sumitomo Forestry Co Ltd | Long-term preserving method of lumber |
| JP2008207144A (en) * | 2007-02-28 | 2008-09-11 | Shiro Saka | Thermoplastic woody biomaterial manufacturing method and thermoplastic woody biomaterial |
| CN101396838A (en) * | 2008-10-31 | 2009-04-01 | 中国林业科学研究院林产化学工业研究所 | Wood liquefier and method for preparing surfactant using liquidated wood |
| CN102515928A (en) * | 2011-10-18 | 2012-06-27 | 西北农林科技大学 | Composition for preparing drought-resisting yellow humic acid fertilizer and method thereof |
-
2013
- 2013-12-25 CN CN201310725526.1A patent/CN103721999B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04357002A (en) * | 1991-02-01 | 1992-12-10 | Nippon Mokuzai Boufu Kogyo Kumiai | Method of treating rot-proof and insect-proof lumber waste material |
| US5364475A (en) * | 1993-07-30 | 1994-11-15 | State Of Oregon Acting By And Through The State Board Of Higher Education On Behalf Of Oregon State University | Process for removing chemical preservatives from wood using supercritical fluid extraction |
| JP2004255362A (en) * | 2003-02-26 | 2004-09-16 | Yasunobu Yoshida | Method of producing fuel for burning cement by drying construction and demolition waste and its device |
| JP2005297250A (en) * | 2004-04-07 | 2005-10-27 | Komiya Kazuhiro | Method and apparatus for solidifying wood chip and solidified wood chip |
| JP2008049691A (en) * | 2006-07-27 | 2008-03-06 | Sumitomo Forestry Co Ltd | Long-term preserving method of lumber |
| JP2008207144A (en) * | 2007-02-28 | 2008-09-11 | Shiro Saka | Thermoplastic woody biomaterial manufacturing method and thermoplastic woody biomaterial |
| CN101396838A (en) * | 2008-10-31 | 2009-04-01 | 中国林业科学研究院林产化学工业研究所 | Wood liquefier and method for preparing surfactant using liquidated wood |
| CN102515928A (en) * | 2011-10-18 | 2012-06-27 | 西北农林科技大学 | Composition for preparing drought-resisting yellow humic acid fertilizer and method thereof |
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