CN105130712A - Tobacco stem biochar organic fertilizer and application method thereof - Google Patents
Tobacco stem biochar organic fertilizer and application method thereof Download PDFInfo
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Abstract
The invention discloses tobacco stem biochar organic fertilizer. The tobacco stem biochar organic fertilizer is formed by evenly mixing, by weight, 40-60 parts of tobacco stem biochar particles and 40-60 parts of calcium-magnesium fertilizer. The formula involves the tobacco stem biochar particles and the calcium-magnesium fertilizer, and the keys of the tobacco stem biochar organic fertilizer are the matching of the tobacco stem biochar particles and the calcium-magnesium fertilizer and preparation of the tobacco stem biochar particles. Resource waste caused by abandonment or direct combustion of tobacco stems serving as waste can be avoided through the tobacco stem biochar, and environmental pollution is reduced; the prepared organic fertilizer can provide necessary potassium, calcium, magnesium, phosphorus and other nutrients for plant growth and can improve heavy soil, increase soil permeability, enhance microorganism activity and prolong chemical fertilizer effect release time when applied as base fertilizer, and compared with single application, heavy metal accumulation on crops can be better reduced through combination of the tobacco stem biochar particles and the calcium-magnesium fertilizer.
Description
Technical field
Patent of the present invention relates to a kind of cigarette stalk charcoal fertilizer and application process thereof, belongs to fertilizer and applied technical field.
Background technology
Tobacco is Solanaceae Nicotiana plant, a kind of important cash crop, it accounts for significant proportion in the cultivated area of southwest, its cigarette stalk quality is harder, after existing tobacco leaf of having gathered, remaining cigarette stalk is often discarded in field by as waste or directly burns, not only waste resource, also easily cause environmental pollution.According to statistics, China about produces 1,500,000 tons of cigarette stalks every year.Therefore, the importance of carrying out the correlative study of cigarette stalk recycling is self-evident.At present the resource utilization method of cigarette stalk is mainly comprised to gac preparation, extracts several aspect such as xylo-oligosaccharide and pectin, processing artificial boards, extraction oil fuel and chemical materials, production fertilizer and culture medium, but the mass-producing in actual production is applied seldom.Still there is in national Main Tobacco Planting district a large amount of discarded cigarette stalks to pile up field at present, not only ecotope and ecoscape are all made a big impact, too increase the probability that tobacco disease insect pest is propagated simultaneously.Along with the development of charcoal research, applicant thinks that pyrolysis cigarette stalk is prepared biomass charcoal and can be become the important channel realizing cigarette stalk recycling.
Biomass charcoal is by biomass agriculture and forestry organic waste material, plant tissue or carcase and ight soil etc. pyrolysis and a kind of solid product containing carbon rich of being formed under high temperature anaerobic condition.Large quantity research shows, after biomass charcoal is manured into soil, can increases soil aeration and water-retentivity, increase soil fertility, and reduces heavy metal and organic pollutant toxicity, improves edatope.All right Promoting plant growth, improves crop yield, and can strengthen fixing carbon by soil, reduces soil carbon quantity discharged.A large amount of scholar adopts different types of biomass to be research object for this reason, has investigated the impact of pyrolysis temperature on biomass charcoal physico-chemical property.But, also rarely have report with the correlative study that cigarette stalk is biomass material.
Simultaneously applicant thinks that single cigarette stalk to be prepared into biomass material effect in the process in also field comparatively single, and economic worth is lower, and itself and other material matching is prepared into fertilizer can further improve its economic worth.
Summary of the invention
The technical problem to be solved in the present invention is, provides a kind of and effectively can utilize the cigarette stalk charcoal fertilizer and application process thereof that cigarette stalk, economic worth are high, result of use is good, can overcome the deficiencies in the prior art.
Technical scheme of the present invention is: cigarette stalk charcoal fertilizer, and it is made up of the former material Homogeneous phase mixing of following weight proportion, cigarette stalk charcoal particle 40-60 part, ca and mg fertilizer 40-60 part.
Above-mentioned cigarette stalk charcoal fertilizer, it is made up of the former material Homogeneous phase mixing of following weight proportion, cigarette stalk charcoal particle 50 parts, ca and mg fertilizer 50 parts.
Described cigarette stalk charcoal is that the cigarette stalk of collection is become water content 8%-15% at field natural air drying; , air-dry cigarette stalk original state is loaded in charring furnace, under anaerobic with 10 DEG C of min
-1the slow pyrolysis of temperature rise rate, pyrolysis top temperature chooses 450 DEG C, continue to keep 2h when reaching top temperature, point is crushed to 10-30 order after the cigarette stalk biomass charcoal after pyrolysis is cooled to room temperature.
Described ca and mg fertilizer index is CaO content 25%, content of MgO 7%, pH10, product standard: Q/DZ4-2012, registration card number: No. 2336, the accurate word of agriculture fertilizer (2012).
The application process of described cigarette stalk charcoal fertilizer is that the cigarette stalk charcoal particle be mixed and ca and mg fertilizer are transported to field, and base fertilizer is spreaded manuer in holes, every mu of usage quantity 220kg, and all the other cultivations are consistent with conventional flue-cured tobacco cultivation technology with management.
Compared with the prior art, formula of the present invention relates to cigarette stalk charcoal particle and ca and mg fertilizer, and the preparation of the collocation both it and cigarette stalk charcoal particle is the key point of the application.And cigarette stalk charcoal can avoid cigarette stalk to abandon as waste or the waste resource brought of directly burning, also environmental pollution can be reduced, but in order to obtain most suitable as the cigarette stalk charcoal particle of soil improvement agent for agriculture production, applicant carried out great many of experiments, it prepares biomass charcoal under different pyrolysis temperature condition.Comparative analysis pyrolysis temperature, on the impact of the physico-chemical property such as productive rate, pH value, specific conductivity, specific surface area, constituent content, surface property of cigarette stalk biomass charcoal, evaluates its application potential as soil improvement agent, concrete process of the test and data as follows:
1 materials and methods
The preparation of 1.1 cigarette stalk biomass charcoals
Test cigarette stalk used and pick up from Bijie City, Guizhou Province prestige Ning County cigarette ground in flakes, the cigarette stalk gathered becomes water content 8%-15% at field natural air drying; , by air-dry cigarette stalk original state loading charring furnace, (ECO5000, charing treatment chamber effective dimensions is
volume 5L, pyrolysis temperature and power can set, chamber temperature 600 ~ 900 DEG C, and charing working spaces temperature 350 ~ 800 DEG C, equipment exposed outer surface temperature is not higher than 50 DEG C.), with 10 DEG C of min under relative anaerobic condition
-1the slow pyrolysis of temperature rise rate, pyrolysis top temperature chooses 350 DEG C, 400 DEG C, 450 DEG C, 500 DEG C, 550 DEG C and 600 DEG C of six temperature respectively, continue when reaching top temperature to keep 2h to make the abundant pyrolysis of sample, counterpoise re-heat solution prepares three times under all temperature conditions, cross 20 and 100 order stainless steel sifts respectively after cigarette stalk biomass charcoal after pyrolysis being cooled to room temperature, preserve to be analyzed.
1.2 sample determination
1.2.1 the basic physical and chemical of cigarette stalk biomass charcoal
Cigarette stalk biomass charcoal yield (Y), by the quality W of cigarette stalk before pyrolysis
1with the quality W of pyrolysis artifact matter charcoal
2calculate gained, calculation formula is Y=W
2/ W
1× 100%.
The pH value of cigarette stalk biomass charcoal, presses 1:20 (w/v) mixing, fully stirs 1h with glass stick, measure the pH value of cigarette stalk biomass charcoal under 25 DEG C of conditions after leaving standstill with pH meter by cigarette stalk biomass charcoal and deionized water.
The specific conductivity (EC) of cigarette stalk biomass charcoal, cigarette stalk biomass charcoal and deionized water are pressed 1:10 (w/v) to mix, under 25 DEG C of conditions, specific conductivity (EC) is measured with conductivitimeter (DDS-307 type, upper marine rainbow benefit instrument company limited) after abundant stirring.
The specific surface area (BET) of cigarette stalk biomass charcoal, utilizes specific surface area analysis instrument (TristarII3020, MicromeriticaInstrumentCorporation, the U.S.) to measure under 77K condition of nitrogen gas.
Measure the content of C, N and H element in cigarette stalk biomass charcoal, and calculate the content of O element, adopt elemental analyser (FlashEA1112, ThermoFinnigan, Italy) measure the content of C, N and H element in cigarette stalk biomass charcoal, and calculate the content of O element.Mineral element (K, Ca, Mg, Al, Cu and Zn etc.) content, adopt nitrate acid and hydrofluoric acid-perchloric acid to disappear to boil, inductively coupled plasma atomic emission (ICP-OES, Optima2000, PerkinElmerCo., the U.S.) measure to disappear and boil the content of liquid Mineral Elements, measure to disappear with employing molybdenum antimony resistance colorimetric method (700nm) and boil the content of P element in liquid.
1.2.2 Fourier transform infrared spectroscopy
Cigarette stalk biomass charcoal sample is mixed with the mass ratio of 1:50 with anhydrous K Br, on tabletting machine, uniform thin slice is pressed into after agate mortar grinding, Fourier transform infrared spectrometer (Nicoletis10, the U.S.) measures, and measurement range is wavelength 4000 ~ 400cm
-1, resolving power is 4cm
-1, the surface characteristic of biomass charcoal is analyzed by Spectral Characteristic.
1.2.3X-diffraction X-ray analysis X
Adopt X-ray diffractometer (X'PertPRO, PANalytical, Holland) to measure cigarette stalk biomass charcoal atomic structure and thing phase, instrument adopts Cuk alpha-ray, and wavelength is 0.1541nm.Operating voltage is 30Kv, electric current 30mA, and step-length is 0.01 °, and scope is from 10 ° to 80 °.
1.2.4 scanning electron microscope-energy spectrum analysis
Use SU8010 emission scan Electronic Speculum (HITACHI, Japan) and OXFORDAztec energy spectrometer (X-Max respectively
n, OxrordInstruments, the U.S.) and measure the surface tissue of cigarette stalk biomass charcoal, form and surface-element composition.
1.2.5 nucleus magnetic resonance
Cigarette stalk biomass charcoal solid-state cross-polarized-Magic angle spinning
13c nuclear magnetic resonance spectroscopy adopts AVANCEII300MH nuclear magnetic resonance analyser (Brooker company),
13c frequency is 75.5MHz, magic angle rotation frequency is 5kHz, duration of contact is 2ms, cycling time is 2.5s, and the diameter of rotor is 7mm.
1.3 data statistic analysis
Excel2007 and SPSS17.0 software is adopted to process and statistical study data, use one-way analysis of variance (ANOVA) and Duncan ' s multiple comparisons to carry out data analysis, in article table, different lowercase alphabet differential is different has statistical significance (P<0.05); The mapping of application Origin8.0 software.
2 results and discussion
The productive rate of 2.1 cigarette stalk biomass charcoals, pH value and specific conductivity
The yield of the cigarette stalk biomass charcoal prepared under condition of different temperatures, pH value and specific conductivity are as shown in table 1.The yield of biomass charcoal reduces gradually with the rising of pyrolysis temperature, and in 350 ~ 600 DEG C, the pyrolysis yield of cigarette stalk is 45.23% ~ 33.42%, when pyrolysis temperature is greater than 500 DEG C, and the yield there was no significant difference of gained biomass charcoal.Compared with 350 DEG C, when pyrolysis temperature rises to 400 DEG C, yield reduces by 9.13%; When pyrolysis temperature rises to 450 DEG C from 400 DEG C, yield reduces by 1.84%; When pyrolysis temperature continues to rise to 500 DEG C, yield reduces by 1.9%.
The cigarette stalk biomass charcoal that between 350 ~ 600 DEG C prepared by pyrolysis all in alkalescence, 9.13 when being 350 DEG C that pH value is minimum, when being up to 450 DEG C 9.98.When pyrolysis temperature is less than 450 DEG C, along with the rising of pyrolysis temperature, the pH value of cigarette stalk biomass charcoal is in remarkable (P<0.05) increasing trend.When pyrolysis temperature rises to 500 DEG C by 450 DEG C, the pH of cigarette stalk biomass charcoal significantly reduces, and research shows, because most of biomass charcoal is in alkalescence, in improvement acid soil, has very large potentiality, by as the very potential soil improvement agent of one.
When pyrolysis temperature rises to 600 DEG C from 350 DEG C, the conductivity variations of gained cigarette stalk biomass charcoal is comparatively large, from 2.29mScm
-1to 5.46mScm
-1, often improve a thermograde, specific conductivity all significantly (P<0.05) increases.Wherein, when pyrolysis temperature is increased to 500 DEG C by 450 DEG C, the specific conductivity amplification of cigarette stalk biomass charcoal is maximum, adds 1.24mScm
-1, cigarette stalk biomass charcoal can improve specific conductivity and the cation exchange capacity of soil as modifying agent.
Table 1 differing temps cigarette stalk biomass charcoal yield, pH value, specific conductivity and specific surface area
Note: between same column different letter representative process, difference reaches conspicuous level (P<0.05).
The specific surface area of 2.2 cigarette stalk biomass charcoals and surface structure analysis
Specific surface area is the total surface area of certain material of unit mass or unit volume, comprises outer surface area and void surface area.Due to the existence in a large amount of space, the specific surface area of biomass charcoal may be tens times even hundreds of times of outer surface area.Therefore, after biomass charcoal is manured into soil, the ventilation property of soil can be increased, thus play the effect improving soil physics structure.The specific surface area of biomass charcoal and surface texture featur are the important parameters affecting its absorption property.The specific surface area of the cigarette stalk biomass charcoal prepared under condition of different temperatures is in table 1.
As seen from table, when pyrolysis temperature is lower than 500 DEG C, along with temperature raises, the specific surface area of cigarette stalk biomass charcoal, in the trend increased gradually, is up to 8.86m
2g
-1.When pyrolysis temperature rises to 550 DEG C, the specific surface area of gained cigarette stalk biomass charcoal is reduced to 4.51m
2g
-1, when pyrolysis temperature is 600 DEG C, the specific surface area of cigarette stalk biomass charcoal then rises to 8.05m again
2g
-1.Fig. 1 shows the scanning electron microscope (SEM) photograph of the cigarette stalk biomass charcoal prepared under 6 kinds of differing tempss.As seen from the figure, the surface tissue of different pyrolysis temperature on cigarette stalk biomass charcoal has different impacts, and cigarette stalk is in high temperature pyrolysis process, and biological surface structure is broken gradually, forms obvious pore texture on surface.The cigarette stalk biomass charcoal that under lower temperature conditions prepared by (350 ~ 500 DEG C) pyrolysis also has the skeleton structure of cigarette stalk, and pore texture is more regular, and size pore distribution is more even.The major cause forming this structure may be that biomass itself have sponge structure, defines bubble or pore when also may be pyrolysis when water vapor and gas effusion.Obviously be weaker than the cigarette biomass stalk charcoal of 450 DEG C and 500 DEG C preparations in the development degree of the cigarette stalk biomass charcoal pore texture of 350 DEG C and 400 DEG C preparations, this may be the continuation along with pyrolytic process, and volatile matter burst size increases and causes.When comparatively high temps (550 ~ 600 DEG C), the structure deteriorate of cigarette stalk biomass charcoal is comparatively serious, and pore texture is irregular, and pore size differs, and difference is larger.
The elementary composition analysis of 2.3 cigarette stalk biomass charcoals
The content balance of C, N, H and O tetra-kinds of elements that table 2 is the cigarette stalk biomass charcoal that utilizes elemental analyser to measure.Result shows, pyrolysis temperature determines the constituent content of cigarette stalk biomass charcoal.Along with the rising of pyrolysis temperature, the C content of cigarette stalk biomass charcoal rises to 66.03% (550 DEG C) from 54.65% (350 DEG C), and when pyrolysis temperature is 600 DEG C, C content is down to 65.04%; N content is then down to 1.64% (600 DEG C) by 2.21% (350 DEG C), and the N element content of different cigarette stalk biomass charcoal is relatively stable; Corresponding H element content then reduces gradually along with the rising of pyrolysis temperature, is down to 1.56% (600 DEG C) from 3.75% (350 DEG C).In general, with the rising of pyrolysis temperature in this research, the C element content of cigarette stalk biomass charcoal increases gradually, the corresponding reduction of H and O constituent content.
As shown in Table 2, H/C, O/C of cigarette stalk biomass charcoal and (O+N)/C atomic ratio with the rising of pyrolysis temperature in the trend reduced gradually.Along with the rising of pyrolysis temperature, cigarette stalk biomass charcoal H/C atomic ratio is down to 0.02 (600 DEG C) by 0.07 (350 DEG C), and O/C ratio and (O+N)/C are than being then down to 0.45 (550 DEG C) and 0.48 (550 DEG C) respectively from 0.72 (350 DEG C) and 0.76 (350 DEG C).Above four kinds of Elements Atom are than can the aromatize degree of characterising biological matter charcoal and polarity, and wherein, H/C and O/C is less, and aromatize degree is higher, and (O+N)/C is larger, and then polarity is larger.
Similar with other biomass charcoal, the elementary composition of cigarette stalk biomass charcoal mainly affects by pyrolysis temperature, along with pyrolysis temperature raises, the stability of cigarette stalk biomass charcoal also improves gradually, the ability of resisting microbial decomposition after being thus manured into soil is stronger, can in soil the stable existence long period, long-range impact is produced on soil carbon sink and edatope.
The elementary composition analysis of table 2 differing temps cigarette stalk biomass charcoal C, N, H and O
| Preparation temperature | C/％ | N/％ | H/％ | O/％ | H/C | O/C | (O+N)/C |
| 350℃ | 54.65 | 2.21 | 3.75 | 39.39 | 0.07 | 0.72 | 0.76 |
| 400℃ | 59.11 | 1.89 | 3.02 | 35.98 | 0.05 | 0.61 | 0.64 |
| 450℃ | 61.65 | 1.89 | 2.75 | 33.72 | 0.04 | 0.55 | 0.58 |
| 500℃ | 62.86 | 1.80 | 2.75 | 32.60 | 0.04 | 0.52 | 0.55 |
| 550℃ | 66.03 | 1.77 | 2.41 | 29.80 | 0.04 | 0.45 | 0.48 |
| 600℃ | 65.04 | 1.64 | 1.56 | 31.77 | 0.02 | 0.49 | 0.51 |
Cigarette stalk biomass charcoal Mineral Elements content is as shown in table 3, similar to C element, and cigarette stalk biomass charcoal Mineral Elements content raises with pyrolysis temperature and increases gradually.Its K, Al, Ca constituent content is higher, is respectively 28.46 ~ 35.47,16.95 ~ 35.86 and 13.15 ~ 24.95gkg
-1, Mg, P element content are lower, are respectively 4.82 ~ 7.73 and 0.43 ~ 0.72gkg
-1, Zn, Cu constituent content is then lower, is respectively 59.57 ~ 149.23 and 22.56 ~ 49.89mgkg
-1.And the rising of these Mineral Elements Contents is also the major cause that cigarette stalk biomass charcoal pH value raises.Can increase soil fertility after cigarette stalk biomass charcoal is manured into soil, for plant, microorganism provide essential nutrient element, thus improve soil quality.
The Mineral Elements Content of table 3 differing temps cigarette stalk biomass charcoal
Note: between same column different letter representative process, difference reaches conspicuous level (P<0.05).
In addition, the biomass charcoal prepared is carried out energy dispersion X-ray (EDS) and detect under condition of different temperatures, analyze the elementary composition and content (table 4) of certain point of cigarette stalk biomass charcoal surface.Result shows, certain of cigarette stalk biomass charcoal surface is a bit elementary composition primarily of C and O, in addition, also has the elements such as a small amount of Mg, Al, K, Ca and Cl.Along with the rising of pyrolysis temperature, C element content raises gradually, by 350 DEG C 79.25% increase to 600 DEG C 94.88%.Contrast table 2 and table 4 known, the surface C content of cigarette stalk biomass charcoal is all higher than the content of C total at same synthesis temperature, and this illustrates that the composition of cigarette stalk biomass charcoal has special heterogeneity.Pyrolysis temperature raises, and the content of cigarette stalk biomass charcoal surface O element reduces gradually, by 350 DEG C 18.99% be down to 550 DEG C 10.66%, when pyrolysis temperature is 600 DEG C, O element does not detect.This variation tendency consistent (table 2) with cigarette stalk biomass charcoal total O constituent content.Each cigarette stalk biomass charcoal is except Ca and Si content distribution irregularities, and the content of other element all increases progressively with pyrolysis temperature increase, and this illustrates that cigarette stalk biomass charcoal prepared by higher temperatures pyrolysis has higher surface polarity, and this illustrates that biomass charcoal surface is containing KCl.
Certain site energy-dispersive X-ray analysis of table 4 differing temps cigarette stalk biomass charcoal surface measures elementary composition and massfraction
| Preparation temperature | C/％ | O/％ | Mg/％ | Al/％ | Si/％ | S/％ | Cl/％ | K/％ | Ca/％ |
| 350℃ | 79.25 | 18.99 | 0.11 | 0.08 | -- | -- | -- | 1.28 | 0.37 |
| 400℃ | 81.52 | 16.30 | 0.08 | 0.08 | 0.46 | 0.15 | 0.12 | 1.10 | 0.19 |
| 450℃ | 82.50 | 13.92 | 0.10 | 0.18 | 0.34 | 0.27 | 0.12 | 2.05 | 0.51 |
| 500℃ | 83.15 | 14.13 | 0.12 | 0.15 | 0.58 | 0.19 | 0.08 | 1.21 | 0.38 |
| 550℃ | 86.87 | 10.66 | 0.18 | -- | 0.15 | 0.33 | -- | 1.81 | -- |
| 600℃ | 94.88 | -- | 0.15 | 0.15 | 0.38 | 0.33 | 0.27 | 3.49 | 0.35 |
Note: "--" representative does not detect.
2.4 cigarette stalk biomass charcoal Infrared spectroscopy
From Fig. 2 infrared spectra (FTIR), cigarette stalk biomass charcoal prepared by differing temps has similar charateristic avsorption band, but the vibration intensity difference of each characteristic peak is larger.When pyrolysis temperature is lower than 450 DEG C, at wavelength 3430cm
-1and 2940cm
-1place all has more weak absorption peak to detect, and proves to have in cigarette stalk biomass charcoal c h bond existence in phenolic hydroxyl group or alcoholic extract hydroxyl group and alkane, and when pyrolysis temperature rises to more than 500 DEG C, Liang Zhong functional group all disappears.When 450 ~ 550 DEG C of pyrolysis temperatures, wavelength 2380cm
-1place finds fats C-H and C=O absorption peak, and increases along with temperature raises absorption peak strength.Wave spectrum 1710cm
-1c=O key in place's representation carboxy, absorption peak strength is less, and when pyrolysis temperature is greater than 550 DEG C, this peak disappears.In addition, 1590cm
-1place's wave spectrum represents the-COO having unsymmetrically to stretch
–or fragrant C=C key exists, wave spectrum 1410cm
-1place represents the c h bond of aromatic series C=C key or distortion, wave spectrum 1100cm
-1place then represents the carbonate (CO of plain bending distortion
3 2-) or O-CH
3, in addition, wavelength 1100cm
-1and 785cm
-1place is all likely Si-O-Si vibration absorption peak.In sum, when preparing cigarette stalk biomass charcoal with lower pyrolysis temperature, multiple oxygen-containing functional group is defined.It is reported, these oxygen-containing functional groups make biomass charcoal have hydrophilic, hydrophobicity, and strengthen its surge capability to soda acid, are also the major reasons that biomass charcoal makes soil pH and CEC and improves.But along with the rising of pyrolysis temperature, these functional groups reduce gradually and even disappear, biomass charcoal cation exchange capacity (CEC) and heavy metal and Adsorption of Organic ability after being manured into soil, may be caused to reduce.
The X-ray diffracting spectrum analysis of 2.5 cigarette stalk biomass charcoals
Fig. 3 is X-ray diffraction (XRD) collection of illustrative plates of cigarette stalk biomass charcoal prepared by differing temps.As seen from the figure, 6 kinds of cigarette stalk biomass charcoals have similar diffraction peak, and different characteristics diffraction peak has varying strength.The crystal detected is respectively silicate or SiO
2(4.27,3.35,
), KCl (3.14,
) and CaCO
3(
), corresponding PDF card [86-1630], [72-1937] and [75-0296] number respectively.Along with the rising of pyrolysis temperature, except the SiO of 450 DEG C of cigarette stalk biomass charcoals
2characteristic peak is relatively more abnormal outer, and other diffraction peak intensity increases all gradually.This shows SiO in cigarette stalk biomass charcoal
2, KCl and CaCO
3crystal is with the raising enrichment gradually of pyrolysis temperature, and this is consistent to cigarette stalk biomass charcoal Mineral Elements Content (table 3) result with this research.Due to the existence of these crystalline structure, after cigarette stalk biomass charcoal is manured into soil, can effectively reduce H in soil
+and exchangeable Al
3+molality.In addition, there is orderly cellulose character peak at 2 θ ≈ 15 ° place in the cigarette stalk biomass charcoal of 350 DEG C, along with the rising of pyrolysis temperature, peak intensity reduces gradually and disappears.At 2 θ ≈ 24 ° and 43 ° of places, all there is the diffraction peak of the symbol graphite-structure that intensity is less, also fade away along with pyrolysis temperature raises, represent that in cigarette stalk biomass charcoal, class graphite microcrystalline structure is tending towards random stratification gradually.In theory, there is at the biomass charcoal that comparatively prepared by cold condition (350 ~ 450 DEG C) pyrolysis the graphite microcrystal of higher unformed and random layer, the stability of biomass charcoal can be improved, and the biomass charcoal aromatize degree that higher temperature conditions is formed is higher, containing class Graphene crystalline structure, the stability of biomass charcoal thus also can be improved.
2.6 cigarette stalk biomass charcoals
13c nuclear magnetic resonance map is analyzed
Cigarette stalk biomass charcoal
13c nucleus magnetic resonance (NMR) collection of illustrative plates as shown in Figure 4.Obviously, cigarette stalk biomass charcoal is primarily of alkyl carbon, aromatic carbon and a small amount of carboxyl, carbonyl charcoal composition.As shown in Table 5, (be less than 400 DEG C) when pyrolysis temperature is lower, organic based on fatty carbon in cigarette stalk biomass charcoal, aromatic carbon content takes second place, and carboxyl, carbonyl carbon content are minimum.Along with the raising of pyrolysis temperature, in biomass charcoal, alkyl carbon, methoxyl group and carbohydrate content reduce all gradually, and fatty total carbon is down to 13.34% by 34.53%, and aromatic carbon content then acutely raises, and rise to 74.04% by 29.21%.Carboxyl and carbonyl carbon content then change not quite, by 350 DEG C 15.43% rise to 550 DEG C 26.62%, 600 DEG C time, be then down to 13.34% again.This result proves the raising with pyrolysis temperature, and the aromatize degree of cigarette stalk biomass charcoal improves gradually.This is also consistent with O/C ratio (table 2) in this test and XRD analysis (Fig. 3) result.In addition, totally it seems, along with the raising of pyrolysis temperature, cigarette stalk biomass charcoal Semi-polarity carbon content reduces gradually, especially reduces the most obvious when pyrolysis temperature is 600 DEG C.This result is consistent with according to (O+N)/C ratio (table 2) conclusion.
The relative content of dissimilar C in table 5 differing temps cigarette stalk biomass charcoal
3 conclusions
(1) yield of cigarette stalk biomass charcoal reduces gradually with the rising of pyrolysis temperature, tends towards stability when pyrolysis temperature is greater than 500 DEG C.The pH value of cigarette stalk biomass charcoal reaches maximum 9.98 when pyrolysis temperature is 450 DEG C; Specific conductivity improves with pyrolysis temperature and increases gradually, and improves rapidly when pyrolysis temperature is 600 DEG C; Along with the raising of pyrolysis temperature, cigarette stalk biomass charcoal surface tissue is destroyed gradually, and surface-area raises gradually, reaches maximum 8.86m at 450 DEG C
2g
-1.
(2) with the raising of pyrolysis temperature, C content, the Mineral Elements Content of cigarette stalk biomass charcoal all increase, H/C, O/C, (O+N)/H reduce than gradually, and the aromaticity of cigarette stalk biomass charcoal and surface polarity improve, and integral polarity reduces gradually.Thus the stability of biomass charcoal and nutrient content all improve with the rising of pyrolysis temperature.
(3) analyze by carrying out FTIR, XRD and NMR to cigarette stalk biomass charcoal, find in pyrolytic process, cigarette stalk biomass charcoal surface forms multiple oxygen-containing functional group, along with the rising of pyrolysis temperature, functional group reduces gradually until disappear, and main based on aromatic carbon in cigarette stalk biomass charcoal organic matter.Biomass charcoal surface is also containing KCl and CaCO
3deng mineral and class graphite microcrystal, these crystal can improve stability and the absorption property of biomass charcoal.
Analyzed by above-mentioned detection, in conjunction with characteristic index variation tendencies such as biomass charcoal yield, pH, specific surface area, constituent content, surface texture featurs, applicant thinks the cigarette stalk biomass charcoal prepared under 450 DEG C of conditions most suitable as soil improvement agent for agriculture production.
And as the ca and mg fertilizer that its soil conditioner of arranging in pairs or groups selects Guangdong Dazhong Agriculture Science Share Ltd. to produce, it is containing CaO25%, MgO7%, pH10, it mates by 1:1 the fertilizer be mixed with the cigarette stalk biomass charcoal prepared under 450 DEG C of conditions can provide the required nutrient such as potassium, calcium, magnesium, phosphorus for plant-growth, use can improve heavy soil as base fertilizer, increase soil permeability, strengthen microorganism active, extend fertilizer efficiency release, simultaneously, combine the accumulation that more can reduce crop heavy metal than single administration.
For prove both with the use of effect, applicant carried out Comparability test, and acquire related data, in process of the test, single mu of conditioning agent, cigarette stalk biological carbon and the application amount of application of filling a prescription is identical, and the mean value eliminated after the highest and minimum data in data sees the following form:
Cigarette stalk charcoal and amendment mix the impact executed flue-cured tobacco economical character
| Process | Plant height (cm) | Effective blade number | Maximum leaf long (cm) | Maximum width of blade (cm) |
| Contrast | 128.65±4.25c | 21.34±0.45b | 69.32±3.19c | 24.44±0.22ab |
| Singly execute conditioning agent | 133.39±3.41c | 25.86±0.79b | 73.37±2.49c | 26.11±0.71ab |
| Singly execute cigarette stalk charcoal | 134.40±2.57ab | 25.46±1.12ab | 73.60±1.92b | 27.91±0.91ab |
| Cigarette stalk charcoal+tune | 137.34±3.19a | 27.32±0.87a | 77.37±3.28a | 28.61±1.21a |
| Reason agent |
As can be seen from the above table, adopt the application to fill a prescription cigarette stalk Biological carbon organic fertilizer Be very effective obtained, tobacco leaf conventional index all has and significantly promotes.
Accompanying drawing explanation
The scanning electron microscope (SEM) photograph of Fig. 1 differing temps cigarette stalk biomass charcoal;
The infrared spectra of Fig. 2 differing temps cigarette stalk biomass charcoal;
The x-ray diffraction pattern of Fig. 3 differing temps cigarette stalk biomass charcoal;
Fig. 4 differing temps cigarette stalk biomass charcoal
13c nuclear magnetic resonance map.
Embodiment
Embodiment 1, cigarette stalk charcoal fertilizer gets 800kg cigarette stalk charcoal particle, and 800kg ca and mg fertilizer is mixed, stand-by by 50kg pack sealing, be transported to field season to transplanting, base fertilizer is spreaded manuer in holes, every mu of usage quantity 220kg, all the other cultivations are consistent with conventional flue-cured tobacco cultivation technology with management.
Described cigarette stalk charcoal is that the cigarette stalk of collection is become water content 8%-15% at field natural air drying; , air-dry cigarette stalk original state loaded in charring furnace, preferred unpowered autothermal environment friendly biological matter automatic carbonization furnace, with 10 DEG C of min under relative anaerobic condition
-1the slow pyrolysis of temperature rise rate, pyrolysis top temperature chooses 450 DEG C, continue to keep 2h when reaching top temperature, point is crushed to 20 orders after the cigarette stalk biomass charcoal after pyrolysis is cooled to room temperature.Described ca and mg fertilizer index is CaO content 25%, content of MgO 7%, pH10, product standard: Q/DZ4-2012, registration card number: No. 2336, the accurate word of agriculture fertilizer (2012).
Embodiment 2, cigarette stalk charcoal fertilizer gets 1000kg cigarette stalk charcoal particle, and 1000kg ca and mg fertilizer is mixed, stand-by by 50kg pack sealing, be transported to field season to transplanting, base fertilizer is spreaded manuer in holes, every mu of usage quantity 220kg, all the other cultivations are consistent with conventional flue-cured tobacco cultivation technology with management.
Described cigarette stalk charcoal is that the cigarette stalk of collection is become water content 8%-15% at field natural air drying; , air-dry cigarette stalk original state loaded in charring furnace, preferred unpowered autothermal environment friendly biological matter automatic carbonization furnace, with 10 DEG C of min under relative anaerobic condition
-1the slow pyrolysis of temperature rise rate, pyrolysis top temperature chooses 450 DEG C, continue to keep 2h when reaching top temperature, point is crushed to 10 orders after the cigarette stalk biomass charcoal after pyrolysis is cooled to room temperature.Described ca and mg fertilizer index is CaO content 25%, content of MgO 7%, pH10, product standard: Q/DZ4-2012, registration card number: No. 2336, the accurate word of agriculture fertilizer (2012).
Embodiment 3: cigarette stalk charcoal fertilizer gets 1200kg cigarette stalk charcoal particle, and 1200kg ca and mg fertilizer is mixed, stand-by by 50kg pack sealing, field is transported to season to transplanting, base fertilizer is spreaded manuer in holes, every mu of usage quantity 220kg, and all the other cultivations are consistent with conventional flue-cured tobacco cultivation technology with management.
Described cigarette stalk charcoal is that the cigarette stalk of collection is become water content 8%-15% at field natural air drying; , air-dry cigarette stalk original state loaded in the charring furnace of autonomous design, preferred unpowered autothermal environment friendly biological matter automatic carbonization furnace, with 10 DEG C of min under relative anaerobic condition
-1the slow pyrolysis of temperature rise rate, pyrolysis top temperature chooses 450 DEG C, continue to keep 2h when reaching top temperature, point is crushed to 30 orders after the cigarette stalk biomass charcoal after pyrolysis is cooled to room temperature.Described ca and mg fertilizer index is CaO content 25%, content of MgO 7%, pH10, product standard: Q/DZ4-2012, registration card number: No. 2336, the accurate word of agriculture fertilizer (2012).
Claims (5)
1. a cigarette stalk charcoal fertilizer, is characterized in that: it is made up of the former material Homogeneous phase mixing of following weight proportion, cigarette stalk charcoal particle 40-60 part, ca and mg fertilizer 40-60 part.
2. cigarette stalk charcoal fertilizer according to claim 1, is characterized in that: it is made up of the former material Homogeneous phase mixing of following weight proportion, cigarette stalk charcoal particle 50 parts, ca and mg fertilizer 50 parts.
3. cigarette stalk charcoal fertilizer according to claim 1 and 2, it is characterized in that: described cigarette stalk charcoal is that the cigarette stalk of collection is become water content 8%-15% at field natural air drying, air-dry cigarette stalk original state is loaded in charring furnace, under anaerobic with 10 DEG C of min
-1the slow pyrolysis of temperature rise rate, pyrolysis top temperature chooses 450 DEG C, continue to keep 2h when reaching top temperature, point is crushed to 10-30 order after the cigarette stalk biomass charcoal after pyrolysis is cooled to room temperature.
4. cigarette stalk charcoal fertilizer according to claim 3, is characterized in that: described ca and mg fertilizer index is CaO content 25%, content of MgO 7%, pH10, product standard: Q/DZ4-2012, registration card number: No. 2336, the accurate word of agriculture fertilizer (2012).
5. the application process of cigarette stalk charcoal fertilizer as claimed in claim 4, it is characterized in that: the method is that the cigarette stalk charcoal particle be mixed and ca and mg fertilizer are transported to field, base fertilizer is spreaded manuer in holes, every mu of usage quantity 220kg, and all the other cultivations are consistent with conventional flue-cured tobacco cultivation technology with management.
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| CN106852215A (en) * | 2016-12-29 | 2017-06-16 | 中国农业大学 | A kind of biomass carbon is spreaded manuer in holes method |
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Application publication date: 20151209 |