CN106984283A - The method for preparing biomass absorbent material under cryogenic conditions using rice husk - Google Patents
The method for preparing biomass absorbent material under cryogenic conditions using rice husk Download PDFInfo
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- CN106984283A CN106984283A CN201710376148.9A CN201710376148A CN106984283A CN 106984283 A CN106984283 A CN 106984283A CN 201710376148 A CN201710376148 A CN 201710376148A CN 106984283 A CN106984283 A CN 106984283A
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- CN
- China
- Prior art keywords
- rice husk
- absorbent material
- biomass
- sieving
- drying
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000002028 Biomass Substances 0.000 title claims abstract description 35
- 235000007164 Oryza sativa Nutrition 0.000 title claims abstract description 35
- 235000009566 rice Nutrition 0.000 title claims abstract description 35
- 239000000463 material Substances 0.000 title claims abstract description 34
- 239000010903 husk Substances 0.000 title claims abstract description 33
- 239000002250 absorbent Substances 0.000 title claims abstract description 27
- 230000002745 absorbent Effects 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 19
- 240000007594 Oryza sativa Species 0.000 title 1
- 241000209094 Oryza Species 0.000 claims abstract description 34
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000007873 sieving Methods 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 238000004140 cleaning Methods 0.000 claims abstract description 9
- 238000007654 immersion Methods 0.000 claims abstract description 9
- 238000010304 firing Methods 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 7
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 4
- 238000001704 evaporation Methods 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- 235000019628 coolness Nutrition 0.000 claims abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052740 iodine Inorganic materials 0.000 abstract description 10
- 239000011630 iodine Substances 0.000 abstract description 10
- 238000007796 conventional method Methods 0.000 abstract description 8
- 238000001179 sorption measurement Methods 0.000 abstract description 8
- 230000004913 activation Effects 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000007812 deficiency Effects 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000004448 titration Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000002154 agricultural waste Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000005445 natural material Substances 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/485—Plants or land vegetals, e.g. cereals, wheat, corn, rice, sphagnum, peat moss
Landscapes
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Solid Fuels And Fuel-Associated Substances (AREA)
Abstract
The method for preparing biomass absorbent material under cryogenic conditions using rice husk：(1) biomass rice husk is cleaned, drying；Drying after rice husk it is ground, sieving, in reactor 180 DEG C firing 12h, natural cooling；(3) the burned product cleaning after coolings, drying, grinding, sieving；(4) a small amount of ethanol wet of burned product after sievings, and add a certain amount of sulfuric acid solution immersion 12h；(5) after immersions terminate, liquid evaporating completely is heated to；(6) cleans remaining solid to sulfate radical-free with deionized water；(7) then dries, grinds, sieving and to obtain biomass absorbent material.Instant invention overcomes the deficiencies in the prior art, biomass absorbent material is prepared under cryogenic, the equipment used is a conventional oven, firing temperature and activation temperature are all significantly lower than conventional method simultaneously, cost is less than conventional method more than 50%, and yield is also greater than conventional method, and the iodine sorption value of biomass carbon raw material is converted into also greater than conventional method.
Description
Technical field
The present invention relates to a kind of preparation method of biomass absorbent material, particularly discarded under cryogenic using agricultural
Thing --- rice husk, the method for preparing biomass absorbent material.
Background technology
China is a large agricultural country, has substantial amounts of agricultural wastes to produce every year, and these discarded objects are arbitrarily stacked not
Big quantity space is only occupied, and easily pollutes environment.Rice husk is a kind of discarded object that will necessarily be produced in rice de-hulling process, its
It is of low nutritive value, has been prohibited from using in animal feed.Therefore the place to go problem of rice husk is as during rice production
The problem of having to be solved.
Adsorb as a kind of effective method for removing heavy metal in solution, significant role is played in water treatment field.Pass
The adsorbent of system is mainly derived from natural sorbing material（Zeolite, diatomite etc.）, these sorbing material limited sources, not
Demand now can be met.Therefore find suitable sorbing material to replace natural material to become the study hotspot of numerous scholars.
Current most study is that rice husk is prepared biomass absorbent material under the high temperature conditions, and its preparation process is substantially
Such as Fig. 1.Although biomass absorbent material iodine sorption value prepared by this method is higher, yield is converted into unit than relatively low
The iodine sorption value of quality rice husk is also relatively low, and required temperature is higher, also corresponding higher to equipment requirement.Preparation technology
Flow chart such as Fig. 1.
The content of the invention
It is an object of the invention to provide a kind of method for preparing biomass absorbent material under cryogenic conditions using rice husk.It is described
Method avoids the hot environment in biomass absorbent material preparation process, reduces the requirement to production equipment.And convert
Iodine sorption value into the rice husk of Unit Weight is of a relatively high.
The technical scheme is that, a kind of method for preparing biomass absorbent material under cryogenic conditions using rice husk, its
It is characterised by, step is as follows：
(1) biomass rice husk solution is cleaned, drying；
Drying after rice husk it is ground, sieving, in reactor 180 DEG C firing 12h, natural cooling；
(3) the burned product cleaning after coolings, drying, grinding, sieving；
(4) a small amount of ethanol wet of burned product after sievings, and add a certain amount of sulfuric acid solution immersion 12h；
(5) after immersions terminate, liquid evaporating completely is heated to；
(6) cleans remaining solid to sulfate radical-free with deionized water；
(7) then dries, grinds, sieving and to obtain biomass absorbent material.
Above step (1) in cleaning be to be cleaned respectively with aqueous slkali and deionized water；Wherein described aqueous slkali is 1.0M
Sodium hydroxide；
Above step (1) in drying be in an oven 100 DEG C drying；
Above step (2) in sieving be 100 mesh sieve；
Above step (3) in cleaning be to be cleaned respectively with ethanol, hydrochloric acid solution, deionized water；
Above step (3) in concentration of hydrochloric acid solution be 0.1M；
Above step (4) in " a small amount of ethanol " consumption, wetted can be defined by burned product；
Above step (4) in sulfuric acid solution refer to sulfuric acid solution volume fraction point 1%-10% dilute sulfuric acid；
Above step (2) with step (7) in sieving be 100 mesh sieve.
In other words, operating method of the invention is as follows：
Biomass rice husk is collected into Jiangsu Province somewhere, is cleaned respectively with aqueous slkali and deionized water, then in an oven 100
DEG C drying.
By the rice husk after drying is ground, the sieving of 100 mesh, certain mass 180 DEG C of firings in reactor are then weighed
12h, natural cooling.
Burned product after cooling is cleaned with ethanol, hydrochloric acid solution, deionized water respectively, drying, grinding, the sieving of 100 mesh.
By a small amount of ethanol wet of the burned product after sieving, and add a certain amount of sulfuric acid solution immersion 12h.
After immersion terminates, it is put into baking oven 180 DEG C and is heated to liquid evaporating completely.
Remaining solid is cleaned with deionized water to sulfate radical-free.
Dry, grinding, 100 mesh sieve to obtain biomass absorbent material, weigh Mass Calculation biomass absorbent material yield.
GB/T12496.8-2015 is referred to using obtained biomass absorbent material《Iodine sorption value is determined》Carry out titration real
Test, it is 416.232mg/g to draw its iodine sorption value, is converted into the rice husk of unit mass, draw the rice husk iodine absorption of unit mass
Value 280.9566mg.
Titration experiments step is as follows：
0.05g biomass absorbent materials are taken, with two drop ethanol wets, 0.1M KI-I are then added2Solution 50ml, absorption
After 15min, filtering.
Filtrate is taken to use 0.1MNa2S2O3Titration, according to KI-I2And Na2S2O3Reaction is by 1：1 amount is carried out, and is calculated few
The Na of consumption2S2O3Amount, so as to calculate the amount of the elemental iodine of absorption, finally calculate iodine sorption value.
The preparation process of the present invention is similar to traditional preparation process, but technological parameter and detail in preparation process
It is different, it is shown in Table 1.It can be seen that, in terms of slave unit, firing temperature and activation temperature, the present invention has certain advantage.
Table 1
It is an advantage of the invention that preparing biomass absorbent material under cryogenic, the equipment used is a conventional oven, simultaneously
Firing temperature and activation temperature are all significantly lower than conventional method, through according to a preliminary estimate, conventional method more than 50% being less than in terms of cost,
And yield is also greater than conventional method, and the iodine sorption value of biomass carbon raw material is converted into also greater than conventional method.
Brief description of the drawings
Fig. 1 is the process chart for preparing biomass absorbent material.
Embodiment：
Embodiment 1：The method for preparing biomass absorbent material under cryogenic conditions using rice husk, technique is as described in Figure 1.(1) will be
Jiangsu Province somewhere is collected into the rice husk obtained by biomass, sieves and then spend 0.1M hydrochloric acid by grinding, crushing, 100 mesh
Solution cleaning removes the inorganic salts in rice husk, obtains the rice husk powder of preliminary treatment.(2) rice husk powder is dried, grinds it by again
Afterwards, 100 mesh sieves are crossed.(3) is put into the rice husk of gained in reactor, in an oven 180 DEG C of baking 12h, natural cooling.(4) will
Material after cooling, cleaning fluid is washed till with ethanol to colourless, then replace ethanol repeated washing to obtain sorbing material with deionized water.
(5) is dried again, uses a little ethanol wet, and 8h is soaked with the dilute sulfuric acid of volume fraction point 5%.(6) is by the sorbing material after immersion
It is put into baking oven, keeps 180 DEG C of dryings to constant weight.(7) deionized waters are cleaned, and drying and grinding obtains novel biomass sorbing material.
Embodiment 2:Substantially the same manner as Example 1, difference is that the volume fraction of dilute sulfuric acid is 10%.
Embodiment 3：Substantially the same manner as Example 1, difference is that the volume fraction of dilute sulfuric acid is 1%.
Claims (6)
1. the method for biomass absorbent material is prepared under a kind of cryogenic conditions using rice husk, it is characterised in that step is as follows：
(1) biomass rice husk is cleaned, drying；
Drying after rice husk it is ground, sieving, in reactor 180 DEG C firing 12h, natural cooling；
(3) the burned product cleaning after coolings, drying, grinding, sieving；
(4) a small amount of ethanol wet of burned product after sievings, and add a certain amount of sulfuric acid solution immersion 12h；
(5) after immersions terminate, liquid evaporating completely is heated to；
(6) cleans remaining solid to sulfate radical-free with deionized water；
(7) then dries, grinds, sieving and to obtain biomass absorbent material.
2. preparing the method for biomass absorbent material under cryogenic conditions according to claim 1 using rice husk, its feature exists
In, step (1) in cleaning be to be cleaned respectively with aqueous slkali and deionized water；Wherein described aqueous slkali is sodium hydroxide solution,
Concentration is 1.0M.
3. preparing the method for biomass absorbent material under cryogenic conditions according to claim 1 using rice husk, its feature exists
In, step (1) in drying be 100 DEG C of drying in an oven；Step (2) in sieving be 100 mesh sieve.
4. preparing the method for biomass absorbent material under cryogenic conditions according to claim 1 using rice husk, its feature exists
In, step (3) in cleaning be to be cleaned respectively with ethanol, hydrochloric acid solution, deionized water；The concentration of wherein described hydrochloric acid solution is
0.1M。
5. the method for biomass absorbent material is prepared under the cryogenic conditions according to one of claim 1-4 using rice husk, its
Be characterised by, step (4) described in sulfuric acid solution refer to sulfuric acid solution volume fraction point 1%-10% dilute sulfuric acid.
6. the method for biomass absorbent material is prepared under the cryogenic conditions according to one of claim 1-4 using rice husk, its
Be characterised by, step (7) in sieving be 100 mesh sieve.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710084275 | 2017-02-16 | ||
| CN2017100842751 | 2017-02-16 |
Publications (1)
| Publication Number | Publication Date |
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| CN106984283A true CN106984283A (en) | 2017-07-28 |
Family
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| CN201710376148.9A Pending CN106984283A (en) | 2017-02-16 | 2017-05-25 | The method for preparing biomass absorbent material under cryogenic conditions using rice husk |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108362119A (en) * | 2018-03-21 | 2018-08-03 | 南京盛焰新能源有限公司 | A kind of biological particles drying screening integrated apparatus |
| CN117299068A (en) * | 2023-10-08 | 2023-12-29 | 保山学院 | Preparation method of copper-based carbon-silicon material and its application in adsorbing radioactive iodine |
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