CN103274390A - Method for increasing yield of biomass-based colloidal carbon - Google Patents
Method for increasing yield of biomass-based colloidal carbon Download PDFInfo
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- CN103274390A CN103274390A CN2013102588418A CN201310258841A CN103274390A CN 103274390 A CN103274390 A CN 103274390A CN 2013102588418 A CN2013102588418 A CN 2013102588418A CN 201310258841 A CN201310258841 A CN 201310258841A CN 103274390 A CN103274390 A CN 103274390A
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Abstract
The invention discloses a method for increasing a yield of biomass-based colloidal carbon, and particularly relates to a method for increasing a yield of colloidal carbon by hydrolyzing a biomass with concentrated acid, condensing and carbonizing a sugar acid solution in situ, and introducing a phenolic compound. The method comprises the following specific steps that the biomass is hydrolyzed by inorganic acid with certain concentration, and filtered to form the sugar acid solution and filter residues; the concentration of the sugar acid solution is adjusted; and colloidal carbon is condensed, carbonized and prepared under the condition that the phenolic compound is added in sugar acid solution dehydration and polymerization processes. The method is simple and easy to realize.
Description
Technical field
The present invention relates to a kind of technology of utilizing different phenolic compounds to influence biomass-based colloid charcoal productive rate.
Background technology
Raising along with the developing rapidly of industry, Increase of population and living standards of the people; energy shortage, environmental pollution etc. have become global problem; searching can replace fossil resource and pursue Sustainable development, protection environment and recycling economy, becomes the important development strategy of many countries.The research that utilizes discarded biomass to produce multi-functional inorganic nano material presents the trend of sustainable growth.Because biological material has advantages such as aboundresources, wide material sources, renewable and biological degradation, has been widely used in synthetic plastics, fiber, functional materials, the prepare composite.Preparing the multifunctional nano carbon material by natural biomass, mainly is by hydrothermal treatment consists (about 200 ℃) preparation colloid charcoal ball.But the productive rate of hydrothermal carbonization and the low problem of scale operation feasibility have limited biomass colloid charcoal Development of Materials.Rice husk and corn cob are two kinds of common biomass, and they all contain a large amount of Mierocrystalline celluloses, hemicellulose and xylogen.Carbon in the biomass is directly changed into the carbon material of functionalization, caused scientific research personnel's very big attention.
Contain a large amount of hemicelluloses, Mierocrystalline cellulose, xylogen etc. in the biomass, under the effect of catalyzer, can change carbohydrate and degraded product thereof into.Mainly adopt protonic acid (sulfuric acid, hydrochloric acid etc.) liquid catalyst at present in the industrial production, they have catalytic effect preferably with molecular conformation generation chemical reaction.Acid hydrolysis has many reports, utilizes sulfuric acid as catalyzer among the patent CN101161666A, to the Mierocrystalline cellulose saccharification that is hydrolyzed.The carbonization that is hydrolyzed obtains monose to corn cob to utilize solid acid among the patent CN102559941A.Utilize the method for acid hydrolysis carbonization among the patent CN102382909A, wastepaper is hydrolyzed, the monose compound that obtains can directly utilize, and also can transform recycling.Disclose a kind of method of dilute acid hydrolysis of cotton stalks among the patent CN101906489A, comprised the pre-treatment step of cotton stalk, the dilute acid hydrolysis step of cotton stalk; This patent also provides a kind of dilute acid hydrolysis of cotton stalks to prepare the method for ethanol.
Be raw material with this renewable resources of biomass, adopt and earlier biomass are carried out acid treatment that its hydrolyzed solution in-situ polycondensation charing of recycling prepares the colloid charcoal, and report has been arranged before.But utilize saccharide compound dehydration polymerization to form to add phenolic compound in the process of colloid charcoal and yet there are no report to improve its productive rate.
Summary of the invention
The object of the invention provides a kind of method that improves biomass-based colloid charcoal productive rate.
The present invention at first with the mineral acid of biomass and 72wt% by solid-to-liquid ratio 1:10(Kg/L) mix, be warming up to 50 ℃, hydrolysis 10 minutes, filter sugar acid solution and filter residue; The acid concentration of adjusting sugar acid solution is 40wt%, is under 95 ℃ in temperature, and the ratio that is respectively 5:1 according to monose/phenols mass ratio mixes, polycondensation and carbonization reaction 6 hours, solid filtering, washing, drying, make the colloid charcoal, realized the raising of biomass-based colloid charcoal productive rate.
The invention is characterized in: described production colloid charcoal biomass be rice husk, corn cob, etc. agricultural wastes and wood sugar, fructose, glucose etc.
The invention is characterized in: the phenolic compound that adds is phenol, Resorcinol, Phloroglucinol.
The invention is characterized in: described mineral acid is sulfuric acid.
The invention is characterized in: add phenolic compound to improve the productive rate of colloid charcoal in the process of saccharide compound dehydration polymerization formation colloid charcoal.
Embodiment
Embodiment 1:
(1) with rice husk and 72% H
2SO
4Be 1:10(Kg/L by solid-to-liquid ratio) mix, place 50 ℃ of water-bath hydrolysis 10 minutes, regulating acid concentration is 40%, filters to obtain sugar acid solution;
(2) sugar acid solution was placed 95 ℃ of water-bath carbonization reaction 6 hours, filtration, washing, drying, the colloid charcoal (be that the ratio of 5:1 is mixed with single phenol in rice husk/phenol mass ratio with sugar acid solution, placed 95 ℃ of water-bath carbonization reaction 6 hours, filtration, wash, 120
oDry under the C, get the colloid charcoal).
(3) productive rate that does not add the colloid charcoal of phenol is 6.82%, and the productive rate that adds the colloid charcoal of phenol is 17.35%,
The productive rate of colloid charcoal has improved 10.53%.
Embodiment 2:
Changing phenol is Resorcinol, and other condition such as embodiment 1, productive rate are 19.8%, and the productive rate of colloid charcoal has improved 12.98%.
Embodiment 3:
Changing phenol is Phloroglucinol, and other conditions such as embodiment 1, productive rate are 18.3%, and the productive rate of colloid charcoal has improved 11.48%.
Embodiment 4:
Changing rice husk is corn cob, and other conditions such as embodiment 1, productive rate are 13.2%.
Embodiment 5:
Changing rice husk is corn cob, other condition such as embodiment 1, and the productive rate that adds phenol is 27.9%, the productive rate of colloid charcoal has improved 14.7%.
Embodiment 6:
Changing phenol is Resorcinol, and other condition such as embodiment 1, productive rate are 41%, and the productive rate of colloid charcoal has improved 27.8%.
Embodiment 7:
Changing phenol is Phloroglucinol, and other condition such as embodiment 1, productive rate are 37.85%, and the productive rate of colloid charcoal has improved 24.65%.
Embodiment 8:
With wood sugar, fructose, glucose is 1:10(Kg/L with 40% sulfuric acid by solid-to-liquid ratio) mix, at 95 ℃ of reaction 6h down, obtain the colloid charcoal, the productive rate of colloid charcoal is 49.4%, 5.25%, 4.8%.
Embodiment 9:
With wood sugar and phenol (Resorcinol, Phloroglucinol) by mass ratio is the mixed of 5:1, be 1:10(Kg/L with 40% sulfuric acid by solid-to-liquid ratio again) mix, react 6h down at 95 ℃, obtain the colloid charcoal, the productive rate of colloid charcoal is 59.25%, 63.75%, 60.25%, and the productive rate of colloid charcoal has improved 9.85%, 14.55,10.85% respectively.
Embodiment 10:
Changing wood sugar is fructose, and other condition such as embodiment 9, the productive rate of colloid charcoal are 18.0%, 35.96%, 34.33%.The productive rate of colloid charcoal has improved 12.75%, 30.71%, 29.08% respectively.
Embodiment 11:
Changing wood sugar is glucose, and other condition such as embodiment 9, the productive rate of colloid charcoal are 22.38%, 37.75%, 35.5%, and the productive rate of colloid charcoal has improved 17.58%, 32.95%, 30.7%.
Claims (3)
1. production method that improves biomass-based colloid charcoal productive rate, its concrete steps as
Down: at first with the mineral acid of biomass and 72wt% by solid-to-liquid ratio 1:10(Kg/L) mix, be warming up to 50 ℃, hydrolysis 10 minutes, filter sugar acid solution and filter residue; Adjust the acid concentration 40t% of sugar acid solution, adding phenolic compound (phenol, Resorcinol, Phloroglucinol) mass ratio is 5:1, is 95 ℃ of following polycondensation and carbonization reaction 6 hours in temperature, filters washing, drying, preparation colloid charcoal.
2. an a kind of method that improves biomass-based colloid charcoal productive rate as claimed in claim 1 is characterized in that: the biomass of described production colloid charcoal are: rice husk, corn cob, wood sugar, fructose, glucose.
3. a kind of method that improves biomass-based colloid charcoal productive rate as claimed in claim 1, it is characterized in that: phenolic compound is: phenol, Resorcinol, Phloroglucinol.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113880069A (en) * | 2021-10-12 | 2022-01-04 | 国际竹藤中心 | Preparation method for efficiently synthesizing micron-sized bamboo cellulose-based carbon microspheres |
Citations (4)
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|---|---|---|---|---|
| US3331783A (en) * | 1964-04-02 | 1967-07-18 | Grace W R & Co | Microspheres containing colloidal carbon |
| CN101811692A (en) * | 2010-05-05 | 2010-08-25 | 吉林大学 | New method for comprehensive utilization of straw resource |
| CN101948106A (en) * | 2010-09-28 | 2011-01-19 | 华东理工大学 | Preparation method of blocky porous carbon with high specific surface area |
| US20110059006A1 (en) * | 2005-04-13 | 2011-03-10 | Continental Carbon Company | Methods for Production of Carbon Nanomaterials in the Presence of a Carbon Black Catalyst |
-
2013
- 2013-06-26 CN CN2013102588418A patent/CN103274390A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3331783A (en) * | 1964-04-02 | 1967-07-18 | Grace W R & Co | Microspheres containing colloidal carbon |
| US20110059006A1 (en) * | 2005-04-13 | 2011-03-10 | Continental Carbon Company | Methods for Production of Carbon Nanomaterials in the Presence of a Carbon Black Catalyst |
| CN101811692A (en) * | 2010-05-05 | 2010-08-25 | 吉林大学 | New method for comprehensive utilization of straw resource |
| CN101948106A (en) * | 2010-09-28 | 2011-01-19 | 华东理工大学 | Preparation method of blocky porous carbon with high specific surface area |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113880069A (en) * | 2021-10-12 | 2022-01-04 | 国际竹藤中心 | Preparation method for efficiently synthesizing micron-sized bamboo cellulose-based carbon microspheres |
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Application publication date: 20130904 |