CN106492763A - The preparation method and applications of esterification modification bagasse - Google Patents
The preparation method and applications of esterification modification bagasse Download PDFInfo
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- CN106492763A CN106492763A CN201610969728.4A CN201610969728A CN106492763A CN 106492763 A CN106492763 A CN 106492763A CN 201610969728 A CN201610969728 A CN 201610969728A CN 106492763 A CN106492763 A CN 106492763A
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- bagasse
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- esterification
- esterification modification
- citric acid
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- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- 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
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a kind of preparation method of esterification modification bagasse, pretreatment is carried out by ultrasonic assistant alkaline hydrogen peroxide to bagasse and extracts bagasse cellulose, pretreated bagasse is with citric acid with N, N dimethylformamides (DMF) are activator and reaction medium, under conditions of sodium hypophosphite is catalyst, carries out esterification and prepare modified bagasse.The method utilizes the swelling action of the cavitation, alkali of ultrasound wave to lignocellulose, make the structure side of lignocellulose obtain loose, the contact area of increase chemical reagent, and carboxyl can be introduced by esterification modification bagasse, lone pair electrons can be provided, strengthen the absorbability of bagasse heavy metal ion.Test shows that the method improves the ability of bagasse Adsorption of Heavy Metal Ions, can achieve bagasse recycling as adsorbent for heavy metal.
Description
Technical field
The invention belongs to biologic recycling utilizes technical field, more particularly to a kind of preparation method of esterification modification bagasse and
Which is applied.
Background technology
Sugar industry is the pillar industry in Guangxi, and it is 51,910,000 tons to end to the accumulative sugarcane-squeezing amount of the whole district of on April 20th, 2015,
About 11,420,000 tons of the bagasse amount of generation.The main comprehensive Utilization Ways of bagasse have combustion power generation and pulping and paper-making.And it is most of
Bagasse is all used for boiler combustion, causes the waste of biomass energy, is comprehensively utilized as raw material with bagasse, can reduce bagasse
Waste, realize recycling.However, being optimal how the utilization rate of lignocellulose in production, it is still to need to be solved
Problem certainly.
Bagasse is mainly made up of cellulose, lignin, hemicellulose, wherein over dry sugarcane fiber cellulose content be 30%～
45%, hemicellulose is 22%～30%, and lignin is 18%～23%, and these materials all contain the hydroxyl for enriching, and hydroxyl
On oxygen atom lone pair electrons and heavy metal ion can be provided complex reaction occurs, to reach the mesh of heavy-metal ion removal
's.The abundant hydroxyl that bagasse contains, the also property of polyhydric alcohol, can pass through the multiple senses with absorbability of modified introducing
Group.Therefore, bagasse is selected to have for processing effluent containing heavy metal ions for the research that object of study is modified adsorbent
Broad prospect.
At present the method for modifying of lignocellulose mainly has physical modification and a chemical modification, physical modification include electromagnetic wave,
Microwave, ultrasound wave, steam explosion, solvent exchange etc.；Chemical modification includes acid-alkali salt infusion method, esterification modification method, oxidation modification
Method and thiolated modified, halogenation modification method, etherification modified method, grafting copolymerization process etc..
Content of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method and application of esterification modification bagasse, to improve sugarcane
The ability of slag Adsorption of Heavy Metal Ions, can achieve bagasse recycling as adsorbent for heavy metal.
For solving above-mentioned technical problem, the present invention is employed the following technical solutions：
The preparation method of esterification modification bagasse, carries out pretreatment by ultrasonic assistant alkaline hydrogen peroxide and extracts sugarcane to bagasse
Slag cellulose, pretreated bagasse and citric acid are with DMF (DMF) as activator and reaction medium, secondary
Under conditions of sodium phosphite is catalyst, carries out esterification and prepare modified bagasse.
The preparation method of above-mentioned esterification modification bagasse, according to the following steps operation are carried out：
(1) bagasse deionized water is washed away after surface impurity, in drying in oven, then mechanical activation comminution is sieved
Point；
(2) by crushing after bagasse powder add toluene-ethano mixed solution in dewax；
(3) bagasse after washing dewaxing with hydrochloric acid solution, washs to neutrality, after drying；
(4) take dried bagasse and add H2O2With the mixed solution of NaOH, and EDTA and magnesium sulfate is added as H2O2Make
For stabilizer, pretreatment is carried out with ultrasonic washing instrument；
(5) pretreated bagasse, citric acid, sodium hypophosphite are placed in there-necked flask and DMF
Mixing, heats and carries out esterification, is cooled to room temperature, and washing and drying, grinding are sieved and obtain modified bagasse.
Described in step (1), screening uses 80 mesh sub-sieves.
Described in step (2), in toluene-ethano mixed solution, the volume ratio of benzene -ol is 2: 1, and dewaxing temperature is 83 DEG C, takes off
The wax time is 6h.
The mass concentration of hydrochloric acid described in step (3) is 1%.
H described in step (4)2O2With H in the mixed solution of NaOH2O2Mass concentration for 0.7%, NaOH quality dense
Spend for 6%, bagasse and H2O2Solid-to-liquid ratio with the mixed solution of NaOH is 1: 30.
Bagasse described in step (4) is 100: 1 with the mass ratio admittedly of EDTA, and bagasse with the mass ratio admittedly of magnesium sulfate is
500∶1.
The ultrasonic power of ultrasonic washing instrument described in step (4) is 200W, and the ultrasonic pretreatment time is 70min.
Bagasse described in step (5), citric acid, the mass ratio admittedly of sodium hypophosphite are 5: 1: 1, and Citric Acid Dosage is
0.1g～2.5g, the consumption of dimethylformamide is 50mL, and heating-up temperature is 100 DEG C～150 DEG C, and reaction time of esterification is
20min～180min, washing are first to wash away organic solvent with dehydrated alcohol, then use a large amount of distilled water flushings, and sieve used point of sample
Sieve as 60 mesh.
The esterification modification bagasse that above-mentioned preparation method is obtained is used as adsorbent for heavy metal.
The problem that a large amount of bagasses produced for sugar industry are not fully utilized, inventor establish a kind of esterification and change
Property bagasse preparation method, pretreatment is carried out by ultrasonic assistant alkaline hydrogen peroxide to bagasse and extracts bagasse cellulose, pre- located
, with DMF (DMF) as activator and reaction medium, sodium hypophosphite is to urge for bagasse after reason and citric acid
Under conditions of agent, carry out esterification and prepare modified bagasse.The method utilizes the cavitation of ultrasound wave, alkali to lignocellulose
Swelling action, obtain the structure side of lignocellulose loose, increase chemical reagent contact area, and pass through esterification modification sugarcane
Slag can introduce carboxyl, using the teaching of the invention it is possible to provide lone pair electrons, strengthen the absorbability of bagasse heavy metal ion.Test shows, the method
The ability of bagasse Adsorption of Heavy Metal Ions is improve, and bagasse recycling is can achieve as adsorbent for heavy metal.
Compared with prior art, the present invention has advantage following prominent：
1) method of ultrasonic assistant alkaline hydrogen peroxide carries out pretreatment to bagasse powder, and one side ultrasound wave can be produced
Cavitation effect, interrupts intermolecular link, chemical reagent and the contact area on bagasse surface is further increased；On the other hand
NaOH can make the lignin dissolution in bagasse, be extracted cellulose, eliminate the interference of lignin, it is also possible to bagasse be played molten
Swollen effect, makes bagasse structure become more loose, can equally increase the specific surface area of bagasse, more active groups exposed
Outward.
2) hydroxyl contained by lignocellulose makes which possess the property of polyhydric alcohol, is modifying agent to sugarcane with citric acid
Slag is modified, and lignocellulose is reacted with citric acid and introduces carboxyl, improves the absorbability of lignocellulose, from
And improve the absorbability of bagasse.
3) it is catalyst with concentrated sulphuric acid identical sodium hypophosphite to select Catalysis Principles, can not only improve esterification
Speed, and react be easily controlled, the corrosion of equipment and the carbonization of bagasse will not be caused.
4) from the activator and reaction medium that dimethylformamide is esterification, not only can be to bagasse further
Swelling and moistening, and be a kind of good organic solvent, can dissolve each other with water and most of organic solvent, can also dissolve Fructus Citri Limoniae
Acid, it is possible to increase the efficiency of esterification, shortens the response time.
Description of the drawings
Fig. 1 is the process route chart of the preparation method of esterification modification bagasse of the present invention.
Fig. 2 is the flow chart for applying gained esterification modification bagasse Adsorption of Heavy Metal Ions of the present invention.
Specific embodiment
Embodiment 1
(1) bagasse deionized water is washed away after surface impurity, in drying in oven, then mechanical activation comminution uses 80 mesh
Sub-sieve is sieved；
(2) by crushing after bagasse powder add dewaxing, dewaxing temperature in toluene-ethano mixed solution (volume ratio 2: 1)
For 83 DEG C, the dewaxing time is 6h；
(3) bagasse after washing dewaxing with 1% hydrochloric acid solution of mass concentration, removes water soluble polysaccharide, washs to neutrality,
After drying；
(4) it is 1: 30 addition H to take dried bagasse by solid-to-liquid ratio2O2Mixed solution (H with NaOH2O2Mass concentration
For 0.7%, NaOH mass concentration for 6%), and be 100: 1,500: 1 to be separately added into EDTA, magnesium sulfate work by mass ratio admittedly
For H2O2As stabilizer, pretreatment (200W, 70min) is carried out with ultrasonic washing instrument；
(5) pretreated bagasse, citric acid, sodium hypophosphite (admittedly mass ratio is 5: 1: 1,5g bagasses admittedly) are placed in three
Mix with 50mL DMFs in mouth flask, 100 DEG C of heating simultaneously carries out esterification 60min, is cooled to room
Temperature, first washes away organic solvent with dehydrated alcohol, then with a large amount of distilled water flushing post-dryings, grinds, and 60 mesh sieve and obtain modified sugarcane
Slag.
Embodiment 2
Step (1)-(4) are with embodiment 1.
(5) pretreated bagasse, citric acid, sodium hypophosphite (admittedly mass ratio is 5: 1: 1,5g bagasses admittedly) are placed in three
Mix with 50mL DMFs in mouth flask, 120 DEG C of heating simultaneously carries out esterification 60min, is cooled to room
Temperature, first washes away organic solvent with dehydrated alcohol, then with a large amount of distilled water flushing post-dryings, grinds, and 60 mesh sieve and obtain modified sugarcane
Slag.
Embodiment 3
Step (1)-(4) are with embodiment 1.
(5) pretreated bagasse, citric acid, sodium hypophosphite (admittedly mass ratio is 5: 1: 1,5g bagasses admittedly) are placed in three
Mix with 50mL DMFs in mouth flask, 140 DEG C of heating simultaneously carries out esterification 80min, is cooled to room
Temperature, first washes away organic solvent with dehydrated alcohol, then with a large amount of distilled water flushing post-dryings, grinds, and 60 mesh sieve and obtain modified sugarcane
Slag.
Embodiment 4
Step (1)-(4) are with embodiment 1.
(5) pretreated bagasse, citric acid, sodium hypophosphite (admittedly mass ratio is 5: 1: 1,5g bagasses admittedly) are placed in three
Mix with 50mL DMFs in mouth flask, 140 DEG C of heating simultaneously carries out esterification 120min, is cooled to room
Temperature, first washes away organic solvent with dehydrated alcohol, then with a large amount of distilled water flushing post-dryings, grinds, and 60 mesh sieve and obtain modified sugarcane
Slag.
Comparative example
To be crushed after bagasse washing and drying, crossed 60 mesh sieves.
Adsorption test
Bagasse after being processed with embodiment 1-4 gained esterification modification bagasse and comparative example is surveyed according to the following steps as adsorbent
Try its heavy metal adsorption：
Take 0.1g bagasses/esterification modification bagasse and put into 0.5mmol/L Cu2+Heavy metal ion solution in, use constant temperature magnetic
Power agitator carries out adsorption reaction 30min.After the completion of to be adsorbed, take supernatant inductively-coupled plasma spectrometer and determine and inhale
Concentration of heavy metal ion in attached solution, and removal of heavy metal ions rate is calculated according to below equation：
Wherein, R be adsorption rate C ' for copper ion initial concentration, C is heavy metal ion in solution after adsorption treatment
Concentration.As a result such as table 1.
1 bagasse of table/esterification modification bagasse adsorption test result
Claims (10)
1. a kind of preparation method of esterification modification bagasse, it is characterised in that：Bagasse is entered by ultrasonic assistant alkaline hydrogen peroxide
Bagasse cellulose is extracted in row pretreatment, and pretreated bagasse and citric acid are with DMF as activator and instead
Under conditions of answering medium, sodium hypophosphite to be catalyst, carry out esterification and prepare modified bagasse.
2. the preparation method of esterification modification bagasse according to claim 1, it is characterised in that operation is carried out according to the following steps：
(1) bagasse deionized water is washed away after surface impurity, in drying in oven, then mechanical activation comminution is sieved；
(2) by crushing after bagasse powder add toluene-ethano mixed solution in dewax；
(3) bagasse after washing dewaxing with hydrochloric acid solution, washs to neutrality, after drying；
(4) take dried bagasse and add H2O2With the mixed solution of NaOH, and EDTA and magnesium sulfate is added as H2O2As steady
Determine agent, pretreatment is carried out with ultrasonic washing instrument；
(5) pretreated bagasse, citric acid, sodium hypophosphite are placed in there-necked flask and are mixed with DMF
Close, heat and carry out esterification, be cooled to room temperature, washing and drying, grinding are sieved and obtain modified bagasse.
3. the preparation method of esterification modification bagasse according to claim 1, it is characterised in that sieving described in step (1) makes
With 80 mesh sub-sieves.
4. the preparation method of esterification modification bagasse according to claim 1, it is characterised in that toluene described in step (2)-
In alcohol mixed solution, benzene -ol volume ratio is 2: 1, and dewaxing temperature is 83 DEG C, and the dewaxing time is 6h.
5. the preparation method of esterification modification bagasse according to claim 1, it is characterised in that hydrochloric acid described in step (3)
Mass concentration is 1%.
6. the preparation method of esterification modification bagasse according to claim 1, it is characterised in that H described in step (4)2O2With
H in the mixed solution of NaOH2O2Mass concentration be 6% for the mass concentration of 0.7%, NaOH, bagasse and H2O2Mixed with NaOH
The solid-to-liquid ratio for closing solution is 1: 30.
7. the preparation method of esterification modification bagasse according to claim 1, it is characterised in that bagasse described in step (4) with
Admittedly the mass ratio of EDTA is 100: 1, and bagasse is 500: 1 with the mass ratio admittedly of magnesium sulfate.
8. the preparation method of esterification modification bagasse according to claim 1, it is characterised in that ultrasound wave described in step (4)
The ultrasonic power of cleaning device is 200W, and the ultrasonic pretreatment time is 70min.
9. the preparation method of esterification modification bagasse according to claim 1, it is characterised in that bagasse described in step (5),
Citric acid, the admittedly mass ratio of sodium hypophosphite are 5: 1: 1, and Citric Acid Dosage is 0.1g～2.5g, the use of dimethylformamide
Measure as 50mL, heating-up temperature is 100 DEG C～150 DEG C, and reaction time of esterification is 20min～180min, and washing is first to use anhydrous second
Alcohol washes away organic solvent, then uses a large amount of distilled water flushings, and the sub-sieve used that sieves is 60 mesh.
10. the esterification modification bagasse that preparation method described in claim 1 is obtained is used as adsorbent for heavy metal.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107417857A (en) * | 2017-09-15 | 2017-12-01 | 桂林理工大学 | Active anticancer derivative bagasse xylan cloves acid esters g AM/MMA synthetic method |
| CN107497407A (en) * | 2017-10-16 | 2017-12-22 | 云南圣清环保科技有限公司 | A kind of preparation method of biomass new material targeting adsorbent for mercury-containing waste water processing and application |
| CN107540789A (en) * | 2017-09-15 | 2018-01-05 | 桂林理工大学 | Biologically active derivatives bagasse xylan cloves acid esters g AM synthetic method |
| CN107694527A (en) * | 2017-10-16 | 2018-02-16 | 云南圣清环保科技有限公司 | A kind of preparation method of the 2 amino terephthalic acid (TPA) modified celluloses for heavy metals removal |
| CN108993434A (en) * | 2018-09-06 | 2018-12-14 | 潘钕 | A kind of preparation method of bagasse cellulose base weight metal ion adsorbent |
| CN110586042A (en) * | 2019-08-13 | 2019-12-20 | 武汉轻工大学 | Method for treating waste water and method for preparing hexavalent chromium ion adsorbent |
| CN113976059A (en) * | 2021-11-18 | 2022-01-28 | 黄小燕 | Preparation process and equipment of cellulose citrate phthalate |
| CN114276817A (en) * | 2021-12-30 | 2022-04-05 | 北京建工环境修复股份有限公司 | Soil repairing agent and preparation method and application thereof |
| CN115739037A (en) * | 2022-12-29 | 2023-03-07 | 中国科学院过程工程研究所 | High-efficiency removal of Fe in ionic liquid aqueous solution 3+ Modified wood-based adsorbent and preparation method and application thereof |
| CN116120114A (en) * | 2022-12-09 | 2023-05-16 | 杭州楠大环保科技有限公司 | Method for producing novel fertilizer by recycling kitchen garbage |
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| CN107540789A (en) * | 2017-09-15 | 2018-01-05 | 桂林理工大学 | Biologically active derivatives bagasse xylan cloves acid esters g AM synthetic method |
| CN107417857A (en) * | 2017-09-15 | 2017-12-01 | 桂林理工大学 | Active anticancer derivative bagasse xylan cloves acid esters g AM/MMA synthetic method |
| CN107497407A (en) * | 2017-10-16 | 2017-12-22 | 云南圣清环保科技有限公司 | A kind of preparation method of biomass new material targeting adsorbent for mercury-containing waste water processing and application |
| CN107694527A (en) * | 2017-10-16 | 2018-02-16 | 云南圣清环保科技有限公司 | A kind of preparation method of the 2 amino terephthalic acid (TPA) modified celluloses for heavy metals removal |
| CN107694527B (en) * | 2017-10-16 | 2020-06-19 | 云南圣清环保科技有限公司 | Preparation method of 2-amino terephthalic acid modified cellulose for removing heavy metals |
| CN108993434A (en) * | 2018-09-06 | 2018-12-14 | 潘钕 | A kind of preparation method of bagasse cellulose base weight metal ion adsorbent |
| CN110586042A (en) * | 2019-08-13 | 2019-12-20 | 武汉轻工大学 | Method for treating waste water and method for preparing hexavalent chromium ion adsorbent |
| CN110586042B (en) * | 2019-08-13 | 2022-11-25 | 武汉轻工大学 | Method for treating wastewater and method for preparing hexavalent chromium ion adsorbent |
| CN113976059B (en) * | 2021-11-18 | 2024-01-05 | 七星柠檬科技有限公司 | Preparation process and equipment of cellulose citrate phthalate |
| CN113976059A (en) * | 2021-11-18 | 2022-01-28 | 黄小燕 | Preparation process and equipment of cellulose citrate phthalate |
| CN114276817A (en) * | 2021-12-30 | 2022-04-05 | 北京建工环境修复股份有限公司 | Soil repairing agent and preparation method and application thereof |
| CN114276817B (en) * | 2021-12-30 | 2023-12-05 | 北京建工环境修复股份有限公司 | Soil restoration agent and preparation method and application thereof |
| CN116120114A (en) * | 2022-12-09 | 2023-05-16 | 杭州楠大环保科技有限公司 | Method for producing novel fertilizer by recycling kitchen garbage |
| CN116120114B (en) * | 2022-12-09 | 2024-01-12 | 杭州楠大环保科技有限公司 | Method for producing novel fertilizer by recycling kitchen garbage |
| CN115739037A (en) * | 2022-12-29 | 2023-03-07 | 中国科学院过程工程研究所 | High-efficiency removal of Fe in ionic liquid aqueous solution 3+ Modified wood-based adsorbent and preparation method and application thereof |
| CN115739037B (en) * | 2022-12-29 | 2024-01-26 | 中国科学院过程工程研究所 | High-efficiency Fe removal method for ionic liquid aqueous solution 3+ Modified wood-based adsorbent as well as preparation method and application thereof |
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Application publication date: 20170315 |