CN104213447A - Bagasse preprocessing method for activating surface groups - Google Patents
Bagasse preprocessing method for activating surface groups Download PDFInfo
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Abstract
The invention discloses a bagasse preprocessing method for activating surface groups. An unique process of immersion by acetic acid, cracking by steam, oxidation by alkali and hydrogen peroxide, bleaching, activating by acetic acid and surface activating is used for preprocessing bagasse fibers, and the surface structure of the bagasse fiber can be greatly improved, so that bagasse is easy to graft and modify so as to prepare various functional materials. By adopting the method, the structure of lignocellulose with components being intertwined with each other can be damaged, the surface of the bagasse fibers can be effectively improved, the surface groups of the bagasse can be activated, and the bagasse is easier to functionally modify.
Description
Technical field
The present invention relates to a kind of biological material pre-treatment field, particularly a kind of bagasse preprocess method of activating surface group.
Background technology
China is third place in the world cane planting big country, produce about 2,000 ten thousand tons sugarcane fibres per year, this is a large number of concentrating very much and a fairly large number of resource, its tradition utilizes field to be sugar refinery itself as fuel directly to burn heat production and the raw material as pulp and paper industry, the economic worth of this Application way is very low, also causes the pollution to ecological environment.On the other hand, substituting fossil resource by living beings such as bagasse is national strategy Journal of Sex Research direction.There is object trans-utilization by the main components cellulose of sugarcane fibre, hemicellulose and lignin, new material significant in modern society and economic life, industrial chemicals, exotic fuels, functional food and medicine can be obtained.
Develop sugarcane fibre resource, not only can improve the economic benefit in sugar refinery, also can be the resource that other industry provides a large amount of, many industries are all significant.But sugarcane fibre structure is very complicated, comprise cellulose, hemicellulose, lignin, wax, inorganic salts, starch, pectic substance, the compositions such as sugar, wherein in three large components, cellulose is 32% ~ 48%, hemicellulose 19% ~ 24%, lignin 23% ~ 32%, and these three kinds of components are wound around mutually, the structure of similar armored concrete, be difficult to be separated completely, in order to make full use of the active ingredient in sugarcane fiber, the hydroxyl activity of bagasse point should be made to have degree of displaying fully as far as possible, therefore bagasse cellulose is carried out to follow-up function and high-valued before must carry out preliminary treatment to bagasse cellulose, object is to increase cellulosic accessibility, thus improve the reaction speed of cellulose in various chemical reaction, the extent of reaction and reaction homogeneity.
Although cellulose preprocess method is a lot, all there is certain drawback, Physical environmental pollution is less, but energy consumption is excessive; In chemical method, independent soda acid process can only remove hemicellulose, and purity is not high, if higher and easily produce environmental pollution without recycling and reusing cost, the cost of lime is lower, but the amount of lime needed is comparatively large, easily produces deposition.Steam explosion and biological treatment are the pretreated developing direction of lignocellulose from now on.
Desirable preconditioning technique should meet following necessary condition: be 1. conducive to the structure destroying bagasse three components reinforced concrete formula, breaks hemicellulose and lignin to cellulosic parcel, improves the purity of bagasse cellulose; 2. be conducive to increasing the specific area of bagasse cellulose and avtive spot displaying degree, be beneficial to follow-uply carry out functionalization to it; 3. chemicals should be reclaimed as far as possible or be reused, to reduce the pollution to environment; 4. economically feasible, reduces the cost of preliminary treatment itself as much as possible.Can make great efforts from the following aspect: the preprocess method 1. selecting the low-corrosiveness such as diluted acid diluted alkaline, reduce the cost of preliminary treatment device therefor material; 2. the preprocess method selected avoids the front Mechanical Crushing to lignocellulose of preliminary treatment as far as possible, because the observable index of Mechanical Crushing is higher; 3. gentle steam blasting preconditioning technique is selected to increase specific area and the accessibility of lignocellulose; 4. chemicals used cheaply and can reuse or recycle, should not produce harmful residue; 5. the least possible water is answered in preliminary treatment, selects suitable liquid-solid ratio.
Summary of the invention
The object of the present invention is to provide a kind of bagasse preprocess method of integrated activating surface group, the method makes full use of the advantage of the various preprocess methods such as acid soak, steam blasting, the process of alkaline oxygen base, surface activation process, while the cellulosic accessibility of increase and avtive spot displaying degree, by recycling medicine, reach pollution abatement, reduce water consumption, reduce the object of energy consumption.
The invention provides the bagasse preprocess method of above-mentioned activating surface group, comprise the steps.
(1) acetic acid soaks bagasse:
Be immersed in by bagasse in acetic acid solution, acetic acid solution concentration is 0.1%-3%v/v, and the volume/weight ratio of acetic acid and bagasse solution is 10-15ml/g, and soak time is 6-24h, is filtered dry after immersion;
(2) Steam explosion treatment:
Above-mentioned bagasse is carried out Steam explosion treatment in steam blasting device, and steam pressure is 1.2-3.2MPa, and maintenance pressure time is 2-8min;
(3) alkali/hydrogen peroxide oxidation process:
The bagasse that step (2) obtains is added in NaOH solution, the concentration of NaOH is 15-50g/L, wherein the volume/weight ratio of NaOH solution and bagasse is 10-15ml/g, then hydrogen peroxide is added, the interpolation of hydrogen peroxide divides and completes for three times, added 1/3rd of the total addition of hydrogen peroxide every one hour, the total addition level of hydrogen peroxide is the 0.7%-4%v/v of NaOH solution volume; Treatment temperature: 30-90 DEG C, total processing time is 3-5h.Be filtered dry after processing, the alkali lye obtained by adding hydrogen peroxide post processing next group bagasse, thus reuses;
(4) bleaching:
Added in certain density bleaching agent solution by the product that step (3) obtains and carry out bleaching, described bleaching agent is hydrogen peroxide, and concentration is 1%-3%v/v, treatment temperature: 60-90 DEG C, processing time 1-3h, after being disposed, and washing, suction filtration;
(5) acetic acid activation:
The product that step (4) obtains is added the acetic acid solution of 0.1%-3%, stir 20min-2h, washing, suction filtration.
(6) surface activation process:
The product that step (4) obtains is added in solution medium and carries out surface activation process, as long as liquor capacity energy submergence bagasse cellulose completely, adopt ultrasonic activation, solution medium is ethanol, methyl alcohol or acetone, ultrasonic treatment temperature is 20-80 DEG C, processing time is 5 ~ 120min, processes rear suction filtration, dries and get final product.
In the claims in the present invention and description unless otherwise specified, otherwise all percentage is percent by volume.
It is little that the preprocess method that the present invention obtains to be provided has pollution, and pretreated bagasse cellulose purity is high, the feature that displaying degree in surface-activity site is high, has the following advantages compared with existing bagasse preprocess method:
(1) steam explosion treatment is carried out again after being soaked by acetic acid, cellulosic accessibility and avtive spot displaying degree can be increased greatly, thus provide great facility for the utilization of follow-up bagasse cellulose, as, improve the ethanol production utilizing lignocellulose direct fermentation to produce alcohol, promote the treatment effect that sugarcane fiber material is follow-up.
(2) on the basis of steam blasting, adopting alkali/hydrogen peroxide oxidation process can improve the purity of bagasse cellulose, can reuse alkali lye by adding hydrogen peroxide, thus reduce medicine use amount and water consumption, pollution abatement, reduce energy consumption.
(3) bleaching can improve the purity of bagasse cellulose further, for the utilization in some field is provided convenience.As the application in cellulose aquagel medical dressing field needs purer cellulose.
(4) acetic acid can activate the group on sugarcane fiber surface, it is made to be easier to graft modification, surface activation process effectively avoids subsiding of follow-up constant pressure and dry central hole structure, can prevent pretreated bagasse from luming, ultrasonic wave effectively improves the specific area of bagasse cellulose, improves pore structure, can increase cellulosic accessibility and avtive spot displaying degree further simultaneously, for the modification of follow-up bagasse cellulose is laid a solid foundation, improve the percent grafting of functional group.
Figure of description:
Fig. 1 is through pretreated Electronic Speculum figure.
The pretreated technological process of Fig. 2 bagasse:
Detailed description of the invention:
Below in conjunction with embodiment, the present invention will be described in detail.It should be noted that embodiment is only as further illustrating invention, instead of as limitation of the present invention.
Embodiment 1
Get the bagasse that sugar refinery is packed, carry out preliminary treatment according to following steps: (1) takes 50g bagasse, add 0.3% acetic acid solution 750ml, soak 12h, be filtered dry; (2) Steam explosion treatment: above-mentioned bagasse is added steam blasting container, setting steam pressure 1.9MPa, release after dimension pressure 5min, takes out bagasse; (3) alkali/hydrogen peroxide oxidation process: take 22.5g NaOH and be dissolved in the aqueous solution that 750ml water is mixed with NaOH, above-mentioned bagasse is added, stir 4 hours at 80 DEG C, reaction initial in reaction respectively adds the hydrogen peroxide that 17ml concentration is 30% in one hour and two hours, is filtered dry; (4) bleaching: added in 700ml water by 50ml30% hydrogen peroxide and prepare hydrogen peroxide solution, added by the bagasse of previous step process, stirs 3 hours at 70 DEG C, and washing, is filtered dry; (5) add the acetic acid solution of 0.5%, stir 20min, washing, suction filtration.(6) surface activation process: add acetone and soak after 1h, at 30 DEG C of ultrasonic 30min, suction filtration, dries and get final product.
After testing, in untreated bagasse raw material, the relative amount of cellulose, hemicellulose and lignin is respectively 45.17%, 22.64% and 23.58%, after preliminary treatment of the present invention, in bagasse material, the relative amount of cellulose, hemicellulose and lignin is respectively 93.17%, 4.25% and 0.78%.
Getting the bagasse cellulose of the present embodiment before and after surface activation process and carry out graft acrylamide, measuring the percent grafting before and after surface activation process, for evaluating the effect of surface activation process.The condition of graft acrylamide is as follows: get 40g acrylamide and be dissolved in 400ml deionized water, add 30g bagasse cellulose, dispersed with stirring, add 2.4g ammonium ceric nitrate, 45 DEG C reaction 2h, suction filtration, washing, with 50 DEG C of vacuumizes to constant weight, weigh, be calculated as follows percent grafting:
In formula: W
gfor quality (g) after bagasse cellulose graft acrylamide; W
0for quality (g) before bagasse cellulose grafting.
As calculated, the percent grafting of the bagasse cellulose graft acrylamide before surface activation process is 31.25%, and the percent grafting of bagasse cellulose graft acrylamide after surface activation process is 87.38%.From then on result can find out that the inventive method can improve the purity of bagasse cellulose, increases accessibility and the avtive spot displaying degree of bagasse cellulose, improves the percent grafting of functional group in follow-up bagasse material functional, thus promote the performance of material each side.
Embodiment 2
Get the bagasse that sugar refinery is packed, carry out preliminary treatment according to following steps: (1) takes 50g bagasse, add 1% acetic acid solution 600ml, soak 12h, be filtered dry; (2) Steam explosion treatment: above-mentioned bagasse is added steam blasting container, setting steam pressure 1.3MPa, release after dimension pressure 8min, takes out bagasse; (3) alkali/hydrogen peroxide oxidation process: take 24.0g NaOH and be dissolved in the aqueous solution that 600ml water is mixed with NaOH, above-mentioned bagasse is added, stir 3 hours at 90 DEG C, reaction initial in reaction respectively adds the hydrogen peroxide that 20ml concentration is 30% in one hour and two hours, is filtered dry; (4) bleaching: by 18ml acetic acid and 5.7gNaClO
2add in 582ml water and prepare mixed bleach solution, added by the bagasse of previous step process, stir 1 hour at 85 DEG C, washing, is filtered dry; (5) add the acetic acid solution of 1%, stir 40min, washing, suction filtration.(6) surface activation process: after adding alcohol immersion 1h, at 20 DEG C of ultrasonic 60min, suction filtration, dries and get final product.
After testing, in untreated bagasse raw material, the relative amount of cellulose, hemicellulose and lignin is respectively 45.17%, 22.64% and 23.58%, after preliminary treatment of the present invention, in bagasse material, the relative amount of cellulose, hemicellulose and lignin is respectively 91.70%, 5.87% and 0.64%
Getting the bagasse cellulose of the present embodiment before and after surface activation process and carry out graft acrylamide, measuring the percent grafting before and after surface activation process, for evaluating the effect of surface activation process.The condition of graft acrylamide is as follows: get 40g acrylamide and be dissolved in 400ml deionized water, add 30g bagasse cellulose, dispersed with stirring, add 2.4g ammonium ceric nitrate, 45 DEG C reaction 2h, suction filtration, washing, with 50 DEG C of vacuumizes to constant weight, weigh, calculate percent grafting
As calculated, the percent grafting of the bagasse cellulose graft acrylamide before surface activation process is 28.97%, and the percent grafting of bagasse cellulose graft acrylamide after surface activation process is 113.82%.From then on result can find out that the inventive method can improve the purity of bagasse cellulose, increases accessibility and the avtive spot displaying degree of bagasse cellulose, improves the percent grafting of functional group in follow-up bagasse material functional, thus promote the performance of material each side.
Embodiment 3
Get the bagasse that sugar refinery is packed, carry out preliminary treatment according to following steps: (1) takes 50g bagasse, add 3% acetic acid solution 700ml, soak 6h, be filtered dry; (2) Steam explosion treatment: above-mentioned bagasse is added steam blasting container, setting steam pressure 2.8MPa, release after dimension pressure 2min, takes out bagasse; (3) alkali/hydrogen peroxide oxidation process: take 10.5g NaOH and be dissolved in the aqueous solution that 700ml water is mixed with NaOH, above-mentioned bagasse is added, stir 5 hours at 70 DEG C, reaction initial in reaction respectively adds the hydrogen peroxide that 31ml concentration is 30% in one hour and two hours, is filtered dry; (4) bleaching: added in 700ml water by 60ml30% hydrogen peroxide and prepare hydrogen peroxide solution, added by previous step bagasse, stirs 2 hours at 80 DEG C, and washing, is filtered dry; (5) add the acetic acid solution of 2.5%, stir 1h, washing, suction filtration.(6) surface activation process: add methyl alcohol and soak after 2h, at 60 DEG C of ultrasonic 20min, suction filtration, dries and get final product.
After testing, in untreated bagasse raw material, the relative amount of cellulose, hemicellulose and lignin is respectively 45.17%, 22.64% and 23.58%, after preliminary treatment of the present invention, in bagasse material, the relative amount of cellulose, hemicellulose and lignin is respectively 94.05%, 4.12% and 0.59%
Getting the bagasse cellulose of the present embodiment before and after surface activation process and carry out graft acrylamide, measuring the percent grafting before and after surface activation process, for evaluating the effect of surface activation process.The condition of graft acrylamide is as follows: get 40g acrylamide and be dissolved in 400ml deionized water, add 30g bagasse cellulose, dispersed with stirring, add 2.4g ammonium ceric nitrate, 45 DEG C reaction 2h, suction filtration, washing, with 50 DEG C of vacuumizes to constant weight, weigh, calculate percent grafting
As calculated, the percent grafting of the bagasse cellulose graft acrylamide before surface activation process is 35.46%, and the percent grafting of bagasse cellulose graft acrylamide after surface activation process is 95.31%.From then on result can find out that the inventive method can improve the purity of bagasse cellulose, increases accessibility and the avtive spot displaying degree of bagasse cellulose, improves the percent grafting of functional group in follow-up bagasse material functional, thus promote the performance of material each side.
Claims (1)
1. a bagasse preprocess method for activating surface group, is characterized in that comprising the following steps:
(1) acetic acid soaks bagasse:
Be immersed in by bagasse in acetic acid solution, acetic acid solution concentration is 0.1%-3%v/v, and the volume/weight ratio of acetic acid and bagasse solution is 10-15ml/g, and soak time is about 6-24h, is filtered dry after immersion;
(2) Steam explosion treatment:
Above-mentioned bagasse is carried out Steam explosion treatment in steam blasting device, and steam pressure is 1.2-3.2MPa, and maintenance pressure time is 2-8min;
(3) alkali/hydrogen peroxide oxidation process:
The bagasse that step (2) obtains is added in NaOH solution, the concentration of NaOH is 15-50g/L, wherein the volume/weight ratio of NaOH solution and bagasse is 10-15ml/g, then hydrogen peroxide is added, the interpolation of hydrogen peroxide divides and completes for three times, added 1/3rd of the total addition of hydrogen peroxide every one hour, the total addition level of hydrogen peroxide is the 0.7%-4%v/v of NaOH solution volume; Treatment temperature: 30-90 DEG C, total processing time is 3-5h.Be filtered dry after processing, the alkali lye obtained by adding hydrogen peroxide post processing next group bagasse, thus reuses;
(4) bleaching:
Added in certain density bleaching agent solution by the product that step (3) obtains and carry out bleaching, described bleaching agent is hydrogen peroxide, and concentration is 1%-3%v/v; Treatment temperature: 60-90 DEG C, processing time 1-3h, after being disposed, washing, suction filtration;
(5) acetic acid activation:
The product that step (4) obtains is added the acetic acid solution of 0.1%-3%, stir 20min-2h, washing, suction filtration.
(6) surface activation process:
The product that step (5) obtains is added in solution medium and carries out surface activation process, as long as liquor capacity energy submergence bagasse cellulose completely, adopt ultrasonic activation, solution medium is ethanol, methyl alcohol or acetone, ultrasonic treatment temperature is 20-80 DEG C, processing time is 5 ~ 120min, processes rear suction filtration, dries and get final product.
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| CN107183781A (en) * | 2017-06-17 | 2017-09-22 | 常州环际商贸有限公司 | A kind of preparation method of reconstituted tobacco |
| CN114319919A (en) * | 2021-12-24 | 2022-04-12 | 广东定源建设工程有限公司 | Reinforcing method for building energy-saving floor slab |
| WO2024078396A1 (en) * | 2022-10-10 | 2024-04-18 | 晋江安润纺织有限公司 | Method for preparing yarn from sugarcane |
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| CN107183781A (en) * | 2017-06-17 | 2017-09-22 | 常州环际商贸有限公司 | A kind of preparation method of reconstituted tobacco |
| CN114319919A (en) * | 2021-12-24 | 2022-04-12 | 广东定源建设工程有限公司 | Reinforcing method for building energy-saving floor slab |
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Address after: 510316 Guangzhou sugar cane sugar Research Institute, Haizhuqu District, Guangdong, China, No. 10, Patentee after: Guangdong Province Institute of Biological Engineering (Guangzhou Sugarcane Industry Research Institute) Address before: 510316 Guangzhou sugar cane sugar Research Institute, Haizhuqu District, Guangdong, China, No. 10, Patentee before: Guangzhou Sugarcane Industry Research Institute |
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