CN102911274A - Method for chemically preparing nano microcrystalline cellulose by utilizing moso bamboo - Google Patents
Method for chemically preparing nano microcrystalline cellulose by utilizing moso bamboo Download PDFInfo
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Abstract
The invention discloses a method for chemically preparing nano microcrystalline cellulose by utilizing moso bamboo. The adopted method has key points that the moso bamboo is respectively subjected to alkali solution treatment and chlorine-containing solution treatment to purify cellulose, moso bamboo fibers are catalyzed and hydrolyzed by adopting an organic acid and a moso bamboo nano microcrystalline cellulose product is collected by virtue of an ultrafiltration membrane. The method disclosed by the invention is rapid and efficient and is especially applicable to preparation of nano microcrystalline cellulose by adopting the moso bamboo raw material. According to the method disclosed by the invention, a moso bamboo resource is introduced into a fiber raw material used for preparing the nano microcrystalline cellulose, the range of the raw material used for preparing the nano microcrystalline cellulose is expanded, rapid break-through of limitation of source of the raw material of the nano microcrystalline cellulose can be facilitated, and an innovative thinking is provided for high-valued utilization of the moso bamboo resource, so that economic income of peasant in bamboo regions in China can be reliably increased, and the method disclosed by the invention has practical significance.
Description
Technical field
The present invention relates to a kind of method for preparing nano micro crystal cellulose, particularly a kind of method of utilizing mao bamboon chemical preparation nano micro crystal cellulose belongs to the Pulp and Paper Engineering field.
Background technology
Mierocrystalline cellulose is the abundantest natural high moleculer eompound of content on the earth, is formed by connecting by β-Isosorbide-5-Nitrae-glycosidic link chain by single D-Glucose unit.Nano micro crystal cellulose is the levelling-off DP solid product with nanoscale and excellent performance that is obtained through glass-ceramic process by natural cellulose.Nano micro crystal cellulose not only has basic structure and the performance of general fibre element, the characteristic that also possesses nano particle, such as huge specific surface area, higher Young's modulus, superpower adsorptive power and sensitive reactive behavior, there are larger difference in its character and general fibre element.Nano micro crystal cellulose has more reactive group than general fibre element, and chemical reactivity is large, can be used for efficient cellulose chemistry modification.
Yet at present, the limitation of raw materials almost becomes " bottleneck " that obstruction nano micro crystal cellulose commercially produced product is come out of the stove.The natural matter that present stage prepares the nano micro crystal cellulose employing is mainly linters, wood pulp and tunicin.There is comparatively small amt in tunicin, extracts the problems such as inconvenient; Linters can be used as the high-quality fibrous material of preparation nano micro crystal cellulose because its content of cellulose can reach more than 90%, but has raw material supplying and the problem such as expensive; Wood raw material can be used for the preparation of nano micro crystal cellulose, but the growth cycle of lignocellulose raw material is relatively long through after the special processing treatment.In the nano micro crystal cellulose preparation field, Chinese patent (ZL 00117261.1) " a kind of nano micro crystal cellulose and method for making " is take linters as raw material, the mixture of one or more in employing sulfuric acid, hydrochloric acid, phosphoric acid and the nitric acid, perhaps adopt in vinylformic acid, phenylformic acid, the oxalic acid mixture of one or more, perhaps adopt solid acid hydrolysis to prepare nano micro crystal cellulose, and its pattern and crystal formation are characterized; Chinese patent (ZL 01107523.6) " a kind of nano micro crystal cellulose and method for making with cellulose Ⅱ crystal formation " is take linters as raw material, adopt simultaneously swelling of DMSO and highly basic, mineral acid, organic acid or solid peracid hydrolysis have prepared nano micro crystal cellulose, and have described its pattern and crystalline structure; Chinese patent (ZL200510100343.6) " method for preparing nano micro crystal cellulose with chlorine oxidation degradation " adopts chlorine oxidation degradation to prepare the pure white spherical nano micro crystal cellulose of color and luster take sisal fibers or lumber fibre as raw material; It is raw material that United States Patent (USP) (US20100124651A1) " Method of manufacturing nano-crystalline cellulose film " adopts the lumber fibre nano micro crystal cellulose, with organic compound with inorganic materials, prepare the high-strength nano composite material film, significantly improved the physicals of former film; United States Patent (USP) (US 008105430B2) " Aircraft anti-icing fluids formulated withnanocrystalline cellulose " with the nano micro crystal cellulose in lumber fibre source as thickening material, be mixed with the chemical machine auxiliary agent, prepare the anti-icing compositions of aircraft, be used for promoting the freezing performance that prevents of aircraft skin.So far, yet there are no and utilize mao bamboon as the Mierocrystalline cellulose thing of originating, occur in order to the related process technology for preparing nano micro crystal cellulose.
Mao bamboon is the most important Economic Bamboo kind of China, and about 3,400,000 hectares of cultivated area accounts for 68% of national bamboo grove area, and the mao bamboon bamboo grove area of Zhejiang, Fujian, Jiangxi San Sheng accounts for the over half of the whole nation, is China mao bamboon emphasis producing region.Mao bamboon has become the important sources of China's bamboo district peasant economy income.Mao bamboon belongs to rank vegetation resource, has fast growth, short, a fibre content advantages of higher of the cycle of becoming a useful person, and its fibre shape and fibrocyte content approach even is higher than general leaf wood.How to take full advantage of the bamboo resource of China's abundant, preparation high added value renewable nanometer novel material becomes practical raisings China bamboo district peasant economy and takes in, and opens one's minds for one of while higher value application bamboo resource, meet the national development circular economy policy, therefore have important practical significance.
Summary of the invention
For the fibrous material undersupply that overcomes present preparation nano micro crystal cellulose, expensive, the problem such as growth cycle is long, the bamboo resource of while recycling China's abundant, with the renewable nanometer novel material of preparation high added value, the purpose of this invention is to provide a kind of method of utilizing mao bamboon chemical preparation nano micro crystal cellulose.
For achieving the above object, technical scheme of the present invention is to adopt following steps:
1) with mao bamboon defoliation, clean, dry, adopt the plant pulverizer to pulverize, filter through 100 eye mesh screens, obtain particle diameter less than or equal to the mao bamboon powder of 0.15mm;
2) with the mao bamboon powder that obtains in the step 1) under mechanical agitation, in 70 ~ 90 ℃ of basic solutions, react 90 ~ 120min, repeat 3 times, clean residual alkali with distilled water therebetween, obtain the mao bamboon fiber;
3) adopt contain chlorine solution under mechanical agitation, 60 ~ 80 ℃ of bleaching steps 2) in mao bamboon fiber 150 ~ 210min of obtaining, repeats 4 times, clean residual chlorine with distilled water therebetween, acquisition high purity mao bamboon fiber;
4) with the high purity mao bamboon fiber that obtains in the step 3) under mechanical agitation, place 40 ~ 60 ℃ of organic acid solns to react 120 ~ 180min, adopt the room temperature distilled water termination reaction of 5 times of above-mentioned organic acid soln volumes, clean residual acid, obtain mao bamboon nano micro crystal cellulose suspension;
5) with the mao bamboon nano micro crystal cellulose suspension centrifugation 8 ~ 15min under 10000rpm that obtains in the step 4), remove the above solid particulate of 1 μ m, take out centrifugate through ultrafiltration membrance filter, collect the solid ingredient that face is held back with distilled water, finally obtain the mao bamboon nano micro crystal cellulose.
Described basic solution is Mg (OH)
2Solution, massfraction are 4.0 ~ 6.0wt%, mao bamboon powder and Mg (OH)
2The mass ratio of solution is 1:5 ~ 10; Containing chlorine solution is Ca (ClO)
2Solution, massfraction are 1.5 ~ 3.0wt%, mao bamboon fiber and Ca (ClO)
2The mass ratio of solution is 1:10 ~ 20; Organic acid soln is the mixing acid of one or several the different proportionings in Phenylsulfonic acid, citric acid, trichoroacetic acid(TCA), the trifluoro sulphur formic acid, and massfraction is 30 ~ 50wt%, and the mass ratio of mao bamboon fiber and organic acid soln is 1:10 ~ 20.
Described ultra-filtration membrane is a kind of in poly (ether sulfone) film, PVDF membrane, the regenerated cellulose film, and its molecular weight cut-off is 50 ~ 100kDa.
Compare with background technology, the beneficial effect that the present invention has is:
The present invention introduces bamboo resource in the fibrous material of preparation nano micro crystal cellulose, expanded the raw material range of preparation nano micro crystal cellulose, be conducive to accelerate break through the raw material sources limitation of nano micro crystal cellulose, realize that early the nano micro crystal cellulose commercially produced product comes out of the stove; Open one's minds for one that proposes simultaneously the higher value application bamboo resource, meet the national development circular economy policy, can conscientiously improve China bamboo district peasant's income.
Description of drawings
This accompanying drawing is the field emission scanning electron microscope photo of the mao bamboon nano micro crystal cellulose product for preparing of the present invention.
Wherein Fig. 1 is that the mao bamboon nano micro crystal cellulose amplifies 10,000 times photo.
Fig. 2 is that the mao bamboon nano micro crystal cellulose amplifies 50,000 times photo.
Embodiment
The invention will be further described below in conjunction with specific embodiment.
Embodiment 1:
1) with mao bamboon defoliation, clean, dry, adopt the plant pulverizer to pulverize, filter through 100 eye mesh screens, obtain particle diameter less than or equal to the mao bamboon powder of 0.15mm;
2) with the mao bamboon powder that obtains in the step 1) under mechanical agitation, place 80 ℃ of 4.0wt%Mg (OH)
2React 100min in the solution, mao bamboon powder and Mg (OH)
2Solution quality repeats 3 times than for 1:5, cleans residual alkali with distilled water therebetween, obtains the mao bamboon fiber;
3) adopt 1.5wt%Ca (ClO)
2Solution under mechanical agitation, 80 ℃ of bleaching steps 2) in the mao bamboon fiber 210min that obtains, mao bamboon fiber and Ca (ClO)
2The mass ratio of solution is 1:10, repeats 4 times, cleans residual chlorine with distilled water therebetween, obtains high purity mao bamboon fiber;
4) with the high purity mao bamboon fiber that obtains in the step 3) under mechanical agitation, place 40 ℃ of 30wt% trichoroacetic acid(TCA) solution to react 150min, the mass ratio of mao bamboon fiber and organic acid soln is 1:15, adopt the room temperature distilled water termination reaction of 5 times of above-mentioned trichoroacetic acid(TCA) liquor capacities, clean residual acid, obtain mao bamboon nano micro crystal cellulose suspension;
5) with the mao bamboon nano micro crystal cellulose suspension centrifugation 10min under 10000rpm that obtains in the step 4), remove the above solid particulate of 1 μ m, taking out centrifugate filters through the 100kDa poly (ether-sulfone) ultrafiltration membrane, collect the solid ingredient that face is held back with distilled water, finally obtain mao bamboon nano micro crystal cellulose (a).
Embodiment 2:
1) with mao bamboon defoliation, clean, dry, adopt the plant pulverizer to pulverize, filter through 100 eye mesh screens, obtain particle diameter less than or equal to the mao bamboon powder of 0.15mm;
2) with the mao bamboon powder that obtains in the step 1) under mechanical agitation, place 90 ℃ of 4.0wt%Mg (OH)
2React 90min in the solution, mao bamboon powder and Mg (OH)
2Solution quality repeats 3 times than for 1:10, cleans residual alkali with distilled water therebetween, obtains the mao bamboon fiber;
3) adopt 2.0wt%Ca (ClO)
2Solution under mechanical agitation, 80 ℃ of bleaching steps 2) in the mao bamboon fiber 180min that obtains, mao bamboon fiber and Ca (ClO)
2The mass ratio of solution is 1:20, repeats 4 times, cleans residual chlorine with distilled water therebetween, obtains high purity mao bamboon fiber;
4) with the high purity mao bamboon fiber that obtains in the step 3) under mechanical agitation, place 45 ℃ of 50wt% Phenylsulfonic acid solution to react 180min, the mass ratio of mao bamboon fiber and organic acid soln is 1:10, adopt the room temperature distilled water termination reaction of 5 times of above-mentioned Phenylsulfonic acid liquor capacities, clean residual acid, obtain mao bamboon nano micro crystal cellulose suspension;
5) with the mao bamboon nano micro crystal cellulose suspension centrifugation 8min under 10000rpm that obtains in the step 4), remove the above solid particulate of 1 μ m, take out centrifugate through 100kDa polyvinylidene fluoride ultrafiltration membrane filtration, collect the solid ingredient that face is held back with distilled water, finally obtain mao bamboon nano micro crystal cellulose (b).
Embodiment 3:
1) with mao bamboon defoliation, clean, dry, adopt the plant pulverizer to pulverize, filter through 100 eye mesh screens, obtain particle diameter less than or equal to the mao bamboon powder of 0.15mm;
2) with the mao bamboon powder that obtains in the step 1) under mechanical agitation, place 70 ℃ of 6.0wt%Mg (OH)
2React 120min in the solution, mao bamboon powder and Mg (OH)
2Solution quality repeats 3 times than for 1:10, cleans residual alkali with distilled water therebetween, obtains the mao bamboon fiber;
3) adopt 3.0wt%Ca (ClO)
2Solution under mechanical agitation, 60 ℃ of bleaching steps 2) in the mao bamboon fiber 150min that obtains, mao bamboon fiber and Ca (ClO)
2The mass ratio of solution is 1:20, repeats 4 times, cleans residual chlorine with distilled water therebetween, obtains high purity mao bamboon fiber;
4) with the high purity mao bamboon fiber that obtains in the step 3) under mechanical agitation, in 60 ℃ of 40wt% citric acids and 30wt% trifluoro sulphur formic acid (volume ratio 1:1) mixing solutions, react 120min, the mass ratio of mao bamboon fiber and organic acid soln is 1:20, adopt the room temperature distilled water termination reaction of 5 times of above-mentioned trifluoro sulphur formic acid solution volumes, clean residual acid, obtain mao bamboon nano micro crystal cellulose suspension;
5) with the mao bamboon nano micro crystal cellulose suspension centrifugation 15min under 10000rpm that obtains in the step 4), remove the above solid particulate of 1 μ m, take out centrifugate through 50kDa regenerated cellulose ultrafiltration membrance filter, collect the solid ingredient that face is held back with distilled water, finally obtain mao bamboon nano micro crystal cellulose (c).
The appearance and size of three kinds of mao bamboon nano micro crystal celluloses that mensuration embodiment 1,2,3 prepares.Table 1 is the characterization result by embodiment 1,2,3 prepared mao bamboon nano micro crystal cellulose appearance and size.By data in the table 1 as can be known, adopt mao bamboon nano micro crystal cellulose (a) that preparation method of the present invention obtains, (b), (c) length distribution at 211 ~ 280nm, width distribution is at 15 ~ 24nm, length-to-diameter ratio is between 12 ~ 15, be nano-scale range, meet nano micro crystal cellulose dimensions feature.
Such as Fig. 1, can find out from the field emission scanning electron microscope photo of the mao bamboon nano micro crystal cellulose product of embodiment 1 preparation, its pattern is close to bar-shaped, because have higher specific surface area and abundant surface hydroxyl, slight attracting each other and agglomeration appearred in the mao bamboon nano micro crystal cellulose of preparation.
Table 1
What more than enumerate only is specific embodiments of the invention.The invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (3)
1. a method of utilizing mao bamboon chemical preparation nano micro crystal cellulose is characterized in that, may further comprise the steps:
1) with mao bamboon defoliation, clean, dry, adopt the plant pulverizer to pulverize, filter through 100 eye mesh screens, obtain particle diameter less than or equal to the mao bamboon powder of 0.15mm;
2) with step 1) in the mao bamboon powder that obtains under mechanical agitation, in 70 ~ 90 ℃ of basic solutions, react 90 ~ 120min, repeat 3 times, clean residual alkali with distilled water therebetween, obtain the mao bamboon fiber;
3) adopt contain chlorine solution under mechanical agitation, 60 ~ 80 ℃ of bleaching steps 2) in mao bamboon fiber 150 ~ 210min of obtaining, repeats 4 times, clean residual chlorine with distilled water therebetween, acquisition high purity mao bamboon fiber.
4) with step 3) in the high purity mao bamboon fiber that obtains under mechanical agitation, place 40 ~ 60 ℃ of organic acid solns to react 120 ~ 180min, adopt the room temperature distilled water termination reaction of 5 times of above-mentioned organic acid soln volumes, clean residual acid, obtain mao bamboon nano micro crystal cellulose suspension.
5) with step 4) in mao bamboon nano micro crystal cellulose suspension centrifugation 8 ~ 15min under 10000rpm of obtaining, remove the above solid particulate of 1 μ m, take out centrifugate through ultrafiltration membrance filter, collect the solid ingredient that face is held back with distilled water, finally obtain the mao bamboon nano micro crystal cellulose.
2. a kind of method of utilizing mao bamboon chemical preparation nano micro crystal cellulose according to claim 1, it is characterized in that: described basic solution is Mg (OH)
2Solution, massfraction are 4.0 ~ 6.0wt%, mao bamboon powder and Mg (OH)
2The mass ratio of solution is 1:5 ~ 10; Containing chlorine solution is Ca (ClO)
2Solution, massfraction are 1.5 ~ 3.0wt%, mao bamboon fiber and Ca (ClO)
2The mass ratio of solution is 1:10 ~ 20; Organic acid soln is the mixing acid of one or several the different proportionings in Phenylsulfonic acid, citric acid, trichoroacetic acid(TCA), the trifluoro sulphur formic acid, and massfraction is 30 ~ 50wt%, and the mass ratio of mao bamboon fiber and organic acid soln is 1:10 ~ 20.
3. a kind of method of utilizing mao bamboon chemical preparation nano micro crystal cellulose according to claim 1, it is characterized in that: described ultra-filtration membrane is a kind of in poly (ether sulfone) film, PVDF membrane, the regenerated cellulose film, and its molecular weight cut-off is 50 ~ 100kDa.
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| CN104387478A (en) * | 2014-12-17 | 2015-03-04 | 菏泽市产品质量监督检验所 | Preparation method of peony stem nano-cellulose for oil |
| CN104558211A (en) * | 2014-12-22 | 2015-04-29 | 尹建 | Method for preparing microcrystalline cellulose |
| CN104592400A (en) * | 2015-01-23 | 2015-05-06 | 湖州展望天明药业有限公司 | Preparation method of microcrystalline cellulose |
| CN105622991A (en) * | 2016-03-28 | 2016-06-01 | 浙江理工大学 | Preparation method of nano microcrystalline cellulose-reinforced chitosan/guar gum composite membrane |
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| CN105903025A (en) * | 2016-04-26 | 2016-08-31 | 浙江理工大学 | Preparation method of moso bamboo cellulose based nano oral drug carrier |
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| CN108779183A (en) * | 2015-12-16 | 2018-11-09 | 梵内塞尔瑞典股份公司 | The manufacture of nano-cellulose and its intermediate is carried out using two oxalic acid hydrates |
| CN105622991B (en) * | 2016-03-28 | 2018-08-31 | 台州浩展婴儿用品有限公司 | Nano micro crystal cellulose enhances the preparation method of chitosan/guar gum composite membrane |
| CN105622991A (en) * | 2016-03-28 | 2016-06-01 | 浙江理工大学 | Preparation method of nano microcrystalline cellulose-reinforced chitosan/guar gum composite membrane |
| CN105833330A (en) * | 2016-04-19 | 2016-08-10 | 常州市好利莱光电科技有限公司 | Preparation method of bamboo-based nano cellulose collagen composite material |
| CN105833330B (en) * | 2016-04-19 | 2018-09-21 | 烟台新时代健康产业日化有限公司 | A kind of preparation method of bamboo based nano-fiber element collagen composite material |
| CN105903025B (en) * | 2016-04-26 | 2018-12-11 | 浙江理工大学 | A kind of preparation method of moso bamboo cellulose based nano oral drugs carrier |
| CN105903025A (en) * | 2016-04-26 | 2016-08-31 | 浙江理工大学 | Preparation method of moso bamboo cellulose based nano oral drug carrier |
| CN108380184A (en) * | 2018-03-01 | 2018-08-10 | 浙江理工大学 | A method of utilizing paper pulp chemical preparation cellulose base material for water treatment |
| CN109485737A (en) * | 2018-12-19 | 2019-03-19 | 国际竹藤中心 | A method of Cellulose nanocrystal is prepared using moso bamboo |
| CN109457524A (en) * | 2018-12-29 | 2019-03-12 | 珠海市东辰制药有限公司 | The purification process and purifier apparatus of nano micro crystal cellulose |
| CN109457524B (en) * | 2018-12-29 | 2023-10-20 | 珠海市东辰制药有限公司 | Purification method and purification equipment of nano microcrystalline cellulose |
| CN110128554A (en) * | 2019-05-22 | 2019-08-16 | 江西农业大学 | A method of nano micro crystal cellulose is prepared using moso bamboo |
| CN111673876A (en) * | 2020-05-29 | 2020-09-18 | 泉州市康洪美傲建材科技有限公司 | Preparation method of high-strength wood composite inorganic particle board |
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