CN103804501B - One prepares the cellulosic method of square micron order - Google Patents
One prepares the cellulosic method of square micron order Download PDFInfo
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- CN103804501B CN103804501B CN201410006184.2A CN201410006184A CN103804501B CN 103804501 B CN103804501 B CN 103804501B CN 201410006184 A CN201410006184 A CN 201410006184A CN 103804501 B CN103804501 B CN 103804501B
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Abstract
The present invention discloses one and prepares the cellulosic method of square micron order, and specific embodiments is as follows: 1). with tosic acid-polyphosphoric acid hydrocellulose; 2). after above-mentioned hydrolysis terminates, thin up obtains white suspension liquid, carries out suction filtration to white suspension liquid, and gained solid water is washed till neutrality; 3). neutral solid will be washed to again with alcohol wash, centrifuging, after drying, obtain square micron order Mierocrystalline cellulose.Micrometer fibers element prepared by the present invention, shortens the reaction times effectively.
Description
Technical field
That the present invention relates to is a kind of preparation method of material, a kind of in particular method preparing square micrometer fibers element.
Background technology
Cellulosic structure is found by french chemist Payen for 1838, and adopted " Mierocrystalline cellulose " this title in 1839.Within 1932, cellulosic polymer form is finally confirmed by chemist Staudinger.Cellulosic chemical structure be by D-Glucopyranose ring each other with the linear polymer that β-Isosorbide-5-Nitrae-glycosidic link connects with C1 chair conformation, with three hydroxyls on each ring, be shown below
Micrometer fibers element (microncellulose) is the ultra-microfibers (forest-science, 11,37-46(2001) of diameter dimension at 10nm-10000nm).It all has broad application prospects in industries such as medicine, food and senior timber floors, it is raw material that model to be established one's virtue etc. with purified cotton, under the mineral acids such as sulfuric acid, hydrochloric acid, Hydrogen bromide exist situation, be heated to 70 DEG C ~ 110 DEG C makes it be hydrolyzed, wash to pH value 6 ± 1 again, wet product obtains product after pulverizing drying, outward appearance is fibrous fine powder, is not block micrometer fibers element (Chinese invention patent application number: CN1414022, title: nano grade alpha cellulose and preparation method thereof); Wang Lushan, commercial fibre element is carried out ball-milling processing by the people such as champion Chen, then product flotation is deposited, again supersound process is carried out to target product and obtain the homogeneous cellulose powder of a kind of micron order, cellulose powder mean polymerisation degree is 100-300, described cellulose powder particle size distribution scope is 1-10 micron, and degree of crystallinity is 70-80%, and specific surface area is 10000-30000CM
2/ CM
3, be mainly used in the mensuration (Chinese invention patent application number: 101220174, title: a kind of micrometre level uniform cellulose powder and preparation method thereof and application) of chemical industry, fermentation industry cellulase activity, this method size distribution is wide and energy consumption is large; Tension force is put down, Chen Guowei etc. are under 40Hz ultrasonic vibration, using the mixing acid of hydrochloric acid and sulfuric acid (volume ratio 1:2) as hydrolyst, 12.5g cellulose pulp be impregnated in 250ml mixed acid solution, constant temperature stirring reaction certain hour under 80 DEG C of bath temperatures.Adjust ph also with deionized water wash to neutral, obtains Mierocrystalline cellulose fluoride micro-nano colloidal solution.After suction filtration drying, with obtaining crystal powder (Beijing Forestry University's journal, 4,1-6(2008) after ball mill pulverizer drying), this method shortcoming is complicated and energy consumption is high.
Summary of the invention
goal of the invention:the object of the invention is to, for the not enough problem of bulk fibers element research, provide a kind of novel method of preparation square micrometer fibers element newly.Tosic acid-polyphosphoric acid system cotton hydrocellulose is used to prepare the Mierocrystalline cellulose of micron-scale.
technical scheme:the method that the present invention prepares square micrometer fibers element is achieved through the following technical solutions,
1). with tosic acid-polyphosphoric acid hydrocellulose;
2). after above-mentioned hydrolysis terminates, thin up obtains white suspension liquid, carries out suction filtration to white suspension liquid, and gained solid water is washed till neutrality;
3). neutral solid will be washed to again with alcohol wash, centrifuging, after drying, obtain square micron order Mierocrystalline cellulose.
Described step 1) in Mierocrystalline cellulose be the cotton fibre of the polymerization degree at 600-1000.
Described step 1) in the cellulolytic reaction conditions of tosic acid-polyphosphoric acid be that temperature of reaction controls at 70 DEG C ~ 80 DEG C, reaction times 25min ~ 35min.
beneficial effect:the present invention invent a kind of newly prepare the cellulosic method of micron order, this method obtains square micron order Mierocrystalline cellulose by tosic acid-polyphosphoric acid system cotton hydrocellulose, and hydrolysising condition is gentle, and the reaction times is short, aftertreatment is simple and have higher yields, is applicable to industrial production.
Embodiment
Elaborate to embodiments of the invention below, the present embodiment is implemented under premised on technical solution of the present invention, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Example 1
The cotton fibre of the polymerization degree 800 of 1.0g, 1.0g p-methyl benzenesulfonic acid and 50g polyphosphoric acid are joined in the beaker of 100ml, is heated to 80 DEG C, stirring reaction 25min.Reaction terminates thin up, obtains white suspension liquid, suction filtration, is washed to neutrality, then use washing with alcohol twice, centrifuging, and solid is dried and obtained white square shape micrometer fibers element, and length and width are all between 0.5um-1.0um.
Example 2
The cotton fibre of the polymerization degree 1000 of 1.0g, 1.0g p-methyl benzenesulfonic acid and 50g polyphosphoric acid are joined in the beaker of 100ml, is heated to 70 DEG C, stirring reaction 30min.Reaction terminates thin up, obtains white suspension liquid, suction filtration, is washed to neutrality, then use washing with alcohol twice, centrifuging, and solid is dried and obtained white square shape micrometer fibers element, and length and width are all between 0.5um-1.0um.
Example 3
The cotton fibre of the polymerization degree 600 of 1.0g, 1.0g p-methyl benzenesulfonic acid and 50g polyphosphoric acid are joined in the beaker of 100ml, is heated to 75 DEG C, stirring reaction 30min.Reaction terminates thin up, obtains white suspension liquid, suction filtration, is washed to neutrality, then use washing with alcohol twice, centrifuging, and solid is dried and obtained white square shape micrometer fibers element, and length and width are all between 0.5um-1.0um.
Claims (2)
1. prepare a method for square micrometer fibers element, it is characterized in that the method comprises following preparation process:
1). with tosic acid-polyphosphoric acid hydrocellulose; Reaction conditions is, temperature of reaction controls at 70 DEG C ~ 80 DEG C, reaction times 25min ~ 35min;
2). after above-mentioned hydrolysis terminates, thin up obtains white suspension liquid, carries out suction filtration to white suspension liquid, and gained solid water is washed till neutrality;
3). neutral solid will be washed to again with alcohol wash, centrifuging, after drying, obtain square micron order Mierocrystalline cellulose.
2., according to a kind of method preparing square micrometer fibers element described in claims 1, it is characterized in that: described step 1) in Mierocrystalline cellulose be the cotton fibre of the polymerization degree at 600-1000.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410006184.2A CN103804501B (en) | 2014-01-07 | 2014-01-07 | One prepares the cellulosic method of square micron order |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410006184.2A CN103804501B (en) | 2014-01-07 | 2014-01-07 | One prepares the cellulosic method of square micron order |
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| CN103804501A CN103804501A (en) | 2014-05-21 |
| CN103804501B true CN103804501B (en) | 2016-01-06 |
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| CN201410006184.2A Expired - Fee Related CN103804501B (en) | 2014-01-07 | 2014-01-07 | One prepares the cellulosic method of square micron order |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005074395A2 (en) * | 2004-02-10 | 2005-08-18 | Samsung Fine Chemicals Co., Ltd. | Method of preparing aqueous dispersion of hydroxypropyl methyl cellulose phthalate nanoparticle composition |
| CN101638441A (en) * | 2009-08-28 | 2010-02-03 | 中国科学院西双版纳热带植物园 | Method for hydrolyzing lignocellulose |
| CN101772515A (en) * | 2007-08-10 | 2010-07-07 | 陶氏环球技术公司 | The nanoparticle of amorphous cellulose |
| CN101942102A (en) * | 2010-09-07 | 2011-01-12 | 东南大学 | Preparation method of powder nano cellulose |
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2014
- 2014-01-07 CN CN201410006184.2A patent/CN103804501B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005074395A2 (en) * | 2004-02-10 | 2005-08-18 | Samsung Fine Chemicals Co., Ltd. | Method of preparing aqueous dispersion of hydroxypropyl methyl cellulose phthalate nanoparticle composition |
| CN101772515A (en) * | 2007-08-10 | 2010-07-07 | 陶氏环球技术公司 | The nanoparticle of amorphous cellulose |
| CN101638441A (en) * | 2009-08-28 | 2010-02-03 | 中国科学院西双版纳热带植物园 | Method for hydrolyzing lignocellulose |
| CN101942102A (en) * | 2010-09-07 | 2011-01-12 | 东南大学 | Preparation method of powder nano cellulose |
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Granted publication date: 20160106 Termination date: 20190107 |