CN103804501A - Method for preparing square micron-sized cellulose - Google Patents
Method for preparing square micron-sized cellulose Download PDFInfo
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- CN103804501A CN103804501A CN201410006184.2A CN201410006184A CN103804501A CN 103804501 A CN103804501 A CN 103804501A CN 201410006184 A CN201410006184 A CN 201410006184A CN 103804501 A CN103804501 A CN 103804501A
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Abstract
The invention discloses a method for preparing square micron-sized cellulose. The method comprises specific steps of (1) hydrolyzing cellulose with p-toluenesulfonic acid-polyphosphoric acid; (2) after hydrolysis, adding water and diluting so as to obtain white turbid liquid, carrying out suction filtering on the white turbid liquid, washing the obtained solids to be neutral by using water; (3) carrying out alcohol washing on the neutral solids, centrifuging, filtering, drying so as to obtain the square micron-sized cellulose. The micron-sized cellulose prepared by the method effectively shortens reaction time.
Description
Technical field
That the present invention relates to is a kind of preparation method of material, in particular a kind of method of preparing square shape micrometer fibers element.
Background technology
Cellulosic structure is to be found by french chemist Payen for 1838, and adopts " Mierocrystalline cellulose " this title in 1839.Within 1932, cellulosic polymer form is finally confirmed by chemist Staudinger.Cellulosic chemical structure is to connect each other by D-Glucopyranose ring the linear polymer forming with C1 chair conformation with β-Isosorbide-5-Nitrae-glycosidic link, on each ring, with three hydroxyls, is shown below
Micrometer fibers element (micron cellulose) is the ultra micro fiber (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, model is established one's virtue etc. take purified cotton as raw material, exist and in situation, be heated to 70 ℃～110 ℃ and make its hydrolysis at mineral acids such as sulfuric acid, hydrochloric acid, Hydrogen bromides, wash again to pH value 6 ± 1, wet product obtains product through pulverizing after dry, 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 target product is carried out supersound process and is obtained a kind of cellulose powder of micron order homogeneous, 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 chemical industry, fermentation industry cellulase activity mensuration (Chinese invention patent application number: 101220174, title: a kind of micrometre level uniform cellulose powder and preparation method thereof and application), this method size distribution is wide and energy consumption is large; Tension force is flat, 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 to constant temperature stirring reaction certain hour under 80 ℃ of bath temperatures.Regulate pH value extremely neutral with deionized water wash, obtain Mierocrystalline cellulose micro-nano crystal colloidal solution.After suction filtration is dry, after being dried with ball mill pulverizer, obtain crystal powder (Beijing Forestry University's journal, 4,1-6(2008)), this method shortcoming is that complexity and energy consumption are high.
Summary of the invention
goal of the invention:the object of the invention is to study not enough problem for block Mierocrystalline cellulose, a kind of new novel method of preparing square shape micrometer fibers element is provided.Use tosic acid-polyphosphoric acid system cotton hydrocellulose to prepare the Mierocrystalline cellulose of micron-scale.
technical scheme:the method that the present invention prepares square shape micrometer fibers element is achieved through the following technical solutions,
1). with tosic acid-polyphosphoric acid hydrocellulose;
2). after above-mentioned hydrolysis finishes, thin up obtains white suspension liquid, and white suspension liquid is carried out to suction filtration, and gained solid water is washed till neutrality;
3). will be washed to neutral solid again with alcohol wash, centrifuging, obtains square shape micron order Mierocrystalline cellulose after being dried.
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 is controlled at 70 ℃～80 ℃, reaction times 25min～35min.
beneficial effect:the present invention has invented a kind of new cellulosic method of micron order of preparing, this method makes square shape micron order Mierocrystalline cellulose by tosic acid-polyphosphoric acid system cotton hydrocellulose, hydrolysising condition gentleness, and the reaction times is short, aftertreatment is simple and have higher yields, is applicable to industrial production.
Embodiment
Below embodiments of the invention are elaborated, the present embodiment is implemented under take technical solution of the present invention as prerequisite, provided 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 of 1.0g 800,1.0g p-methyl benzenesulfonic acid and 50g polyphosphoric acid are joined in the beaker of 100ml, be heated to 80 ℃, stirring reaction 25min.Reaction finishes thin up, obtains white suspension liquid, and suction filtration, is washed to neutrality, then uses washing with alcohol twice, centrifuging, and solid is dried and is 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 of 1.0g 1000,1.0g p-methyl benzenesulfonic acid and 50g polyphosphoric acid are joined in the beaker of 100ml, be heated to 70 ℃, stirring reaction 30min.Reaction finishes thin up, obtains white suspension liquid, and suction filtration, is washed to neutrality, then uses washing with alcohol twice, centrifuging, and solid is dried and is 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 of 1.0g 600,1.0g p-methyl benzenesulfonic acid and 50g polyphosphoric acid are joined in the beaker of 100ml, be heated to 75 ℃, stirring reaction 30min.Reaction finishes thin up, obtains white suspension liquid, and suction filtration, is washed to neutrality, then uses washing with alcohol twice, centrifuging, and solid is dried and is obtained white square shape micrometer fibers element, and length and width are all between 0.5um-1.0um.
Claims (3)
1. prepare a method for square shape micrometer fibers element, it is characterized in that the method comprises following preparation process:
1). with tosic acid-polyphosphoric acid hydrocellulose;
2). after above-mentioned hydrolysis finishes, thin up obtains white suspension liquid, and white suspension liquid is carried out to suction filtration, and gained solid water is washed till neutrality;
3). will be washed to neutral solid again with alcohol wash, centrifuging, obtains square shape micron order Mierocrystalline cellulose after being dried.
2. according to a kind of method of preparing square shape 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.
3. according to a kind of method of preparing micrometer fibers element described in claims 1, it is characterized in that: described step 1) in the cellulolytic reaction conditions of tosic acid-polyphosphoric acid be, temperature of reaction is controlled at 70 ℃～80 ℃, reaction times 25min～35min.
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 |
Applications Claiming Priority (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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| Publication Number | Publication Date |
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| CN103804501A true CN103804501A (en) | 2014-05-21 |
| CN103804501B 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 |