CN1104647A - Manufacture of nm avicel powder by solvent process - Google Patents
Manufacture of nm avicel powder by solvent process Download PDFInfo
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- CN1104647A CN1104647A CN 94115873 CN94115873A CN1104647A CN 1104647 A CN1104647 A CN 1104647A CN 94115873 CN94115873 CN 94115873 CN 94115873 A CN94115873 A CN 94115873A CN 1104647 A CN1104647 A CN 1104647A
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- organic solvent
- solvent
- mierocrystalline cellulose
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- sized crystal
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Abstract
A solvent method is used in chemical treatment of plant fibres such as cotton or ramie to obtain nm-class (2.5-10nm) avicel. Its technical steps include washing cellulose by water-soluble organic solvent (acetone or alcohol) with low boiling point, centrifugal removal of solvent, repeating the washing step; low-temp. drying, breaking and sieving.
Description
The present invention relates to produce the method for nano-sized crystal Mierocrystalline cellulose powder with solvent.
Common Microcrystalline Cellulose is widely used as aspects such as medicine excipient, welding agent filler and industrial chemicals.Producing of Microcrystalline Cellulose is with hydrochloric acid hydrolysis cotton or natural fibers such as storage fiber crops etc., again through operation such as washing, neutralization, dehydration, drying, pulverizing and must product.It is fibrous that Microcrystalline Cellulose is, long 20 μ m-50 μ m, and mouthfeel is bad when using as foodstuff additive (as beverage, the pouring of ice fine jade, cream setting agent etc.), and non-uniform phenomenon still responds when using as the chemical reaction raw material.Microcrystalline Cellulose is easy to make product with spraying drying because particle is thicker, non-caked mutually, water-absorbent is lower.The nano-sized crystal Mierocrystalline cellulose is particulate state, and size is between 2.5nm-10nm, and it is further to handle and make with chemical process on the basis of Microcrystalline Cellulose, and its smooth mouth feel can be made plurality kinds of health care type foodstuff additive, and is more even during as chemical reaction.The nano-sized crystal Mierocrystalline cellulose is bonded to greatly firmly soon product because cellulose grain and water molecules are formed hydrogen bond behind drying and dewatering, is difficult for pulverizing.
The objective of the invention is to attempt to provide a kind of method of producing nano-sized crystal Mierocrystalline cellulose powder with solvent.
Preparation method provided by the invention, be to adopt water-soluble lower boiling organic solvent, washing nano-sized crystal Mierocrystalline cellulose, solvent and cellulosic weight ratio are 1: 1, handle the back and remove with centrifuging and desolvate, use organic solvent repeated washing treating processes again after, pass through centrifuge dehydration again and at≤45 ℃, drying is 2 hours under the 600mmHg-700mmHg vacuum tightness, pulverizes then, sieves, and obtains nano-sized crystal Mierocrystalline cellulose powder product.Used organic solvent is acetone or the alcohol of purity more than 85%, and these solvents can recycling after using.Organic solvent role in washing process is as follows:
1, the moisture content in the Mierocrystalline cellulose is cemented out and dewater, and can not be combined into hydrogen bond with water when making Mierocrystalline cellulose dry.
2, because the organic solvent boiling point is low, and vaporization heat is little, therefore make material dry easily, and the effusion of organic solvent make the cellulose particles intergranular stay the space, be easy to pulverize.
3, but lysochrome and the impurity of organic solvent in can the flush away Mierocrystalline cellulose improves product purity.
Preparation method provided by the invention, products obtained therefrom has following advantage:
The Microcrystalline Cellulose water-absorbent is strong, and can play thickening power, because particle is minimum, smooth mouth feel when making foodstuff additive during as if the participation chemical reaction, near homogeneous reaction, can be improved the quality of products.
Embodiment
Adopt chemical process to handle the nano-sized crystal Mierocrystalline cellulose that cotton obtains, without grinding or high-speed stirring the time, a plurality of cellulose grains are combined into larger particles with loose form, proportion is greater than water, this moment, available clear water washing was to neutral, place the whizzer that is placed with filter cloth to dewater, get the nano-sized crystal Mierocrystalline cellulose of water content about 50%.Add 25 kilograms of purity in per 25 kilograms of wet feeds greater than 85% washing with acetone in whizzer, the centrifugal acetone that takes off adds the new acetone of equivalent and repeats above-mentioned washing process.Centrifugal or Mierocrystalline cellulose put in 45 ℃ of baking ovens vacuum-drying 2 hours, with bar type rotating disintegrator comminuting matter, cross 300 mesh sieves and get product.The washing with acetone mother liquor reclaims acetone with distillation method for the first time, and the acetone mother liquor of washing gives over to next batch of material work and washs usefulness for the first time for the second time, and the acetone that baking oven steams reclaims with condensation method.
Claims (4)
1, a kind of method of producing nano-sized crystal Mierocrystalline cellulose powder with solvent, it is characterized in that with water-soluble lower boiling organic solvent, washing nano-sized crystal Mierocrystalline cellulose, solvent and cellulosic weight ratio are 1: 1, except that desolvating, use organic solvent repeated washing process with centrifuging again, passed through centrifuge dehydration and drying again 2 hours, pulverize then and sieve, obtain nano-sized crystal Mierocrystalline cellulose powder product.
2,, it is characterized in that described organic solvent purity is acetone or the alcohol more than 85% according to the method described in the claim 1.
3, according to the method described in the claim 1, it is characterized in that 45 ℃ of described drying temperatures, vacuum tightness is 600mmHg-700mmHg.
4,, it is characterized in that described organic solvent can reclaim again to use according to the method described in the claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94115873A CN1051093C (en) | 1994-09-16 | 1994-09-16 | Manufacture of nm avicel powder by solvent process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94115873A CN1051093C (en) | 1994-09-16 | 1994-09-16 | Manufacture of nm avicel powder by solvent process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1104647A true CN1104647A (en) | 1995-07-05 |
| CN1051093C CN1051093C (en) | 2000-04-05 |
Family
ID=5037687
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN94115873A Expired - Fee Related CN1051093C (en) | 1994-09-16 | 1994-09-16 | Manufacture of nm avicel powder by solvent process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1051093C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1075515C (en) * | 1998-12-30 | 2001-11-28 | 中国科学院广州化学研究所 | Preparation of microcrystal cellulose colloid |
| CN1089618C (en) * | 1998-07-30 | 2002-08-28 | 武汉大学 | Process for preparing porous filler of regenerated cellulose for gel permeation chromatographic column |
| WO2004055250A1 (en) * | 2002-12-18 | 2004-07-01 | The Hong Kong Polytechnic University | Method for pulverizing natural organic substance into nano-scale fibrous material |
| CN101864684A (en) * | 2010-06-11 | 2010-10-20 | 中国林业科学研究院林产化学工业研究所 | Method for preparing pharmaceutical-grade microcrystalline cellulose from cotton linter |
| CN107365392A (en) * | 2017-08-31 | 2017-11-21 | 泸州北方化学工业有限公司 | A kind of method for improving water-soluble cellulose ether product free-running property |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3345357A (en) * | 1964-02-06 | 1967-10-03 | Fmc Corp | Method of purifying cellulose crystallite aggregates |
| JPS5255513A (en) * | 1975-10-30 | 1977-05-07 | Fujitsu Ltd | Magnetic head |
| JP2733259B2 (en) * | 1988-09-20 | 1998-03-30 | 旭化成工業株式会社 | Porous microcellulose particles |
| JPH0611793B2 (en) * | 1989-08-17 | 1994-02-16 | 旭化成工業株式会社 | Suspension of micronized cellulosic material and method for producing the same |
| JP3044470B2 (en) * | 1990-06-07 | 2000-05-22 | 日清紡績株式会社 | Method for producing cellulose fine powder |
| CN1037846C (en) * | 1992-07-04 | 1998-03-25 | 苏志刚 | Technology for producing microcrystalline cellulose with sulfated waste cotton velvet |
-
1994
- 1994-09-16 CN CN94115873A patent/CN1051093C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1089618C (en) * | 1998-07-30 | 2002-08-28 | 武汉大学 | Process for preparing porous filler of regenerated cellulose for gel permeation chromatographic column |
| CN1075515C (en) * | 1998-12-30 | 2001-11-28 | 中国科学院广州化学研究所 | Preparation of microcrystal cellulose colloid |
| WO2004055250A1 (en) * | 2002-12-18 | 2004-07-01 | The Hong Kong Polytechnic University | Method for pulverizing natural organic substance into nano-scale fibrous material |
| CN100374629C (en) * | 2002-12-18 | 2008-03-12 | 香港理工大学 | Method for pulverizing natural organic matter into nano-grade fiber material |
| CN101864684A (en) * | 2010-06-11 | 2010-10-20 | 中国林业科学研究院林产化学工业研究所 | Method for preparing pharmaceutical-grade microcrystalline cellulose from cotton linter |
| CN107365392A (en) * | 2017-08-31 | 2017-11-21 | 泸州北方化学工业有限公司 | A kind of method for improving water-soluble cellulose ether product free-running property |
| CN107365392B (en) * | 2017-08-31 | 2019-10-18 | 泸州北方化学工业有限公司 | A method of improving water-soluble cellulose ether product free-running property |
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| Publication number | Publication date |
|---|---|
| CN1051093C (en) | 2000-04-05 |
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