CN1141321C - Method for preparing nanocrystal cellulose by means of acid hydrolysis - Google Patents
Method for preparing nanocrystal cellulose by means of acid hydrolysis Download PDFInfo
- Publication number
- CN1141321C CN1141321C CNB011297174A CN01129717A CN1141321C CN 1141321 C CN1141321 C CN 1141321C CN B011297174 A CNB011297174 A CN B011297174A CN 01129717 A CN01129717 A CN 01129717A CN 1141321 C CN1141321 C CN 1141321C
- Authority
- CN
- China
- Prior art keywords
- ncc
- hydrolysis
- cellulose
- nanocrystal cellulose
- acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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- 229920002678 cellulose Polymers 0.000 title claims abstract description 37
- 239000001913 cellulose Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000002159 nanocrystal Substances 0.000 title claims abstract description 19
- 238000005903 acid hydrolysis reaction Methods 0.000 title claims abstract description 17
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 31
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 29
- 230000007062 hydrolysis Effects 0.000 claims abstract description 29
- 239000000835 fiber Substances 0.000 claims description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 29
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- 239000012528 membrane Substances 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 11
- 229920000742 Cotton Polymers 0.000 claims description 9
- 230000018044 dehydration Effects 0.000 claims description 8
- 238000006297 dehydration reaction Methods 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000007670 refining Methods 0.000 claims description 5
- 238000006386 neutralization reaction Methods 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 3
- 235000010755 mineral Nutrition 0.000 claims description 3
- 239000011707 mineral Substances 0.000 claims description 3
- 230000003472 neutralizing effect Effects 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical group [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims 3
- 238000010129 solution processing Methods 0.000 claims 1
- 239000003513 alkali Substances 0.000 abstract description 7
- 239000001117 sulphuric acid Substances 0.000 abstract description 4
- 235000011149 sulphuric acid Nutrition 0.000 abstract description 4
- 229920003043 Cellulose fiber Polymers 0.000 abstract 1
- 150000007522 mineralic acids Chemical class 0.000 abstract 1
- 235000010980 cellulose Nutrition 0.000 description 22
- 239000000243 solution Substances 0.000 description 12
- 239000002253 acid Substances 0.000 description 10
- 239000002105 nanoparticle Substances 0.000 description 10
- 235000011121 sodium hydroxide Nutrition 0.000 description 9
- 229940083608 sodium hydroxide Drugs 0.000 description 8
- 241000212978 Amorpha <angiosperm> Species 0.000 description 7
- 239000012535 impurity Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 229920001131 Pulp (paper) Polymers 0.000 description 4
- 229920002301 cellulose acetate Polymers 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 230000008030 elimination Effects 0.000 description 4
- 238000003379 elimination reaction Methods 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- -1 sulfuric acid ester Chemical class 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 230000002950 deficient Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000003301 hydrolyzing effect Effects 0.000 description 3
- 238000002329 infrared spectrum Methods 0.000 description 3
- 229920002521 macromolecule Polymers 0.000 description 3
- 239000004677 Nylon Substances 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- GOYYUYNOGNSLTE-UHFFFAOYSA-N copper;2-azanidylethylazanide Chemical compound [Cu+2].[NH-]CC[NH-].[NH-]CC[NH-] GOYYUYNOGNSLTE-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010612 desalination reaction Methods 0.000 description 2
- 238000006266 etherification reaction Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 229920001778 nylon Polymers 0.000 description 2
- 229920002492 poly(sulfone) Polymers 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 238000005185 salting out Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 240000008564 Boehmeria nivea Species 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 229920000168 Microcrystalline cellulose Polymers 0.000 description 1
- 241000237502 Ostreidae Species 0.000 description 1
- 238000007171 acid catalysis Methods 0.000 description 1
- 230000004931 aggregating effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 230000035614 depigmentation Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 235000019813 microcrystalline cellulose Nutrition 0.000 description 1
- 239000008108 microcrystalline cellulose Substances 0.000 description 1
- 229940016286 microcrystalline cellulose Drugs 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 235000020636 oyster Nutrition 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
Description
Claims (7)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB011297174A CN1141321C (en) | 2001-09-30 | 2001-09-30 | Method for preparing nanocrystal cellulose by means of acid hydrolysis |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB011297174A CN1141321C (en) | 2001-09-30 | 2001-09-30 | Method for preparing nanocrystal cellulose by means of acid hydrolysis |
Publications (2)
Publication Number | Publication Date |
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CN1341663A CN1341663A (en) | 2002-03-27 |
CN1141321C true CN1141321C (en) | 2004-03-10 |
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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CNB011297174A Expired - Lifetime CN1141321C (en) | 2001-09-30 | 2001-09-30 | Method for preparing nanocrystal cellulose by means of acid hydrolysis |
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Families Citing this family (34)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101070352B (en) * | 2007-03-27 | 2011-05-11 | 鲁东大学 | Method for preparing sheet-like microcrystal cellulose and modification processing method |
EP2344689B1 (en) * | 2008-10-14 | 2014-04-23 | SAPPI Netherlands Services B.V. | Process for the manufacture of cellulose-based fibres and the fibres thus obtained |
JP5717646B2 (en) * | 2008-12-11 | 2015-05-13 | エフピーイノベイションズ | Redispersible dry nanocrystalline cellulose |
BRPI1011265A2 (en) * | 2009-05-06 | 2019-09-24 | Fpinnovations | pulp, method and process for producing pulp, and process for producing pulp materials. |
EP2464599B1 (en) * | 2009-08-11 | 2016-09-07 | FPInnovations | Fractionation of a waste liquor stream from nanocrystalline cellulose production |
CN101768221B (en) * | 2010-03-12 | 2012-02-29 | 福建农林大学 | Method for preparing nano-crystal cellulose II by using basic anion-exchange resin |
CN101864606B (en) * | 2010-06-30 | 2011-09-07 | 东北林业大学 | Preparation method of biomass cellulose nanofibers with high length-diameter ratio |
CN102080342B (en) * | 2010-11-25 | 2013-04-24 | 山东轻工业学院 | Anionic organic particles and preparation and application thereof |
CN102080343B (en) * | 2010-11-25 | 2013-05-29 | 山东轻工业学院 | Application of anion nano microcrystalline cellulose as paper reinforcer |
CN102080341B (en) * | 2010-11-25 | 2013-04-24 | 山东轻工业学院 | Cationic organic particles and preparation and application thereof |
CN102040663B (en) * | 2010-12-06 | 2012-08-29 | 东华大学 | Preparation method of narrow-distribution cellulose nanocrystalline |
CN102311505B (en) * | 2011-07-18 | 2012-12-05 | 东华大学 | Method for preparing cellulose nanospheres based on waste dissolvable fibers |
FI126118B (en) * | 2012-02-10 | 2016-06-30 | Upm Kymmene Corp | Cellulose pulp pretreatment method |
CN102585017B (en) * | 2012-03-27 | 2013-12-11 | 东华大学 | Preparation method of nanoscale solidago canadensis L. microcrystalline cellulose |
WO2014029001A1 (en) * | 2012-08-21 | 2014-02-27 | Noram Engineering And Constructors Ltd. | Purification process for partly-hydrolyzed cellulose |
US20140155301A1 (en) * | 2012-11-30 | 2014-06-05 | Api Intellectual Property Holdings, Llc | Processes and apparatus for producing nanocellulose, and compositions and products produced therefrom |
CN103304824A (en) * | 2013-06-15 | 2013-09-18 | 浙江理工大学 | Preparation method of high-concentration nano microcrystalline cellulose gel |
CN104288842A (en) * | 2013-07-19 | 2015-01-21 | 中国国旅贸易有限责任公司 | Injectable bone joint lubricating material and preparation method thereof |
CN104342850B (en) * | 2013-08-08 | 2017-03-15 | 北京纳迅科技股份有限公司 | polyimide film containing nanocrystal cellulose and preparation method thereof |
CN104629276B (en) * | 2013-11-12 | 2017-01-11 | 珠海市红旌发展有限公司 | Preparation method for nanocrystal cellulose composite material, product and application thereof |
CN104381591A (en) * | 2013-12-19 | 2015-03-04 | 珠海市红旌发展有限公司 | Feed containing nanocrystalline cellulose |
KR102358824B1 (en) * | 2014-01-29 | 2022-02-07 | 이섬 리서치 디벨러프먼트 컴파니 오브 더 히브루 유니버시티 오브 예루살렘 엘티디. | Porous nanocrystalline cellulose structures |
US9499637B2 (en) * | 2014-06-23 | 2016-11-22 | Api Intellectual Property Holdings, Llc | Nanocellulose compositions and processes to produce same |
CN104448007A (en) * | 2014-11-14 | 2015-03-25 | 中国科学院青岛生物能源与过程研究所 | Method for preparing nano-cellulose |
CN104887583B (en) * | 2015-06-15 | 2017-11-24 | 天津科技大学 | A kind of preparation method of cellulose base Polyphenols natural anti-oxidation compound |
CN105670005B (en) * | 2016-03-25 | 2017-12-19 | 西南交通大学 | A kind of process that Cellulose nanocrystal dispersion liquid is prepared based on controllable dissolving |
CN106380613B (en) * | 2016-09-28 | 2019-01-22 | 武汉纺织大学 | A kind of preparation method of ramie core Cellulose nanocrystal self-assembled structures color film |
CN106810614B (en) * | 2017-01-21 | 2019-04-12 | 深圳市优普惠药品股份有限公司 | A kind of preparation process of nanocrystal cellulose |
CN108084278A (en) * | 2018-01-02 | 2018-05-29 | 青岛大学 | A kind of preparation method of small size Cellulose nanocrystal |
CN109208366B (en) * | 2018-09-06 | 2021-05-25 | 刘永红 | Preparation method and application of micro-nano cellulose |
CN109438580B (en) * | 2018-11-27 | 2021-04-27 | 陕西科技大学 | Method for preparing nano cellulose crystal from ultralow acid hydrolysis fiber |
CN109608555A (en) * | 2018-12-25 | 2019-04-12 | 天津科技大学 | A kind of method that ultrasonic wave assist acid hydrolysis microcrystalline cellulose prepares nanofiber crystalline substance |
CN110183538A (en) * | 2019-06-21 | 2019-08-30 | 大连工业大学 | A kind of method of the slightly sour preparation Cellulose nanocrystal body of promotion system altogether of inorganic fused salt- |
CN114345129A (en) * | 2022-02-14 | 2022-04-15 | 天津如米新材料有限公司 | Cellulose nanocrystalline separation and purification method based on microfiltration separation and direct deacidification |
-
2001
- 2001-09-30 CN CNB011297174A patent/CN1141321C/en not_active Expired - Lifetime
Also Published As
Publication number | Publication date |
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CN1341663A (en) | 2002-03-27 |
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