CN100374629C - Method for pulverizing natural organic matter into nano-grade fiber material - Google Patents
Method for pulverizing natural organic matter into nano-grade fiber material Download PDFInfo
- Publication number
- CN100374629C CN100374629C CNB2003801062645A CN200380106264A CN100374629C CN 100374629 C CN100374629 C CN 100374629C CN B2003801062645 A CNB2003801062645 A CN B2003801062645A CN 200380106264 A CN200380106264 A CN 200380106264A CN 100374629 C CN100374629 C CN 100374629C
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- Prior art keywords
- natural organic
- organic substance
- ground
- nano
- suspension
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- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000002657 fibrous material Substances 0.000 title claims abstract description 4
- 238000010298 pulverizing process Methods 0.000 title abstract description 22
- 239000005416 organic matter Substances 0.000 title abstract 5
- 239000000725 suspension Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000007921 spray Substances 0.000 claims abstract description 7
- 239000002105 nanoparticle Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims abstract description 3
- 239000000126 substance Substances 0.000 claims description 29
- 239000000463 material Substances 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 5
- 239000012459 cleaning agent Substances 0.000 claims description 4
- 239000008187 granular material Substances 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000004851 dishwashing Methods 0.000 claims description 2
- 239000004519 grease Substances 0.000 claims description 2
- 239000000344 soap Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 36
- 239000000835 fiber Substances 0.000 abstract description 29
- 239000011368 organic material Substances 0.000 abstract description 4
- 239000011362 coarse particle Substances 0.000 abstract 1
- 239000010419 fine particle Substances 0.000 abstract 1
- 210000002268 wool Anatomy 0.000 description 22
- 229920000742 Cotton Polymers 0.000 description 9
- 241000050051 Chelone glabra Species 0.000 description 7
- 239000004753 textile Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 208000012886 Vertigo Diseases 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 108010022355 Fibroins Proteins 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241000208202 Linaceae Species 0.000 description 1
- 235000004431 Linum usitatissimum Nutrition 0.000 description 1
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C19/00—Other disintegrating devices or methods
- B02C19/18—Use of auxiliary physical effects, e.g. ultrasonics, irradiation, for disintegrating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C21/00—Disintegrating plant with or without drying of the material
Landscapes
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Disintegrating Or Milling (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
A method for comminuting natural organic matter into a nano-scale fibrous material, comprising the steps of: cleaning oil on the natural organic matter raw material and drying the natural organic matter raw material by adopting common equipment; coarsely pulverizing the prepared natural organic matter into small particles with a length dimension of about 500 μm by using a common mechanical pulverizer; mixing the coarse particles and pure water to form suspension, and finely crushing the suspension by a professional ultrasonic crusher to form particles, wherein the diameters and the length sizes of the particles are less than 20 mu m; feeding the suspension containing fine particles into a nano-collider under high pressure to divide the suspension into two parts, causing them to collide with each other and generate vibration, thereby causing the raw material to have a nano-scale size; if it is desired to dry the nanoscaled organic material fibre particles, the nanoparticles are dried using a conventional spray dryer.
Description
Technical field
The present invention relates to breaking method, especially relate to the method that natural organic substance is crushed into nanometer stage material.
Background of invention
Since ancient times, natural fabric has played important function in textile material, and because its peculiar property as high-quality textile material has still obtained extensive use in modern textile industry.Yet in view of the restrictive condition and the requirement in spinning stage, not all fiber can both be used for spinning, and reason is that the length of some fiber is shorter.Therefore, some the time during processing, just cause the waste of some natural fabric such as wool, silk, cotton or fiber crops etc.Because the intrinsic property of these fibers is outstanding, therefore exploitation utilizes the new method of these fibers to have very big market potential again.Simultaneously, be not only textile industry, other many industry also need this class technology in new material, functionalized design or application facet.
Existing many prior aries attempt utilizing again described short length fiber, for example, US6,437,050B1 discloses the polymer that a kind of nano particle is formed, it prepares by dispersion copolymerization method, has the superficial layer that poly-(conjugated diene) examined and comprised to poly-(alkenyl benzene), and the diameter average-size is below the 100nm.CN94115873.X discloses a kind of from cotton or flax fibre, by chemical treatment in conjunction with low temperature drying and pulverizing and filtration, thereby prepare the method that average-size is the 2.5--10nm cellulose powder.The prior art of these U.S. and China has been instructed the specific process for preparing a few specific nanometer organic dust.But how the method for preparing nano-scale particle from various natural organic substances yet there are no open.
Usually organic material shows the draftability of high strength and height, and therefore required failure energy height adopts that traditional steel or iron pulverizer are very difficult crushes them/grind/be ground into small particle size.Simultaneously, traditional metal machine will produce big energy during milling, if mill for a long time, organic material is easy to be damaged.
Summary of the invention
The purpose of this invention is to provide a kind of method that natural organic substance is ground into nanometer stage material.
For realizing this purpose, the present invention utilizes several different crushing technologies to combine satisfying the different requirements in each stage, thereby a kind of new method that natural organic substance is ground into nanometer stage material is provided.Adopt this method, organic substance can be easily and is ground into the nano level superfine fiber grain effectively.This method comprises the following steps:
1. raw material preparing: adopt conventional equipment cleaning and dry natural organic substance.For example, can adopt any washing machine and drier on the market.
2. pulverize for the first time: adopt mechanical type pulverizer (as rotary mill) that organic substance is ground into small pieces.After this step, the length dimension of particle can reach 500 μ m.
3. pulverize for the second time: the product and the pure water in the 2nd step are mixed into suspension, and adopt professional ultrasonic disintegrator to pulverize.After pulverizing through this time, the organic granular in the suspension is below the size on diameter and the length all will be for 20 μ m.
4. pulverize for the third time: the suspension that contains particle that the 3rd step was obtained is fed in the nanometer collider, with described suspension separated into two parts, makes it collide and produce vibration mutually, and then makes described natural organic substance become nano-scale.After this step, the diameter dimension of particle will be less than 100nm, and length is less than 800nm.Can hit the size that pressure and collision time are controlled the gained particle by regulating magnetic.
The organic substance fiber grain of drying nano level then further needs the following step if desired.This step is:
5. prepare the dried fibres particle: adopt the nano particle of common spray dryer drying steps 4, obtain dry nanoscale organic substance fiber grain.
The accompanying drawing summary
Fig. 1 a is the wool fibre enlarged drawing, and diameter is about 25 μ m, and length is about 60-120mm.
Fig. 1 b is an enlarged drawing of pulverizing the described wool fibre in back for the first time, and length dimension is reduced to 0.5mm.
Fig. 1 c is an enlarged drawing of pulverizing the described wool fibre in back for the second time, and length and diameter dimension all are reduced to 20 μ m.
Fig. 1 d pulverizes the enlarged drawing of described wool fibre afterwards for the third time, and diameter dimension is reduced to 50nm, and length dimension is reduced to 200-800nm.
Fig. 1 e is the 3D SPM photo of wool fibre particle.
The continuous tow of Fig. 2 a fibroin silk, its diameter are 15-30 μ m.
Fig. 2 b is an enlarged drawing of pulverizing the described silk fiber in back for the first time, and length dimension is reduced to 0.5mm.
Fig. 2 c is an enlarged drawing of pulverizing the described silk fiber in back for the second time, and length and diameter dimension all are reduced to below the 20 μ m.
Fig. 2 d is the enlarged drawing of the nanoscale silk particle after pulverizing for the third time.
Fig. 3 a is an enlarged drawing of pulverizing the back cotton fiber for the first time, and length dimension is about 0.5mm.
Fig. 3 b is an enlarged drawing of pulverizing the described cotton fiber in back for the second time, and length and diameter dimension all are reduced to below the 20 μ m.
Fig. 3 c is an enlarged drawing of pulverizing the cotton particle of back nanoscale for the third time.
Fig. 4 a is an enlarged drawing of pulverizing back root of large-flowered skullcap particle for the first time, and length dimension is about 0.5mm.
Fig. 4 b is an enlarged drawing of pulverizing back root of large-flowered skullcap particle for the second time, and length and diameter dimension all are reduced to below the 20 μ m.
Fig. 4 c is an enlarged drawing of pulverizing the back nanoscale root of large-flowered skullcap for the third time.
Fig. 4 d shows the SEM photo that is deposited on the lip-deep nanoscale root of large-flowered skullcap of cotton fiber particle.
Preferred implementation describes in detail
As example, adopting length is about 60-120mm, and diameter is the wool fibre of about 25 μ m, pulverize according to the method described above, this wool fibre at the micrograph of different step shown in Fig. 1 a to Fig. 1 e.
Fig. 1 a shows length and is about 60-120mm, and diameter is the wool fibre of about 25 μ m.When carrying out step 1, this wool fibre must be wrapped in mesh bag.Can adopt any cleaning agent, remove grease on the wool fibre as lauryl sodium sulfate or anion surfactant.In this embodiment, at first in washing machine, add cleaning agent (as soap or dish washing agent etc.) and in big bathtub or washing machine, put into hot water (preferred 50-90 ℃), but do not stir with the submergence wool.Make wool in suds, leave standstill half an hour approximately.The washing machine rotation that is set to only circulate then adds clear water afterwards, once more rotation.At last, take out wool and it is carried out dried with conventional equipment.
It is about 0.5mm that Fig. 1 b shows the length dimension of pulverizing the back particle for the first time.In step 2, pulverize the described first time is coarse crushing.Can adopt a series of mechanical type pulverizer that the organic substance of step 1 is pulverized and be described undersized particle.For example, can adopt the miniature rotating disintegrator in this laboratory of FZ102 that wool fibre is ground into small fragment.
Fig. 1 c shows the wool fibre particle is ground into littler size, and the length and the diameter dimension of particle all are below the 20 μ m afterwards to pulverize (600W, 270 seconds) for the second time.In step 3, for further pulverizing, the coarse granule of step 2 is mixed into suspension mutually with pure water, and pulverizes with professional ultrasonic disintegrator.Can adopt multiple professional ultrasonic disintegrator in this step, as ultrasonic disintegrator JY92-II.Pulverizing power in output is under the 600W, and the circulation of ultrasonic disintegrator is set to turn round 3 seconds, stops 2 seconds.In this embodiment, adopted altogether 270 seconds.But should be according to pulverized organic material setting operation parameter.
Fig. 1 d shows and adopts collider at 1000kgf/cm
2The wool particle of pressure after pulverizing down once, its diameter dimension is below the 50nm, and length dimension is 200-800nm.In step 4, for carrying out final pulverizing, the mechanism that has adopted high pressure and vibration to combine.For example, adopt NT1500/5 nanometer collider that the wool particle is crushed into nano level fibrous material according to this mechanism design.Raw material are subjected to the high-pressure pump pressurization, and pass through the pressure piping system feeding in the nanometer collider.In the nanometer collider, raw material are divided into two parts, and these two parts collide and produce vibration mutually, thereby finish pulverizing at the moment.For example, the condition of work of machine is set pressure 1000kgf/cm
2, it is below the 100nm that the wool fibre particle can be crushed to diameter dimension.By regulating impact pressure and collision time, can control particle size.
Fig. 1 e shows the 3D SPM photo of wool fibre particle.In step 5, spray dryer is the equipment of choosing wantonly, only just needs when requiring dried particles.Can adopt multiple spray dryer.For example, can adopt Mini Spray Dryer, it is set to 2900W, 100 ℃ of temperature, compressed air 5bar.
Prepared wool fibre particle of the present invention, and its particle size has been measured.Test result can find in corresponding photo.
In addition, adopt the present invention natural organic substance to be ground into the method for nanometer stage material, the silk particle of nano-grade size, cotton particle and root of large-flowered skullcap particle have been obtained, their particle microphotos in different step are shown in respectively among the following figure: silk particle such as Fig. 2 a-Fig. 2 d, cotton particle such as Fig. 3 a-Fig. 3 c, and root of large-flowered skullcap particle such as Fig. 4 a-Fig. 4 d.
Method of the present invention is a kind of the associating to adopt different crushing technologies satisfying the requirement of different phase, thereby organic substance is crushed into the new method of nano-scale particle.By this method, can be easily and effectively organic substance is crushed into nano level superfine fibre particle.
The embodiment that should be appreciated that aforementioned wool, silk, cotton and the root of large-flowered skullcap is not intended to limit scope of the present invention.Method of the present invention can be used for any natural organic is crushed into nano-grade size.
The equipment specification that embodiment adopted that is used for pulverizing natural organic substance is as follows:
1.FZ102 laboratory micropulverizer
A. voltage 220V
B. motor power (output) 150W
C. rotary speed 1400rpm
D. sieve 0.5mm
2.JY92-II ultrasonic disintegrator
A. supply voltage 220V
B. power 650W
C. capacity 0.5-500ml
D. duty ratio 0.1-99%
3. collider
A. supply voltage 380V
B. power 1.5KW
C. maximum pressure 1500Mpa
D. heap(ed) capacity 5L/hr
4. spray dryer
A. supply voltage 380V
B. power 2900W
C. compressed air 5Bar
Claims (7)
1. natural organic substance is ground into the method for nanometer stage material, wherein said method comprises the following steps:
(1) raw material preparing: adopt conventional equipment cleaning natural organic substance to remove degrease and dry natural organic substance;
(2) pulverize for the first time: adopt standard machinery formula pulverizer that the natural organic substance of step 1 preparation is carried out coarse crushing, obtain the granule that length dimension is 500 μ m;
(3) pulverize for the second time: coarse granule and pure water that the 2nd step was obtained are mixed into suspension, and adopt professional ultrasonic disintegrator to carry out essence and pulverize, and obtaining diameter and length dimension all will be less than the particulate of 20 μ m;
(4) pulverize for the third time: the 3rd particulate that goes on foot in the suspension that obtains is fed in the nanometer collider, with described suspension separated into two parts, makes it collide and produce vibration mutually, and then make described natural organic substance become nano-scale.
2. the method that natural organic substance is ground into nanometer stage material according to claim 1, wherein said method further comprises the nano particle that adopts common spray dryer drying steps 4 to obtain, and obtains dry nanoscale organic substance fibrous material.
3. according to claim 1 natural organic substance is ground into the method for nanometer stage material, wherein said conventional equipment comprises any washing machine, drier and mesh bag.
4. according to claim 1 natural organic substance is ground into the method for nanometer stage material, wherein uses any cleaning agent that to remove grease in the step 1.
5. according to claim 4 natural organic substance is ground into the method for nanometer stage material, wherein said cleaning agent comprises soap and dish washing agent.
6. according to claim 1 natural organic substance is ground into the method for nanometer stage material, wherein said standard machinery formula pulverizer comprises rotary mill.
7. according to claim 1 natural organic substance is ground into the method for nanometer stage material, wherein said professional ultrasonic disintegrator comprises JY92-II.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| HK02109161.2 | 2002-12-18 | ||
| HK02109161 | 2002-12-18 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1735718A CN1735718A (en) | 2006-02-15 |
| CN100374629C true CN100374629C (en) | 2008-03-12 |
Family
ID=32587174
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2003801062645A Expired - Lifetime CN100374629C (en) | 2002-12-18 | 2003-12-18 | Method for pulverizing natural organic matter into nano-grade fiber material |
Country Status (3)
| Country | Link |
|---|---|
| CN (1) | CN100374629C (en) |
| AU (1) | AU2003294605A1 (en) |
| WO (1) | WO2004055250A1 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100344824C (en) * | 2004-10-18 | 2007-10-24 | 香港理工大学 | Functional finishing adjuvant for fabric, its preparation and application process |
| JP5144086B2 (en) * | 2007-02-20 | 2013-02-13 | 独立行政法人物質・材料研究機構 | Dispersion or grinding apparatus and dispersion or grinding method |
| CN109963978B (en) * | 2016-11-25 | 2022-02-08 | 帝人富瑞特株式会社 | Fiber powder and aqueous dispersion thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1416745A (en) * | 1922-01-12 | 1922-05-23 | Peters James Arthur | Motor cycle |
| CN1104647A (en) * | 1994-09-16 | 1995-07-05 | 中国科学院广州化学研究所 | Manufacture of nm avicel powder by solvent process |
| JPH10273809A (en) * | 1997-03-28 | 1998-10-13 | Tosuko Kk | Powdery wool fiber and its production |
| CN1334272A (en) * | 2000-07-18 | 2002-02-06 | 中国科学院广州化学研究所 | Nm-class microcrystal cellulose and its preparing process |
| US6437050B1 (en) * | 2001-10-04 | 2002-08-20 | Bridgestone Corporation | Nano-particle preparation and applications |
| CN1369508A (en) * | 2001-02-13 | 2002-09-18 | 中国科学院广州化学研究所 | Nano microcrystal cellulose with crystal form of cellulose II and its preparing process |
| CN1377699A (en) * | 2002-04-22 | 2002-11-06 | 武汉大学 | Nano aloe and its preparing method and use |
| CN1383762A (en) * | 2001-05-09 | 2002-12-11 | 汪景山 | Ultramicrobe powder and its prepn and use |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1416745A (en) * | 2001-11-07 | 2003-05-14 | 焦柏忠 | Nanometer level carrot product and its production process |
-
2003
- 2003-12-18 CN CNB2003801062645A patent/CN100374629C/en not_active Expired - Lifetime
- 2003-12-18 WO PCT/CN2003/001083 patent/WO2004055250A1/en not_active Application Discontinuation
- 2003-12-18 AU AU2003294605A patent/AU2003294605A1/en not_active Abandoned
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1416745A (en) * | 1922-01-12 | 1922-05-23 | Peters James Arthur | Motor cycle |
| CN1104647A (en) * | 1994-09-16 | 1995-07-05 | 中国科学院广州化学研究所 | Manufacture of nm avicel powder by solvent process |
| JPH10273809A (en) * | 1997-03-28 | 1998-10-13 | Tosuko Kk | Powdery wool fiber and its production |
| CN1334272A (en) * | 2000-07-18 | 2002-02-06 | 中国科学院广州化学研究所 | Nm-class microcrystal cellulose and its preparing process |
| CN1369508A (en) * | 2001-02-13 | 2002-09-18 | 中国科学院广州化学研究所 | Nano microcrystal cellulose with crystal form of cellulose II and its preparing process |
| CN1383762A (en) * | 2001-05-09 | 2002-12-11 | 汪景山 | Ultramicrobe powder and its prepn and use |
| US6437050B1 (en) * | 2001-10-04 | 2002-08-20 | Bridgestone Corporation | Nano-particle preparation and applications |
| CN1377699A (en) * | 2002-04-22 | 2002-11-06 | 武汉大学 | Nano aloe and its preparing method and use |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2004055250A1 (en) | 2004-07-01 |
| AU2003294605A1 (en) | 2004-07-09 |
| CN1735718A (en) | 2006-02-15 |
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