CN102505387B - Preparing device for keratin original fibers with forked head ends and method - Google Patents
Preparing device for keratin original fibers with forked head ends and method Download PDFInfo
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- CN102505387B CN102505387B CN 201110357345 CN201110357345A CN102505387B CN 102505387 B CN102505387 B CN 102505387B CN 201110357345 CN201110357345 CN 201110357345 CN 201110357345 A CN201110357345 A CN 201110357345A CN 102505387 B CN102505387 B CN 102505387B
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Abstract
The invention provides a preparing device for keratin original fibers with forked head ends and a method. The preparation method for keratin original fibers is characterized in that specific steps include adding formic acid solution into a container of a differential type mechanical stirring device, feeding spindle-shaped keratin original fibers with the diameter ranging from 3mum to 5mum and thelength ranging from 80mum to 120mum into the formic acid solution, and obtaining the keratin original fibers with the forked head ends by means of centrifugation or filtration under joint effects of ultrasonic oscillation and differential type mechanical stirring. As the preparation method adopts differential stirring, the force and the probability of forking the head ends of the spindle-shaped animal keratin original fibers are increased, yield of the forked original fibers is improved effectively, and the average number of the forked head ends and superficial area can be directly increased by 20% at least.
Description
Technical field
The present invention relates to the former slim technology of preparing of head end bifurcated, especially adopt comb sheet differential type mechanical agitation preparation method, and with former slim being applied in the keratin homogeneous composite membrane in the natural hair of coming from of gained.
Background technology
Profiled filament can be divided into two kinds, and first global sections is the fiber of abnormity, for example triangle fiber, I-shaped fiber etc.It two is the cross section special-shaped fibers of head end (or on length direction), for example bone (dumbbell) shape fiber, laemodipodiform fiber, bifurcated fiber etc.
By retrieval, the relevant patent of fiber of first kind global sections abnormity and preparation method thereof has: application number is to have described when the melt spinning of high polymer in 201020200715.9 the patent of invention " the special-shaped spinnerets of three leaves ", trilobal is made in the shape design of spinneret orifice, obtained the big trilobal profiled filament of specific area.Application number is to have reported by profile spinneret in 200810124782.4 the patent of invention " a kind of polypropylene profiled fiber and silk spraying method thereof " to extrude, and the as-spun fibre crystal region below spinnerets is arranged outside annular cross blowing system.The cross sectional shape that forms fiber is C shape or circle hollow shape or trilobal or cross or M shape or triangle, and the fibre section degree of profile is 20-55%.More than the patent report of relevant profiled filament, all be by changing the spinneret orifice shape or change the fibre section by additive, obtaining the profiled filament that surface area increases, but in the longitudinal direction, especially be still flat end at head end.If it as the fortifying fibre in the composite, is still occurred stress easily and concentrates, cause composite material toughness to reduce.
The relevant patent of second class profiled filament and preparation method thereof has: application number is disclosed a kind of profiled filament in 201010520316.5 the patent of invention " the special-shaped concrete in heavy in section strengthens modified polypropylene fiber and production method thereof ", its cross section is flat, the ratio of interface length and width is 3-4:1, particularly be the ridge design shape at fiber surface, the fibre section is long-pending to be 0.1mm
2-1mm
2, fibre length is 15-30mm, and the component of polymer of fiber accounts for the 90-100% of total weight of fiber, and additive accounts for the 0-10% of total weight of fiber.Beginning of the nineties in 19th century particularly, (the Los Alamos National Lab of U.S. Los Alamos National Laboratories, LANL) carried out bone shape (dumb-bell shape) fiber applications in the system research of composite, that reports among the U. S. application patent WO 99/41440 that applies for " Reinforced Composites Including Bone-Shaped Short Fibers " is a kind of for the steel fibre that strengthens toughness reinforcing cement-based material, its length is 25mm, the middle part fibre diameter is 0.84mm, and the head end diameter is 1.6mm.Find that the bone shape head end of steel fibre can improve intensity and the toughness of cement material effectively, has improved 40% and 260% than the fibre-reinforced cement of ordinary steel respectively.But above-mentioned fiber is the fiber of macro-size, although played toughening effect in composite, the non-ecology because of the character of material own can't be applied to the toughness reinforcing of biological species material.
Since the keratin that can obtain at present former slim all be its original structure form, namely two is thin, central thick spindle is former slim.Therefore, in actual reinforced composite, it a little less than gripping effect of head end, is easy to slippage and destruction as strengthening body.If can be the branching shape structure by the bionical head end that is prepared into, then improve the gripping of its head end greatly and subdue the stress concentration phenomenon, thereby reach enhancing, toughening effect to this composite, especially toughness reinforcing.
Summary of the invention
The object of the present invention is to provide a kind of former slim preparation method of keratin and device of head end bifurcated, the former slim enhancing body that can be used as the homojunction combined material of keratin of the keratin of the head end bifurcated of gained strengthens with toughness reinforcing composite.
In order to achieve the above object, the invention provides a kind of differential type mechanical stirring device, it is characterized in that, comprise at least one stirring rod of being located in the container, described stirring rod comprises first drive link and is located at the second interior drive link of first drive link, one end of first drive link connects to go up to stir to be combed, the other end connects travelling gear, travelling gear connects to go up to stir combs stepper motor, one end of second drive link connects to stir down to be combed, stirring comb stepper motor under the other end connects, the last comb that stirs is relative with the comb sheet of following stirring comb.
Preferably, described container is located on the sample bench, and described sample bench connects stepper motor by turning cylinder.
Preferably, number and the spacing of the described size that goes up the stirring comb and stir comb down, shape, comb sheet are all equal.
Preferably, the described number that stirs comb and stir the comb sheet of comb down that goes up is all 1-12.
The present invention also provides a kind of keratin of head end bifurcated former slim preparation method, it is characterized in that, concrete steps are: formic acid solution is joined in the container of above-mentioned differential type mechanical stirring device, be that 3-5 μ m, length are in the described formic acid solution of the former slim input of spindle keratin of 80-120 μ m with diameter, under supersonic oscillations and the acting in conjunction of differential type mechanical agitation, centrifugal or to filter the keratin obtain the head end bifurcated former slim.
Described diameter is that to be that the spindle keratin of 80-120 μ m is former slimly make for the disclosed method of Chinese patent that can be 200910047254.8 by application number, name is called " method of fibril shape structure in a kind of separation and Extraction natural keratin fiber " for 3-5 μ m, length.
Preferably, described spindle keratin is former slim by extracting in the natural keratin fiber.
More preferably, described natural keratin fiber be that wool, yak hair, people are sent out, cashmere, camel hair, horsehair or ox hair.
Preferably, the temperature of described formic acid solution is 10-40 ℃, and volumetric concentration is 70-98%.
Preferably, the power of described supersonic oscillations is 50-150W, and the time is 5-30min.
Preferably, comb and the following direction of rotation that stirs comb are stirred in going up of described differential type mechanical stirring device, and rotational frequency is identical, is 0.01-2Hz, and rotational angle is identical, is 30o-1800o.
Preferably, the rotating speed of the sample bench of described differential type mechanical stirring device is 0-10rpm.
Preferably, described centrifugal temperature is 20 ℃, and centrifugal speed is 6000-12000rpm, and the time is 15-30min.
Compared with prior art, characteristics of the present invention and beneficial effect are as follows:
(a) owing to adopt the stirring of differential type, strengthened dynamics and probability to the former slim head end bifurcated of fusiform animal ceratin, can effectively increase the former slim yield of bifurcated, the average bifurcated number of head end and surface area surface area can directly increase more than 20%;
(b) owing to adopt the stirring comb of many comb sheets, strengthened to a greater extent fusiform animal ceratin former slim effect dynamics and probability, except improving feature in above-mentioned (a) widely, can also increase the average bifurcated length of head end;
(c) gripping of fibril point, section increase, and the surface area increment rate increases, and are conducive to stress and evenly distribute and high effective adhesive and gripping; Former slim bifurcated at head end strengthens the lock knot to stressed section of matrix, prevents the matrix cracking expansion, improves intensity and toughness, the especially toughness of composite; Its enhancing and toughness reinforcing mechanism are that the root bifurcated makes the head end of fiber have the mechanical keying action of bigger specific area and branch, grip point and gripping area so not only increase effectively, and the stress that significantly reduces head end is concentrated.
(d) the former slim and solution of keratin of the present invention all comes from natural hair fibers, as wool, yak hair, people send out, cashmere, camel hair, horsehair or ox hair etc., have abundant raw material, with low cost, processing characteristics such as simple, and the head end bifurcated of gained former slim be nontoxic, harmless keratin crystal whisker.It strengthens toughness reinforcing composite membrane and can be used for bio-medical, institutional framework material.
Description of drawings
Fig. 1 is differential type mechanical stirring device structural representation;
The head end bifurcated fibril bulk optics microphotograph that Fig. 2 obtains for the inventive method.
The specific embodiment
Specify the present invention below in conjunction with embodiment.Embodiment helps to understand the present invention, but does not limit content of the present invention.
Embodiment 1
As shown in Figure 1, be differential type mechanical stirring device structural representation, described differential type mechanical stirring device, comprise at least one stirring rod of being located in the container 11, described stirring rod comprises first drive link 2 and is located at second drive link 6 in first drive link 2, one end of first drive link 2 connects to go up to stir combs 1, the other end connects travelling gear 3, travelling gear 3 connects to go up to stir combs stepper motor 4, one end of second drive link 6 connects to stir down combs 5, stirring comb stepper motor 7 under the other end connects, the last comb 1 that stirs is relative with the comb sheet of following stirring comb 5.Container 13 is located on the sample bench 8, and described sample bench 8 connects stepper motor 9 by turning cylinder.Number and the spacing of the described size that go up to stir comb 1 and stir comb 2 down, shape, comb sheet are all equal.The last number that stirs the comb sheet of comb 1 and following stirring comb 2 is 1-12.
Embodiment 2
The wool of cleaning oven dry being cut into the long segment of fiber of 5mm, immersing in 98% formic acid and boil 10min, is that the ultrasonic oscillation 10min of 400W and ultrasonic oscillation 20min that power is 200W finish and scale through overpower successively.The solid-to-liquid ratio of wool with 1g/100ml of scaling is immersed in 98% formic acid, is that 20kHz, power are that 200W carries out ultrasonic oscillation 5h with the frequency in 20 ℃ of waters bath with thermostatic control.Remove undecomposed wool fibre with 100 purpose screen filtrations afterwards, again through 400 eye mesh screens, the spindle that obtains diameter and be 4.8 μ m, length and be 120.0 μ m is former slim with filtrate.
Adopt embodiment 1 described differential type mechanical stirring device, be that 20 ℃, volumetric concentration are that 85% formic acid solution 10 places container 13 with temperature, the former slim concentration that is put into of spindle of getting section diameter and be 4.8 μ m, length and be 120.0 μ m wools is in the formic acid solution 10, setting the supersonic oscillations frequency is 20kHz, and power is 50W; Last comb 1 and the following direction of rotation that stirs comb 2 of stirring, stirring frequency is all 0.05Hz, and rotational angle is all 1800o, adopts two stirring rod, and the last comb 1 that stirs is all 2 with the number that stirs the comb sheet of comb 2 down; It is 30min that supersonic oscillations and mechanical differential type stir the acting in conjunction time.The setting centrifuge speed is 6000rpm, and the time is 30min, collects the former slim of head end bifurcated in the mixed liquor.The yield of bifurcated fibril is 99%, and through microscopic, calculating its surface area increment rate is 31%.
Embodiment 3
The cashmere of cleaning oven dry is cut into the long segment of fiber of 5mm, and with embodiment 1 in consistent to the former slim preparation method of wool and step.The spindle that obtains diameter and be 3.0 μ m, length and be 105.5 μ m is former slim.
Adopt embodiment 1 described differential type mechanical stirring device, be that 40 ℃, volumetric concentration are that 70% formic acid solution 10 places container 13 with temperature, getting section diameter is that 3.0 μ m, length are former slim being put in the formic acid solution 10 of spindle of the cashmere of 105.5 μ m, setting the supersonic oscillations frequency is 20kHz, and power is 150W; Last comb 1 and the following direction of rotation that stirs comb 2 of stirring, stirring frequency is all 2Hz, and rotational angle is all 30o, adopts 6 stirring rod, and the last comb 1 that stirs is all 4 with the number that stirs the comb sheet of comb 2 down, and the sample bench rotating speed is 200rpm; It is 10min that supersonic oscillations and mechanical differential type stir the acting in conjunction time.The setting centrifuge speed is 12000rpm, and the time is 15min, collects the former slim of head end bifurcated in the mixed liquor.The yield of bifurcated fibril is 96%, and through microscopic, calculating the surface area increment rate is 29%.
Embodiment 4
The yak hair of cleaning oven dry is cut into the long segment of fiber of 5mm, and with embodiment 1 in consistent to the former slim preparation method of wool and step.The spindle that obtains diameter and be 4.3 μ m, length and be 89.4 μ m is former slim.
Adopt embodiment 1 described differential type mechanical stirring device, be that 30 ℃, volumetric concentration are that 80% formic acid solution 10 places container 13 with temperature, the diameter of getting the part yak hair is that 4.3 μ m, length are former slim being put in the formic acid solution 10 of spindle of 89.4 μ m, setting the supersonic oscillations frequency is 20kHz, and power is 100W; Last comb 1 and the following direction of rotation that stirs comb 2 of stirring, stirring frequency is all 1Hz, and rotational angle is all 1080o, adopts 4 rods, and the last comb 1 that stirs is all 8 with the number that stirs the comb sheet of comb 2 down; It is 20min that supersonic oscillations and mechanical differential type stir the acting in conjunction time.The setting centrifuge speed is 8000rpm, and the time is 25min, collects the former slim of head end bifurcated in the mixed liquor.The yield of bifurcated fibril is 94%, and its surface area increment rate is 23%.
Embodiment 5
The people's hair clipper that to clean oven dry become the long segment of fiber of 5mm, and with embodiment 1 in consistent to the former slim preparation method of wool and step.The spindle that obtains diameter and be 4.7 μ m, length and be 114.6 μ m is former slim.
Adopt embodiment 1 described differential type mechanical stirring device, be that 10 ℃, volumetric concentration are that 90% formic acid solution 10 places container 13 with temperature, getting the diameter that groups of people send out is that 4.7 μ m, length are former slim being put in the formic acid solution 10 of spindle of 114.6 μ m, setting the supersonic oscillations frequency is 20kHz, and power is 100W; Last comb 1 and the following direction of rotation that stirs comb 2 of stirring, stirring frequency is all 1.5Hz, and rotational angle is all 720o, adopts 4 stirring rod, and the last comb 1 that stirs is all 12 with the number that stirs the comb sheet of comb 2 down; It is 5min that supersonic oscillations and mechanical differential type stir the acting in conjunction time.The setting centrifuge speed is 10000rpm, and the time is 20min, collects the former slim of head end bifurcated in the mixed liquor.The yield of bifurcated fibril is 94%, and through microscopic, calculating the surface area increment rate is 24%.
Below only being part example of the present invention, is not that the present invention is done any pro forma restriction.Every technical scheme according to the present invention is made other various corresponding simple modification, equivalent variations or modification, all should belong to the protection domain of claim of the present invention.
The former slim preparation condition of the bifurcated of embodiment 2-embodiment 5 and result thereof
| Parameter and result | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Former slim source | Wool | Cashmere | Yak hair | The people sends out |
| Former slim size (diameter/length, μ m) | 4.8/120.0 | 3.0/105.5 | 4.3/89.4 | 4.7/114.6 |
| The formic acid solution temperature (℃) | 20 | 40 | 30 | 10 |
| Formic acid solution volumetric concentration (%) | 85 | 70 | 80 | 90 |
| Ultrasonic power (W) | 50 | 150 | 100 | 100 |
| The stirring rod number | 2 | 6 | 4 | 4 |
| Stir angle of rotation (o) | 1800 | 30 | 1080 | 720 |
| Stir comb comb sheet number | 2 | 4 | 8 | 12 |
| Stirring frequency (Hz) | 0.05 | 2 | 1 | 1.5 |
| Sample bench rotating speed (rpm) | 0 | 10 | 0 | 0 |
| The combined treatment time (min) | 15 | 25 | 10 | 5 |
| Centrifugal speed (rpm) | 6000 | 12000 | 8000 | 10000 |
| Centrifugation time (min) | 30 | 15 | 25 | 20 |
| The former slim yield of bifurcated (%) | 99 | 96 | 94 | 94 |
| The average bifurcated number of head end | 2.4 | 2.2 | 2.0 | 2.3 |
| Average bifurcated length (μ m) | 9.5 | 8.6 | 9.1 | 9.0 |
| Surface area increment rate (%) | 31 | 29 | 23 | 24 |
Claims (9)
1. differential type mechanical stirring device, it is characterized in that, comprise at least one stirring rod of being located in the container (11), described stirring rod comprises first drive link (2) and is located at interior second drive link (6) of first drive link (2), one end of first drive link (2) connects to go up to stir combs (1), the other end connects travelling gear (3), stir comb stepper motor (4) in travelling gear (3) connection, one end of second drive link (6) connects to stir down combs (5), stirring comb stepper motor (7) under the other end connects, the last comb (1) that stirs is relative with the comb sheet of following stirring comb (5).
2. differential type mechanical stirring device as claimed in claim 1 is characterized in that, described container (11) is located on the sample bench (8), and described sample bench (8) connects stepper motor (9) by turning cylinder.
3. differential type mechanical stirring device as claimed in claim 1 is characterized in that, number and the spacing of the described size that goes up stirring comb (1) and stir comb (5) down, shape, comb sheet are all equal.
4. differential type mechanical stirring device as claimed in claim 1 is characterized in that, the described number that stirs comb (1) and stir the comb sheet of comb (5) down that goes up is all 2-12.
5. the former slim preparation method of the keratin of a head end bifurcated, it is characterized in that, concrete steps are: formic acid solution is joined in the container (11) of each described differential type mechanical stirring device of claim 1-4, be that 3-5 μ m, length are in the described formic acid solution of the former slim input of spindle keratin of 80-120 μ m with diameter, under supersonic oscillations and the acting in conjunction of differential type mechanical agitation, the centrifugal keratin that obtains the head end bifurcated is former slim.
6. the former slim preparation method of the keratin of head end bifurcated as claimed in claim 5 is characterized in that, described spindle keratin is former slim by extracting in the natural keratin fiber.
7. the former slim preparation method of the keratin of head end bifurcated as claimed in claim 5 is characterized in that, the temperature of described formic acid solution is 10-40 ℃, and volumetric concentration is 70-98%.
8. the former slim preparation method of the keratin of head end bifurcated as claimed in claim 5 is characterized in that, the power of described supersonic oscillations is 50-150W, and the time is 5-30min.
9. the former slim preparation method of the keratin of head end bifurcated as claimed in claim 5, it is characterized in that, comb (1) and the following direction of rotation that stirs comb (5) are stirred in going up of described differential type mechanical stirring device, rotational frequency is identical, be 0.01-2Hz, rotational angle is identical, is 30o-1800o.
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| CN 201110357345 CN102505387B (en) | 2011-11-13 | 2011-11-13 | Preparing device for keratin original fibers with forked head ends and method |
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|---|---|---|---|
| CN 201110357345 CN102505387B (en) | 2011-11-13 | 2011-11-13 | Preparing device for keratin original fibers with forked head ends and method |
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| CN102505387A CN102505387A (en) | 2012-06-20 |
| CN102505387B true CN102505387B (en) | 2013-10-09 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1854531A1 (en) * | 2005-03-02 | 2007-11-14 | Kabushiki Kaisha Kobe Seiko Sho (Kobe Steel, Ltd.) | Kneading machine and kneading control method |
| CN201760246U (en) * | 2010-08-17 | 2011-03-16 | 山东万盛环保科技发展有限公司 | Sectional acid mixer |
| CN201823523U (en) * | 2010-09-14 | 2011-05-11 | 苏州工业园区南华生物科技有限公司 | Coaxial stirrer for chemical-reaction kettle |
-
2011
- 2011-11-13 CN CN 201110357345 patent/CN102505387B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1854531A1 (en) * | 2005-03-02 | 2007-11-14 | Kabushiki Kaisha Kobe Seiko Sho (Kobe Steel, Ltd.) | Kneading machine and kneading control method |
| CN201760246U (en) * | 2010-08-17 | 2011-03-16 | 山东万盛环保科技发展有限公司 | Sectional acid mixer |
| CN201823523U (en) * | 2010-09-14 | 2011-05-11 | 苏州工业园区南华生物科技有限公司 | Coaxial stirrer for chemical-reaction kettle |
Non-Patent Citations (2)
| Title |
|---|
| 最新的搅拌混合技术;赵青;《日用化学工业》;20011031(第5期);第46-48页 * |
| 赵青.最新的搅拌混合技术.《日用化学工业》.2001,(第5期),第46-48页. |
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