CN107603242A - A kind of preparation method of bionical shell pearl material - Google Patents
A kind of preparation method of bionical shell pearl material Download PDFInfo
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- CN107603242A CN107603242A CN201710933513.1A CN201710933513A CN107603242A CN 107603242 A CN107603242 A CN 107603242A CN 201710933513 A CN201710933513 A CN 201710933513A CN 107603242 A CN107603242 A CN 107603242A
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Abstract
The present invention relates to a kind of preparation method of bionical shell pearl material, belong to materials processing technology field.The present invention takes hydriopsis cumingii to obtain shell fragment, after shell fragment is mixed into immersion with liquor natrii hypochloritis, must handle shell matrix material；Boiled silk is mixed with ethanol solution, heating water bath is simultaneously cooled to room temperature, filter to get filtrate, calcium chloride solution is mixed with filtrate, obtain mixed liquor and rotary evaporated to dryness, crush to obtain silk extract gel particle, weigh deionized water, silk extract gel particle, sodium carbonate liquor mixes, ultrasonic disperse obtains dispersion liquid, in mass ratio, processing shell matrix material is dipped in dispersion liquid, immersion treatment and mineralising processing, standing is cooled to room temperature and filtered and to obtain filter residue, after deionized water rinsing, dry in an oven to constant weight again, a kind of bionical shell pearl material can be prepared into.
Description
Technical field
The present invention relates to a kind of preparation method of bionical shell pearl material, belong to materials processing technology field.
Background technology
There is many sclerous tissueses with some specific functions, such as shell, coral, bone and tooth etc. in organism.
Substantial amounts of inorganic matter, such as calcium carbonate, calcium phosphate and silica are included in these sclerous tissueses, we are referred to as them to make a living
Thing mineral.
In nature, many biogenic minerals form answering with organic-inorganic structure by the mineralising regulating and controlling effect of itself
Condensation material.And structure orderly in biomaterial and accurate assembling mode impart the unique feature of biogenic mineral, such as
The properties such as the mechanics of almost Perfect, optics and magnetics.Therefore, biomaterial is with than itself simple composition compound and commonly
The obvious excellent characteristic of artificial material with chemistry similar composition.Wherein, shell nacre is due to its outstanding mechanical property
Cause the extensive concern of the area research person such as material and chemistry, it has been found that shell can regulate and control to form height by itself mineralising
Orderly organo-mineral complexing structure is spent, wherein inorganic phase is calcium carbonate, and organic phase then includes chitin, protein and one
A little large biological molecules.Exactly this organo-mineral complexing structure imparts the outstanding fracture toughness of shell, and intensity is rigid and hard
Degree, therefore bionical shell composite is prepared into for the research emphasis of different field worker.Derive from shell knot at present
The various composites of structure are synthesized in the lab, and some of which is being built, and packaging, coating, and field of functional materials have very
Big directive significance and application potential.But excellent properties are prepared especially based on calcium carbonate with simple and environmentally-friendly means
The preparation of the composite of body still has some problems, and mechanism therein is not fully set forth clear, therefore bionical shellfish yet
The research that shell prepares high performance material has huge scientific meaning and application value.
Biomineralization refers in the case where organic substrate participates in and regulates and controls, and the forming process of biogenic mineral in vivo, participates in
Organic substrate can be it is intracellular can also be it is extracellular, this is relevant with the site into ore deposit, with general mineralising most very much not
Be it be biology at specific position, under certain physical and chemical condition, in biological organic material (cell, organic group
Matter) participation, control or under the influence of, by the ion transit in solution be solid phase mineral process.Another significant difference is logical
The interaction of organic molecule and inorganic ions in interface is crossed, nucleation and the growth of inorganic matter are controlled from molecular level, from
And make biomineralization that there are various structures and assembling mode from nanometer to micron.
The pattern for the strict regulation and control inorganic phase of effect that biogenic mineral passes through organic matter, crystal formation, size and orientation, form height
Orderly organic/inorganic composite material is spent, therefore there is mysterious property.In nature, many biogenic minerals have rule
Structure and mysterious mechanical property.Wherein shell nacre due to its unique optics and mechanical property it is wide by people
General research, its outstanding intensity, toughness and hardness are then largely attributed to the fact that calcium carbonate and organic matter alternating in nacre
The higher order structures of formation.Therefore bionical shellfish material work becomes a big focus and has very big finger in many fields
Lead meaning and application value.
The content of the invention
The technical problems to be solved by the invention：The bionical shell nacre material mechanical performance prepared for prior art
A kind of the problem of existing defects, there is provided preparation method of bionical shell pearl material.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
（1）Take hydriopsis cumingii and cutting of polishing, obtain the wide shell fragments of the long 10mm of 20mm, in mass ratio 1：10, by shell fragment with
Liquor natrii hypochloritis is stirred, and filter cake is filtered to obtain after immersion, washing, dries, must handle shell matrix material；
（2）In mass ratio 1：8, boiled silk and ethanol solution are stirred, heating water bath and stand be cooled to room temperature, filter
Filtrate, in mass ratio 1：5, calcium chloride solution and filtrate are stirred, obtain mixed liquor；
（3）By mixed liquor rotary evaporated to dryness, silk extract gel particle is crushed to obtain, is counted in parts by weight, weigh 45~50 parts respectively
Deionized water, 10~15 parts of silk extract gel particles, 10~15 parts of sodium carbonate liquors of mass fraction 5% are stirred, ultrasonic disperse
10~15min, obtain dispersion liquid；
（4）In mass ratio 1：8, processing shell matrix material is dipped in dispersion liquid, soaks and mineralising is handled, stand cooling simultaneously
Filter residue is filtered to obtain, washing, is dried, you can be prepared into a kind of bionical shell pearl material.
Step（1）Described liquor natrii hypochloritis's mass fraction is 5%.
Step（3）Described rotating evaporation temperature is 45~50 DEG C.
Step（4）Described mineralising treatment temperature is 45~50 DEG C.
Compared with other method, advantageous effects are the present invention：
（1）The present invention causes strand by preparing silk protein liquid and rotary evaporated to dryness by the foldable structure of fibroin
It is partially oriented, assembled by the forming core dependence of foldable structure, the presoma for forming bionical shellfish material tends to absorption and existed
The oriented crystalline region of fibroin macromolecular, so as to form the bionical shell pearl material being stabilized, make bionical shell pearl
Material has excellent mechanical property；
（2）The present invention is that matrix is deposited by shellfish material, can be preferentially adsorbed on by the functional group in organic matter
Shell matrix surface, induced orientation form controllable crystallization, make the shell pearl material of preparation have excellent intensity and fracture
Toughness, then under fibroin albumen and inorganic particle compound action, by organic-inorganic interface composite behaviour, be greatly enhanced multiple
Intensity of the condensation material on parallel to in-plane, the inorganic phase of high-sequential arrangement can absorbing load power immediately, lift material
The hardness and rigidity of material.
Embodiment
Hydriopsis cumingii is taken, its shell is cleaned and cutting of polishing, obtains the wide shell fragments of the long 10mm of 20mm, in mass ratio 1：
10, shell fragment and the liquor natrii hypochloritis of mass fraction 5% are stirred, soak 3~5h after, filter filter cake and spend from
Sub- water rinses 3~5 times, must handle shell matrix material；In mass ratio 1：8, boiled silk and the ethanol of mass fraction 70% is molten
Liquid is stirred, at 75~80 DEG C heating water bath and stand be cooled to room temperature, filter to get filtrate, in mass ratio 1：5, by quality
The calcium chloride solution of fraction 10% is stirred with filtrate, is obtained mixed liquor and is placed at 45~50 DEG C, rotary evaporated to dryness, crushes
Silk extract gel particle, is counted in parts by weight, respectively weigh 45~50 parts of deionized waters, 10~15 parts of silk extract gel particles, 10~
15 parts of sodium carbonate liquors of mass fraction 5% are stirred, and 10~15min of ultrasonic disperse, obtains dispersion liquid under 200~300W, presses
Mass ratio 1：8, processing shell matrix material is dipped in dispersion liquid, immersion treatment is placed in mineralising processing 3 at 45~50 DEG C
~5h, standing is cooled to room temperature and filtered and to obtain filter residue, after deionized water rinsing 3~5 times, then is done in 105~110 DEG C of baking ovens
It is dry to constant weight, you can be prepared into a kind of bionical shell pearl material.
Example 1
Hydriopsis cumingii is taken, its shell is cleaned and cutting of polishing, obtains the wide shell fragments of the long 10mm of 20mm, in mass ratio 1：10, will
Shell fragment is stirred with the liquor natrii hypochloritis of mass fraction 5%, after soaking 3h, filters filter cake and to use deionized water rinsing
3 times, shell matrix material must be handled；In mass ratio 1：8, boiled silk and the ethanol solution of mass fraction 70% are stirred,
At 75 DEG C heating water bath and stand be cooled to room temperature, filter to get filtrate, in mass ratio 1：5, by the calcium chloride of mass fraction 10%
Solution is stirred with filtrate, is obtained mixed liquor and is placed at 45 DEG C, rotary evaporated to dryness, crushes to obtain silk extract gel particle, by weight
Number meter is measured, weighs 45 parts of deionized waters, 10 parts of silk extract gel particles, the 10 parts of sodium carbonate liquor of mass fraction 5% stirrings respectively
Mixing, the ultrasonic disperse 10min under 200W, obtains dispersion liquid, in mass ratio 1：8, processing shell matrix material is dipped to scattered
In liquid, immersion treatment is placed in mineralising at 45 DEG C and handles 3h, and standing is cooled to room temperature and filtered and to obtain filter residue, uses deionized water rinsing
After 3 times, then dried in 105 DEG C of baking ovens to constant weight, you can be prepared into a kind of bionical shell pearl material.
Example 2
Hydriopsis cumingii is taken, its shell is cleaned and cutting of polishing, obtains the wide shell fragments of the long 10mm of 20mm, in mass ratio 1：10, will
Shell fragment is stirred with the liquor natrii hypochloritis of mass fraction 5%, after soaking 4h, filters filter cake and to use deionized water rinsing
4 times, shell matrix material must be handled；In mass ratio 1：8, boiled silk and the ethanol solution of mass fraction 70% are stirred,
At 78 DEG C heating water bath and stand be cooled to room temperature, filter to get filtrate, in mass ratio 1：5, by the calcium chloride of mass fraction 10%
Solution is stirred with filtrate, is obtained mixed liquor and is placed at 48 DEG C, rotary evaporated to dryness, crushes to obtain silk extract gel particle, by weight
Number meter is measured, weighs 48 parts of deionized waters, 12 parts of silk extract gel particles, the 12 parts of sodium carbonate liquor of mass fraction 5% stirrings respectively
Mixing, the ultrasonic disperse 12min under 250W, obtains dispersion liquid, in mass ratio 1：8, processing shell matrix material is dipped to scattered
In liquid, immersion treatment is placed in mineralising at 47 DEG C and handles 4h, and standing is cooled to room temperature and filtered and to obtain filter residue, uses deionized water rinsing
After 4 times, then dried in 108 DEG C of baking ovens to constant weight, you can be prepared into a kind of bionical shell pearl material.
Example 3
Hydriopsis cumingii is taken, its shell is cleaned and cutting of polishing, obtains the wide shell fragments of the long 10mm of 20mm, in mass ratio 1：10, will
Shell fragment is stirred with the liquor natrii hypochloritis of mass fraction 5%, after soaking 5h, filters filter cake and to use deionized water rinsing
5 times, shell matrix material must be handled；In mass ratio 1：8, boiled silk and the ethanol solution of mass fraction 70% are stirred,
At 80 DEG C heating water bath and stand be cooled to room temperature, filter to get filtrate, in mass ratio 1：5, by the calcium chloride of mass fraction 10%
Solution is stirred with filtrate, is obtained mixed liquor and is placed at 50 DEG C, rotary evaporated to dryness, crushes to obtain silk extract gel particle, by weight
Number meter is measured, weighs 50 parts of deionized waters, 15 parts of silk extract gel particles, the 15 parts of sodium carbonate liquor of mass fraction 5% stirrings respectively
Mixing, the ultrasonic disperse 15min under 300W, obtains dispersion liquid, in mass ratio 1：8, processing shell matrix material is dipped to scattered
In liquid, immersion treatment is placed in mineralising at 50 DEG C and handles 5h, and standing is cooled to room temperature and filtered and to obtain filter residue, uses deionized water rinsing
After 5 times, then dried in 110 DEG C of baking ovens to constant weight, you can be prepared into a kind of bionical shell pearl material.
Reference examples：The bionical shell pearl material of Dongguan Materials Co., Ltd production.
The bionical shell pearl material of example and reference examples is detected, specific detection is as follows：
Extension test：Grow in 12mm, completed on small pieces wide 12mm.The speed of test is 0.0lmm/s, the maximum, force of test
For 5N.Final tensile strength and elongation at break is the average value of sample.
Hardness and modulus：Calculated by Oliver Pharr methods.
Specific testing result such as table 1.
Table 1
| Detection project | Example 1 | Example 2 | Example 3 | Reference examples |
| Hardness (G Pa) | 3.5 | 3.2 | 3.3 | 3.0 |
| Modulus of elasticity (G Pa) | 87.8 | 83.6 | 84.5 | 83 |
| Tensile strength (M Pa) | 136.4 | 130.8 | 132.1 | 125 |
| Elongation at break (%) | 2.0 | 1.8 | 1.9 | 1 |
As shown in Table 1, bionical the shell nacre material modulus and tensile strength that prepare of the present invention respectively reached 87.8GPa and
136.4MPa, the nacreous optimum value of shell is exceeded.The final fracture elongation of film is better than shell nacre.This illustrates this hair
The bionical shell pearl material of bright preparation has ductility more more preferable than shell nacre.
Claims (4)
1. a kind of preparation method of bionical shell pearl material, it is characterised in that specifically preparation process is：
（1）Take hydriopsis cumingii and cutting of polishing, obtain the wide shell fragments of the long 10mm of 20mm, in mass ratio 1：10, by shell fragment with
Liquor natrii hypochloritis is stirred, and filter cake is filtered to obtain after immersion, washing, dries, must handle shell matrix material；
（2）In mass ratio 1：8, boiled silk and ethanol solution are stirred, heating water bath and stand be cooled to room temperature, filter
Filtrate, in mass ratio 1：5, calcium chloride solution and filtrate are stirred, obtain mixed liquor；
（3）By mixed liquor rotary evaporated to dryness, silk extract gel particle is crushed to obtain, is counted in parts by weight, weigh 45~50 parts respectively
Deionized water, 10~15 parts of silk extract gel particles, 10~15 parts of sodium carbonate liquors of mass fraction 5% are stirred, ultrasonic disperse
10~15min, obtain dispersion liquid；
（4）In mass ratio 1：8, processing shell matrix material is dipped in dispersion liquid, soaks and mineralising is handled, stand cooling simultaneously
Filter residue is filtered to obtain, washing, is dried, you can be prepared into a kind of bionical shell pearl material.
A kind of 2. preparation method of bionical shell pearl material according to claim 1, it is characterised in that：Step（1）
Described liquor natrii hypochloritis's mass fraction is 5%.
A kind of 3. preparation method of bionical shell pearl material according to claim 1, it is characterised in that：Step（3）
Described rotating evaporation temperature is 45~50 DEG C.
A kind of 4. preparation method of bionical shell pearl material according to claim 1, it is characterised in that：Step（4）
Described mineralising treatment temperature is 45~50 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109336560A (en) * | 2018-10-04 | 2019-02-15 | 南京航空航天大学溧水仿生产业研究院有限公司 | Porous shell ceramic matric composite and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105385875A (en) * | 2015-12-04 | 2016-03-09 | 中北大学 | Preparation method for shell-nacreous-layer-imitating magnesium-based composite material |
| CN105774182A (en) * | 2016-03-24 | 2016-07-20 | 中国科学技术大学 | Composite material having shell nacre-imitated layered structure as well as preparation method and application of composite material |
| CN106431384A (en) * | 2016-08-31 | 2017-02-22 | 佛山市高明区生产力促进中心 | Artificial bionic shell and preparing method thereof |
| CN107174970A (en) * | 2017-06-01 | 2017-09-19 | 江苏大学 | A kind of GO/CaCO3The preparation method and its usage of the bionical composite film material of class shell |
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2017
- 2017-10-10 CN CN201710933513.1A patent/CN107603242A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105385875A (en) * | 2015-12-04 | 2016-03-09 | 中北大学 | Preparation method for shell-nacreous-layer-imitating magnesium-based composite material |
| CN105774182A (en) * | 2016-03-24 | 2016-07-20 | 中国科学技术大学 | Composite material having shell nacre-imitated layered structure as well as preparation method and application of composite material |
| CN106431384A (en) * | 2016-08-31 | 2017-02-22 | 佛山市高明区生产力促进中心 | Artificial bionic shell and preparing method thereof |
| CN107174970A (en) * | 2017-06-01 | 2017-09-19 | 江苏大学 | A kind of GO/CaCO3The preparation method and its usage of the bionical composite film material of class shell |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109336560A (en) * | 2018-10-04 | 2019-02-15 | 南京航空航天大学溧水仿生产业研究院有限公司 | Porous shell ceramic matric composite and preparation method thereof |
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Application publication date: 20180119 |