CN109608659A - High efficiency photocatalysis type casein/carbon quantum dot multiple emulsion preparation method - Google Patents
High efficiency photocatalysis type casein/carbon quantum dot multiple emulsion preparation method Download PDFInfo
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- CN109608659A CN109608659A CN201811421999.1A CN201811421999A CN109608659A CN 109608659 A CN109608659 A CN 109608659A CN 201811421999 A CN201811421999 A CN 201811421999A CN 109608659 A CN109608659 A CN 109608659A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L89/00—Compositions of proteins; Compositions of derivatives thereof
- C08L89/005—Casein
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Abstract
The invention discloses a kind of casein of high efficiency photocatalysis performance/carbon quantum dot multiple emulsion preparation method, technical solution: firstly, casein, which is carried out graft modification using caprolactam under alkaline condition, forms lotion；Then, the hydrophily carbon quantum dot (CQDs) prepared using citric acid as carbon source；Finally, the hydrophily carbon quantum dot being prepared is slowly added in proportion in modified casein emulsion, keep the two sufficiently compound by magnetic agitation/ultrasonic disperse, to form casein/carbon quantum dot multiple emulsion.The present invention is by the way that inorganic nano material carbon quantum dot to be introduced into casein emulsion, the mechanical performance of casein emulsion film forming not only can be improved, simultaneously, the good glossiness of film and certain photocatalysis performance can also be assigned, the practicability and added value that product is improved in fields such as leather, papermaking, weavings are applied as finishing agent.
Description
Technical field
The invention belongs to functional form multiple emulsion preparation fields, and in particular to a kind of casein/carbon of high efficiency photocatalysis performance
The preparation method of quantum dot multiple emulsion.
Background technique
As research direction is turned to green energy resource by energy shortage and the more and more researchers of environmental issue, it is desirable to grind
Study carefully product environmentally protective out.Photocatalysis technology, which is used as, is thoroughly degraded to carbon dioxide and water for organic dirt using solar energy,
Loss-free a special kind of skill of catalysis material itself simultaneously, the favor by numerous scholars.
More researchs are to utilize inorganic nano-particle TiO at present2Photocatalysis and metal is doped to it
Such as Au, Ag improve its photocatalysis effect[1-2][Liao T W, Verbruggen S, Claes N, et al.
TiO2Films Modified with Au Nanoclusters as Self-Cleaning Surfaces under
Visible Light[J]. Nanomaterials, 2018, 8(1):30.Dudem B, Bharat L K, Leem J W,
et al. Hierarchical Ag/TiO2/Si Forest-Like Nano/Micro-Architectures as
Antireflective, Plasmonic Photocatalytic, and Self-Cleaning Coatings[J]. Acs
Sustainable Chemistry & Engineering, 2018,6 (2): 1580-1591.], but utilize simple nothing
Its application range of machine material has certain limitation, and Organic/Inorganic Composite Nanomaterials can not only overcome simple inorganic particulate
Grain is not easy to be processed and the disadvantages such as organic macromolecule stability is poor, intensity is low, can also be under the collective effect of the two, acquisition
Performance more superior than inorganic particle and organic polymer, such as the mechanics of material, electricity, calorifics, in terms of it is excellent
Performance.Therefore, in view of the distinctive performance of Organic/Inorganic Composite Nanomaterials, in light, electricity, mechanics, biology, magnetics and micro-
The development and application etc. of type device suffer from wide application prospect[3][Liu Xiaobo is organic by Shi Zhiqiang, Liu Xiaolei/nothing
Progress [J] of machine nanocomposite synthesizes chemistry, 2004,12 (3): 251-254.].
Casein is the native protein extracted from milk as a kind of natural polymer, have raw material be easy to get, can biology
Degrade and regenerate, good biocompatibility the advantages that.However, pure casein often has the disadvantages of film forming is hard crisp, easily mouldy, limit
Its application, it is, therefore, necessary to be modified to it.With our improvements of living standard, for the article of comfortable convenient type
It is required that higher and higher.Casein emulsion itself has the limitation of application, in order to preferably promote its performance, widens answering for it
With more and more researchers are modified it or by it in conjunction with inorganic nano-particle.Seminar where the present inventor
By nano-ZnO in conjunction with casein, the good anti-microbial property of casein emulsion is assigned [4][Wang Yanan antimicrobial form casein base nano-ZnO
The synthesis of composite leather coating and decorating material and performance study [D] Shaanxi Tech Univ, 2017.].By casein and SiO2In conjunction with,
Leather sample after gained multiple emulsion is covered with paint, lacquer, colour wash, etc. has preferably mechanical performance[5] [Xu Q, Ma J, Zhou J, et al. Bio-
based core–shell casein-based silica nano-composite latex by double-in situ
polymerization: Synthesis, characterization and mechanism[J]. Chemical
Engineering Journal, 2013, 228(28):281-289.]。
With the development of science and technology, more and more organic materials and inorganic material are compound, it is desirable to new material can be assigned more
Good performance.Inorganic nano-particle carbon quantum dot, preparation method is simple, and synthesis cost is low, and toxicity is low, is easy to function of surface
Change, there is good photocatalytic, so all having received widespread attention in many fields[6] [Lim S Y, Shen W, Gao
Z. Carbon quantum dots and their applications[J]. Chemical Society Reviews,
2015, 44(1):362-81.].So far, the research that carbon quantum dot is introduced into casein emulsion is also rarely reported.
Summary of the invention
The object of the present invention is to provide a kind of casein of high efficiency photocatalysis performance/carbon quantum dot multiple emulsion preparation sides
Method, has widened the application range of casein, carbon quantum dot, while developing a kind of novel film-formable with photocatalysis performance
Multiple emulsion has widened the application of lotion.
The technical solution adopted by the present invention are as follows:
A kind of preparation method of high efficiency photocatalysis type casein/carbon quantum dot multiple emulsion, comprising the following steps:
Step 1: the preparation of modified Casein lotion:
Firstly, the alkaline solution that the concentration for preparing 75-225g is 1wt%-3wt%, weighs 8.3-24.9g casein (commercially available), adds
Enter into three-necked flask and carry out heating water bath stirring, obtains casein lysate；Then the concentration for preparing 18-54g is 10wt%-
The caprolactam solution of 30wt%, is added into casein lysate, continues to stir 0.5-2.5h under the same conditions, be changed
Property casein solution.
Step 2: the preparation of carbon quantum dot solution:
Take 4.0-6.0g citric acid firstly, weighing, measure 1.3-1.9mL ethylenediamine, 40-60mL deionized water pour into beaker into
Row stirring, pours into them after completely dissolution and carries out hydro-thermal reaction in autoclave, obtain carbon quantum dot solution.
Step 3: the preparation of casein/carbon quantum dot multiple emulsion:
By the modified Casein casein solution that step 1 is prepared and the carbon quantum dot solution that step 2 is prepared by 1:1~1:
50 mass ratio progress is compound, and complex method is mechanical blending, obtains casein/carbon quantum dot multiple emulsion.
Preferably, in step 1, the alkaline solution is diethanol amine aqueous solution, triethanolamine aqueous solution, Boratex water
One of solution, aqueous sodium carbonate, sodium bicarbonate aqueous solution.
Preferably, in step 1, the temperature of the heating water bath stirring of the casein is 50 ~ 70 DEG C, and the speed of stirring is
100-400r/min, the time of heating stirring are 0.5-2.5h.
Preferably, in step 2, the carbon quantum dot is Water-soluble carbon quantum dot；The temperature of the hydro-thermal reaction is 160-
200 DEG C, the time of hydro-thermal reaction is 5h.
Preferably, in step 3, the mechanical blending complex method of modified Casein casein solution and carbon quantum dot solution is used
The method of magnetic agitation or ultrasonic disperse.Wherein, the speed of magnetic agitation is 300-400r/min, and the time of stirring is 0.5-
3h；The power of ultrasonic disperse is 200-300W, and the ultrasonic time is 0.5-2h.
The invention has the following advantages that
1. the present invention obtains casein/carbon quantum dot multiple emulsion by mechanical blending method, it is expected to apply in coating, weaving, food
The practicability and added value of product are improved in field etc., assign the good photocatalysis performance of product.
2. the preparation method of the raw materials used in the present invention inorganic nano-particle carbon quantum dot is simple, synthesis cost is low, and toxicity is low,
It is easy to surface-functionalized, there is good photocatalytic.
3. inorganic nano material carbon quantum dot is introduced into casein emulsion by the present invention, casein emulsion film forming not only can be improved
Mechanical performance answered it is also possible to assign the good glossiness of film and certain photocatalysis performance as finishing agent
Used in fields such as leather, papermaking, weavings, the practicability and added value of product are improved, the application field for widening casein has
Significance.
Detailed description of the invention
Fig. 1 is under ultraviolet lighting, and modified Casein lotion is to rhodamine degradation situation；
Fig. 2 is under UV illumination, and casein/carbon quantum dot multiple emulsion is to rhodamine degradation situation.
Specific embodiment
The present invention is described in detail With reference to embodiment.
Carbon quantum dot is introduced into modified Casein solution by the present invention, prepares casein/carbon using simply mechanical blending method
Quantum dot multiple emulsion.
Casein of the present invention/carbon quantum dot multiple emulsion preparation method, comprising the following specific steps
Step 1: the preparation of modified Casein lotion:
Firstly, prepare 75-225g concentration be 1wt%-3wt% alkaline solution, weigh 8.3-24.9g casein it is (commercially available) plus
Enter into three-necked flask and carry out heating water bath stirring, wherein the temperature of heating water bath is 50 ~ 70 DEG C, and the speed of stirring is 100-
400r/min, the time 0.5-2.5h of heating, is prepared casein lysate；Then the concentration for preparing 18-54g is 10wt%-
The caprolactam solution of 30wt%, is then added into casein lysate, continues to stir 0.5-2.5h under the same conditions, obtain
To modified Casein solution.
Further, the alkaline solution is diethanol amine aqueous solution, triethanolamine aqueous solution, boric acid sodium water solution, carbon
One of acid sodium aqueous solution, sodium bicarbonate aqueous solution.
Step 2: the preparation of carbon quantum dot solution:
4.0-6.0g citric acid, 1.3-1.9mL ethylenediamine are taken firstly, weighing, 40-60mL deionized water is poured into beaker and carried out
Stirring, pours into them after completely dissolution and carries out hydro-thermal reaction in autoclave, carbon quantum dot solution is prepared.
Further, the temperature of the hydro-thermal reaction is 160-200 DEG C, and the time of hydro-thermal reaction is 5h.
Step 3: the preparation of casein/carbon quantum dot multiple emulsion:
By the modified Casein casein solution that step 1 is prepared and the carbon quantum dot solution that step 2 is prepared by 1:1~1:
50 mass ratio progress is compound, and complex method is mechanical blending, and recombination time 0.5-3h finally obtains casein/carbon quantum
Point multiple emulsion.
Further, modified Casein casein solution and the compound of carbon quantum dot solution use magnetic agitation or ultrasonic disperse
Blend technique；When wherein, using magnetic agitation, the speed of stirring is 300-400r/min, and the time of stirring is 0.5-
3h；When using ultrasonic disperse, the power of ultrasonic disperse is 200-300W, and the ultrasonic time is 0.5-2h.
Embodiment 1:
Step 1: the preparation of modified Casein lotion:
Firstly, the diethanol amine aqueous solution that the concentration for preparing 75g is 1wt%, weighs 8.3g casein (commercially available) and is added to three mouthfuls of burnings
Heating water bath stirring is carried out in bottle, wherein the temperature of heating water bath is 50 DEG C, mixing speed 100r/min, and heating 0.5h is obtained
To casein lysate；Then the concentration for preparing 18g is the caprolactam solution of 10wt%, is then added into casein lysate,
Continue to stir 0.5h under the same conditions, obtains modified Casein solution.
Step 2: the preparation of carbon quantum dot solution:
It takes citric acid 4.0g, ethylenediamine 1.3mL, deionized water 40mL to pour into beaker and be stirred firstly, weighing, fills them
It is poured into autoclave after dividing dissolution, then in 160 DEG C of at a temperature of heating reaction 5h, obtains Water-soluble carbon quantum dot solution.
Step 3: the preparation of casein/carbon quantum dot multiple emulsion:
It will be prepared in step 1 in obtained modified Casein casein solution and step 2 and prepare obtained carbon quantum dot solution
Carried out by the mass ratio of 1:1 compound, complex method is magnetic agitation, mixing speed 400r/min, mixing time 0.5h,
Finally obtain casein/carbon quantum dot multiple emulsion.
Embodiment 2:
Step 1: the preparation of modified Casein lotion:
Firstly, the boric acid sodium water solution that the concentration for preparing 150g is 2wt%, weighs 16.6g casein (commercially available) and is added to three mouthfuls of burnings
Heating water bath stirring is carried out in bottle, wherein bath temperature is 60 DEG C, mixing speed 200r/min, and the time of heating is 1h, is obtained
To casein lysate；Then the concentration for preparing 36g is the caprolactam solution of 20wt%, is then added into casein lysate,
Continue to stir 1h under the same conditions, obtains modified Casein solution.
Step 2: the preparation of carbon quantum dot solution:
It takes 5.0g citric acid, 1.6mL ethylenediamine, 50mL deionized water to pour into beaker and be stirred firstly, weighing, fills them
Point dissolution after pour into autoclave, then 180 DEG C at a temperature of, heating reaction 5h, Water-soluble carbon quantum dot is prepared
Solution.
Step 3: the preparation of casein/carbon quantum dot multiple emulsion:
By the carbon quantum dot solution being prepared in the modified Casein casein solution being prepared in step 1 and step 2 by 1:
10 mass ratio carries out compound, and complex method is magnetic agitation, mixing speed 300r/min, mixing time 1h, finally
Obtain casein/carbon quantum dot multiple emulsion.
Embodiment 3:
Step 1: the preparation of modified Casein lotion:
Firstly, the triethanolamine aqueous solution that the concentration for preparing 225g is 3wt%, weighs 24.9g casein (commercially available) and is added to three mouthfuls
Heating water bath stirring is carried out in flask, wherein bath temperature is 70 DEG C, and the speed of stirring is 300r/min, heating stirring when
Between be 2h so that casein lysate be prepared；Then the concentration for preparing 54g is the caprolactam solution of 30wt%, then by it
It is added in casein lysate, continues to stir 2h under the same conditions, obtain modified Casein solution.
Step 2: step 2: the preparation of carbon quantum dot solution:
It pours into beaker and is stirred firstly, weighing 6.0g citric acid, 1.9mL ethylenediamine, 60mL deionized water, make them sufficiently
Poured into autoclave after dissolution, then 200 DEG C at a temperature of, heating reaction 5h, prepare Water-soluble carbon quantum dot solution.
Step 2: the preparation of casein/carbon quantum dot multiple emulsion:
By the carbon quantum dot solution being prepared in the modified Casein casein solution being prepared in step 1 and step 2 by 1:
50 mass ratio progress is compound, and complex method is ULTRASONIC COMPLEX, and power 300r/min, recombination time 1h are finally obtained
Casein/carbon quantum dot multiple emulsion.
In order to test the performance of the preparation-obtained casein/carbon quantum dot multiple emulsion of the present invention, the present inventor to its into
Row photocatalysis simulation test.Specifically, being surveyed in the absorbance change situation of ultraviolet specrophotometer measurement different time points solution
Test result analysis is as depicted in figs. 1 and 2.
Situation is reduced by the absorbance of comparison diagram 1, the same time point of Fig. 2 it is found that the Composite Milk of carbon quantum dot is added
Liquid has preferable degradation situation to rhodamine, therefore deduces that a conclusion: the multiple emulsion that carbon quantum dot is added has more
Good photocatalysis performance.
The contents of the present invention are not limited to cited by embodiment, and those of ordinary skill in the art are by reading description of the invention
And to any equivalent transformation that technical solution of the present invention is taken, it is all that claim of the invention is covered.
Claims (6)
1. a kind of preparation method of high efficiency photocatalysis type casein/carbon quantum dot multiple emulsion, which is characterized in that including following step
It is rapid:
Step 1: the preparation of modified Casein lotion:
Firstly, the alkaline solution that the concentration for preparing 75-225g is 1wt%-3wt%, weighs 8.3-24.9g casein (commercially available), adds
Enter into three-necked flask and carry out heating water bath stirring, obtains casein lysate；Then the concentration for preparing 18-54g is 10wt%-
The caprolactam solution of 30wt%, is added into casein lysate, continues to stir 0.5-2.5h under the same conditions, be changed
Property casein solution；
Step 2: the preparation of carbon quantum dot solution:
Take 4.0-6.0g citric acid firstly, weighing, measure 1.3-1.9mL ethylenediamine, 40-60mL deionized water pour into beaker into
Row stirring, pours into them after completely dissolution and carries out hydro-thermal reaction in autoclave, obtain carbon quantum dot solution；
Step 3: the preparation of casein/carbon quantum dot multiple emulsion:
By the modified Casein casein solution that step 1 is prepared and the carbon quantum dot solution that step 2 is prepared by 1:1~1:
50 mass ratio progress is compound, and complex method is mechanical blending, obtains casein/carbon quantum dot multiple emulsion.
2. the preparation method of high efficiency photocatalysis type casein/carbon quantum dot multiple emulsion according to claim 1, feature exist
In:
In step 1, the alkaline solution is diethanol amine aqueous solution, triethanolamine aqueous solution, boric acid sodium water solution, sodium carbonate
One of aqueous solution, sodium bicarbonate aqueous solution.
3. the preparation method of high efficiency photocatalysis type casein/carbon quantum dot multiple emulsion according to claim 2, feature exist
In:
In step 1, the temperature of the heating water bath stirring of the casein is 50 ~ 70 DEG C, and the speed of stirring is 100-400r/
Min, the time of heating stirring are 0.5-2.5h.
4. the preparation method of high efficiency photocatalysis type casein/carbon quantum dot multiple emulsion according to claim 3, feature exist
In:
In step 2, the carbon quantum dot is Water-soluble carbon quantum dot；
The temperature of the hydro-thermal reaction is 160-200 DEG C, and the time of hydro-thermal reaction is 5h.
5. the preparation method of high efficiency photocatalysis type casein/carbon quantum dot multiple emulsion according to claim 4, feature exist
In:
In the step 3, the mechanical blending complex method of modified Casein casein solution and carbon quantum dot solution uses magnetic agitation
Or the method for ultrasonic disperse.
6. the preparation method of high efficiency photocatalysis type casein/carbon quantum dot multiple emulsion according to claim 5, feature exist
In:
In the step 3, the speed of magnetic agitation is 300-400r/min, and the time of stirring is 0.5-3h；The function of ultrasonic disperse
Rate is 200-300W, and the ultrasonic time is 0.5-2h.
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| CN109967064A (en) * | 2019-04-25 | 2019-07-05 | 陕西科技大学 | It is a kind of using natural casein as the porous spherical TiO of template2The preparation method of nanocatalyst |
| CN111019157A (en) * | 2019-12-27 | 2020-04-17 | 陕西科技大学 | Antibacterial casein-based ZIF-8 composite emulsion and preparation method thereof |
| CN115651277A (en) * | 2022-11-07 | 2023-01-31 | 凌滋透明质酸(海南)生物科技有限公司 | Preparation method of carbon quantum dot modified hyaluronic acid and food preparation |
| CN116716745A (en) * | 2023-08-10 | 2023-09-08 | 福建省永建皮革科技股份有限公司 | Multilayer finishing antibacterial leather |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109967064A (en) * | 2019-04-25 | 2019-07-05 | 陕西科技大学 | It is a kind of using natural casein as the porous spherical TiO of template2The preparation method of nanocatalyst |
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| CN115651277A (en) * | 2022-11-07 | 2023-01-31 | 凌滋透明质酸(海南)生物科技有限公司 | Preparation method of carbon quantum dot modified hyaluronic acid and food preparation |
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| CN116716745A (en) * | 2023-08-10 | 2023-09-08 | 福建省永建皮革科技股份有限公司 | Multilayer finishing antibacterial leather |
| CN116716745B (en) * | 2023-08-10 | 2023-10-27 | 福建省永建皮革科技股份有限公司 | Multilayer finishing antibacterial leather |
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Application publication date: 20190412 |
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| RJ01 | Rejection of invention patent application after publication |