CN109967043A - A kind of organic-inorganic hybrid material LYZ-PTA of novel adjustable particle size - Google Patents
A kind of organic-inorganic hybrid material LYZ-PTA of novel adjustable particle size Download PDFInfo
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- CN109967043A CN109967043A CN201910256838.XA CN201910256838A CN109967043A CN 109967043 A CN109967043 A CN 109967043A CN 201910256838 A CN201910256838 A CN 201910256838A CN 109967043 A CN109967043 A CN 109967043A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0218—Compounds of Cr, Mo, W
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0259—Compounds of N, P, As, Sb, Bi
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/34—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of chromium, molybdenum or tungsten
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/38—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with substituted hydrocarbon radicals attached to ring carbon atoms
- C07D307/40—Radicals substituted by oxygen atoms
- C07D307/46—Doubly bound oxygen atoms, or two oxygen atoms singly bound to the same carbon atom
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
Abstract
The invention belongs to novel heterogeneous solid field of material synthesis technology, provide a kind of novel organic-inorganic hybrid material of adjustable particle size.The Bronsted acidity and lysozyme carried the present invention is based on phosphotungstic acid is as positively charged macro-molecular protein, and the two is combined under specified conditions special ratios, for the first time by phosphotungstic acid and bacteriolyze enzymatic synthesis the LYZ-PTA hybrid material of adjustable dimension, and it is applied to Dye Adsorption and fructose converting.
Description
Technical field
The invention belongs to novel heterogeneous solid field of material synthesis technology, a kind of the new of adjustable particle size is provided
Type organic-inorganic hybrid material LYZ-PTA.
Background technique
5 hydroxymethyl furfural (HMF) is a kind of important platform chemicals, is widely used in medicine, fuel, polymer etc.
Field.Containing methylol and aldehyde radical Liang Zhong functional group in the molecular structure of HMF, unique structure can be used to synthesize various function
The compounds such as energy property compound such as 5- ethoxyl methyl furfural, furandicarboxylic acid.It is one that HMF is efficiently produced using carbohydrate
The high reaction path of kind economy return.Therefore, how research efficiently becomes the current country from carbohydrate production HMF
The hot spot of outer scholar's research.
As strongest substance acid in metal heteropoly acid, the catalyst that can be used as organic synthesis replaces phosphotungstic acid
The liquid acid that environmental pollution is serious, or carry out reaction from different dyestuffs and form sediment.The aqueous solution of phosphotungstic acid can mention
For sufficiently strong Bronsted acidity and stronger oxidisability, homogeneous and heterogeneous reaction can be used as, to environment without dirt
Dye, is a kind of catalyst of green.How phosphotungstic acid is prepared into heterogeneous solid material with high economy return and green by research
Color benefit, more and more people begin to focus on research phosphotungstic acid support materials and are put into industrial production at present.
Lysozyme (lysozyme) is a kind of alkaline enzyme that can destroy pathogen cell wall, it is by 18 kinds of 129 amino
The single peptide chain that sour residue is constituted, be widely present in the Various Tissues of human body and the egg white of birds and poultry in.Lysozyme
Molecule is positively charged in the environment of slant acidity, can be adsorbed on weakly acidic cation exchange resin, and by using resin
The method of absorption extracts lysozyme from egg white.
This patent has mainly inquired into a kind of novel organic-inorganic hybrid material of adjustable particle size.In specified conditions spy
Under certainty ratio, for the first time by the phosphotungstic acid of the Bronsted acidity of carrying and positively charged macro-molecular protein lysozyme, preparation
A kind of novel organic-inorganic hybrid material LYZ-PTA of adjustable particle size is gone out.And for the pattern of LYZ-PTA material,
Functional group's type is analyzed.By the end of currently, the novel organic-inorganic hybrid material of this adjustable particle size is ground
Study carefully there is not yet document report.
Summary of the invention
The present invention provides a kind of organic-inorganic hybrid material LYZ-PTA of novel adjustable particle size, and describes it
Preparation method and two application, preparation process green are simple.
The present invention is realized by following experimental technique schemes, and a kind of organic-inorganic of novel adjustable particle size is miscellaneous
Change material LYZ-PTA, which is characterized in that the organic-inorganic hybrid material LYZ-PTA of the novel adjustable particle size be by
Keggin-type phosphotungstic acid and egg white lysozyme are constituted, wherein, the particle of formation different from the molar ratio of phosphotungstic acid based on lysozyme
Size is differed from 50nm to 600nm.
The preparation method of the organic-inorganic hybrid material LYZ-PTA of above-mentioned various sizes of novel adjustable particle size,
Including the following steps:
Step 1: the configuration of lysozyme soln:
The lysozyme of 14.6mg is dissolved in 2ml deionized water, 3ml isopropanol is added after rocking clarification, it is ultrasonic in Ultrasound Instrument
3min obtains solution A to clarifying;
Step 2: the configuration of Salkowski's solution:
It will be 1:15 with the molar ratio of lysozyme, 1:21,1:27, the phosphotungstic acid of 1:36 is dissolved in 5ml isopropanol, in Ultrasound Instrument
Ultrasonic 3min is completely dissolved to particle, obtains solution B;
Step 3: the preparation of LYZ-PTA material:
Solution B is placed in ultrasound, solution A is instilled in solution B dropwise with dropper, is added dropwise completely to solution A, ultrasound
30min obtains turbid solution, and turbid solution is filtered and is washed with deionized, and will be deposited in vacuum drying 10h at 60 DEG C and obtains
To LYZ-PTA material.According to the difference of lysozyme and phosphotungstic acid molar ratio, it is named as LYZ-PTA15, LYZ-PTA21,
LYZ-PTA27, LYZ-PTA36.
The organic-inorganic hybrid material LYZ-PTA of novel adjustable particle size obtained by the above method is applied to malachite
Green absorption, adsorbance is 41.67mgg in 20min-1, i.e. 25mgL-1Malachite green solution, 30mg material is 20
The malachite green in 50ml solution can be adsorbed completely in minute.
The organic-inorganic hybrid material LYZ-PTA of novel adjustable particle size obtained by the above method is applied in DMSO
The conversion of fructose has obtained 97.33% HMF yield for 20 minutes.
Compared with prior art, the invention has the advantages that:
Provide a kind of novel organic-inorganic hybrid material LYZ-PTA of adjustable particle size.Hydridization material provided by the invention
Material can adjust the particle size of catalyst by changing the ratio of lysozyme and phosphotungstic acid, and pass through scanning electron microscope, Fourier
The infrared conversion spectrum of leaf carried out phenetic analysis to material, it was demonstrated that the contained functional group of material and material are constituted, it was demonstrated that
The controllability of material particle size.The process of materials synthesis is simple to operation, no pollution to the environment, be it is a kind of green it is new
Profile material.And this novel organic-inorganic hybrid material LYZ-PTA can with but do not limit to be applied to solution Malachite Green
Absorption and DMSO in fructose conversion.
Detailed description of the invention
Fig. 1 is scanning electron microscope (SEM) phenogram of present invention gained LYZ-PTA15.
Fig. 2 is scanning electron microscope (SEM) phenogram of present invention gained LYZ-PTA21.
Fig. 3 is scanning electron microscope (SEM) phenogram of present invention gained LYZ-PTA27.
Fig. 4 is scanning electron microscope (SEM) phenogram of present invention gained LYZ-PTA36.
Fig. 5 is Fourier transform infrared spectroscopy (FI-IR) figure of present invention gained catalyst.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are only section Example,
Instead of all the embodiments, it is only illustrative of the invention and is not intended to limit the scope of the invention.Furthermore, it is to be understood that readding
After having read documented content of the invention, those skilled in the art can make various modifications or changes to the present invention, these etc.
Valence form equally falls within limited range of the present invention.
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Embodiment one
Catalyst preparation process are as follows: weigh lysozyme 14.6mg(0.001mmol), it is dissolved in 2ml deionized water, to solution
Completely after clarification, 3ml isopropanol is added into Lysozyme in Aqueous Solution, and ultrasonic in Ultrasound Instrument, solution is clarified completely after 3 minutes
And it is denoted as solution A.A certain amount of phosphotungstic acid is weighed, 5ml isopropanol is dissolved in, phosphotungstic acid is completely dissolved after stirring 3min,
Solution clear is labeled as B solution.In the case of stirring, lysozyme soln (solution A) is dripped dropwise by rubber head dropper
It adds in Salkowski's solution (B solution), it can be observed that occurring white opacity in solution rapidly.After solution A is all added dropwise, stir
It takes out, is filtered after mixing 30 minutes, and (40ml*6) is washed with deionized, the product after washing is finally put into vacuum and is done
It is dry in dry case, it is dried overnight at 60 DEG C, grinding is placed in centrifuge tube with to be used.
Embodiment two
Malachite green 25mg is weighed, is dissolved in 1000ml deionized water, with graduated cylinder weighing hole sparrow malachite green solution 50ml in beaker
In, rotor is added and is placed in magnetic agitation, by rotating-speed modulation 300rpm.LYZ-PTA15 material 30mg is weighed, is added to above-mentioned
In beaker, is sampled respectively at 0min, 5min, 10min, 20min, and measured with ultraviolet specrophotometer, hole is calculated
The absorption result of sparrow malachite green.LYZ-PTA15 material can remove in solution 79.98% malachite green at 5 minutes, and 20 minutes
The malachite green for eliminating in solution 99.9%, it is 41.67mgg that 20 minutes adsorbances of LYZ-PTA15 material, which are calculated,-1。
Embodiment three
Fructose 200mg is weighed, catalyst 50mg is simultaneously added in reaction kettle, is weighed dimethyl sulfoxide 5ml with graduated cylinder and is added to three
In mouth flask, in the case where reflux, three-necked flask is put into stirring and timing in the oil bath of certain temperature.After reaction starts,
A certain amount of reaction solution distilled water dilution several times were taken every 10 minutes, and were filtered with 0.22 micron of organic filter film,
Then liquid-phase chromatographic analysis product is carried out, 5 hydroxymethyl furfural yield is calculated.When 10 minutes, HMF yield reaches
62.43%, fructose converting rate has reached 64.39%;At 20 minutes, HMF yield reached highest 97.33%, fructose converting rate
Reach 99.99%.
Above embodiments are only illustrated embodiments of the present invention.It should be pointed out that the present invention is not limited to upper
Embodiment is stated, it to those of ordinary skill in the art, without departing from the principle of the present invention, can also be to this
Some improvement and modification can also be carried out for invention.All within the spirits and principles of the present invention, any modification for being made, changes equivalent replacement
Into etc., it should all fall within the scope of protection of the claims of the present invention.
Claims (5)
1. a kind of organic-inorganic hybrid material LYZ-PTA of novel adjustable particle size, it is characterised in that for the first time by phosphotungstic acid
With the bacteriolyze enzymatic synthesis nano material of adjustable dimension.
2. a kind of according to claim 1, organic-inorganic hybrid material LYZ-PTA of novel adjustable particle size, special
Sign is that the lysozyme of the selection of the material is egg white lysozyme, and phosphotungstic acid is Keggin-type phosphotungstic acid.
3. a kind of according to claim 1, organic-inorganic hybrid material LYZ-PTA of novel adjustable particle size, special
Sign exists, comprising following preparation method:
Step 1: the configuration of lysozyme soln:
Suitable lysozyme is dissolved in the water of certain volume, the isopropanol of addition certain volume after clarification is rocked, in Ultrasound Instrument
Middle ultrasound 3min obtains solution A to clarifying;
Step 2: the configuration of Salkowski's solution:
Suitable phosphotungstic acid is dissolved in the isopropanol of certain volume, ultrasound 3min is completely dissolved to particle in Ultrasound Instrument, is obtained
To solution B;
Step 3: the preparation of LYZ-PTA material:
Solution B is placed in ultrasound, solution A is instilled in solution B dropwise with dropper, is added dropwise completely to solution A, ultrasound
30min obtains turbid solution, and turbid solution is filtered and is washed with deionized, and will be deposited in vacuum drying 10h at 60 DEG C and obtains
To LYZ-PTA material.
4. a kind of according to claim 1, organic-inorganic hybrid material LYZ-PTA of novel adjustable particle size, special
Sign exists, and the material as described in right 1 is applied to the absorption of organic dyestuff, the absorption for malachite green, the maximum in 20min
Adsorbance is 41.67mgg-1, i.e. 25mgL-1Malachite green solution in, 30mg material can be by peacock in 20 minutes
Malachite green adsorbs completely.
5. a kind of according to claim 1, organic-inorganic hybrid material LYZ-PTA of novel adjustable particle size, special
Sign exists, and the material as described in right 1 is applied to conversion fructose in dimethyl sulfoxide and is prepared 5 hydroxymethyl furfural (HMF), and 20 minutes
The yield of HMF has reached 97.33%.
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101289435A (en) * | 2008-06-05 | 2008-10-22 | 大连理工大学 | Process for preparing 5-hydroxymethyl-furfural |
CN102153527A (en) * | 2011-02-28 | 2011-08-17 | 浙江师范大学 | Method for preparing 5-hydroxymethylfurfural with fructose |
CN102552166A (en) * | 2012-01-09 | 2012-07-11 | 北京化工大学 | Preparation method for lysozyme/poly (alpha-cyano acrylic butyl ester) medicine loading microsphere |
CN102911141A (en) * | 2011-08-05 | 2013-02-06 | 中国科学院大连化学物理研究所 | Method for preparing 5-ethyoxyl methylfurfural |
WO2013101970A1 (en) * | 2011-12-30 | 2013-07-04 | E. I. Du Pont De Nemours And Company | Production of 5-hydroxymethyl-2-furfural from levoglucosenone |
CN107494539A (en) * | 2017-08-28 | 2017-12-22 | 北京化工大学 | A kind of lysozyme/hydrotalcite composite antibacterial material and preparation method thereof and antibacterial applications |
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2019
- 2019-04-01 CN CN201910256838.XA patent/CN109967043A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101289435A (en) * | 2008-06-05 | 2008-10-22 | 大连理工大学 | Process for preparing 5-hydroxymethyl-furfural |
CN102153527A (en) * | 2011-02-28 | 2011-08-17 | 浙江师范大学 | Method for preparing 5-hydroxymethylfurfural with fructose |
CN102911141A (en) * | 2011-08-05 | 2013-02-06 | 中国科学院大连化学物理研究所 | Method for preparing 5-ethyoxyl methylfurfural |
WO2013101970A1 (en) * | 2011-12-30 | 2013-07-04 | E. I. Du Pont De Nemours And Company | Production of 5-hydroxymethyl-2-furfural from levoglucosenone |
CN102552166A (en) * | 2012-01-09 | 2012-07-11 | 北京化工大学 | Preparation method for lysozyme/poly (alpha-cyano acrylic butyl ester) medicine loading microsphere |
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黄承志等: "磷钨酸银纳米立方体的合成及光散射法测定溶菌酶", 《西南大学学报(自然科学版)》 * |
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