CN110707222B - Method for preparing flexible substrate material capable of adsorbing lanthanum oxide by aid of mantis shrimp diaphragms - Google Patents
Method for preparing flexible substrate material capable of adsorbing lanthanum oxide by aid of mantis shrimp diaphragms Download PDFInfo
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- CN110707222B CN110707222B CN201910636777.XA CN201910636777A CN110707222B CN 110707222 B CN110707222 B CN 110707222B CN 201910636777 A CN201910636777 A CN 201910636777A CN 110707222 B CN110707222 B CN 110707222B
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K77/00—Constructional details of devices covered by this subclass and not covered by groups H10K10/80, H10K30/80, H10K50/80 or H10K59/80
- H10K77/10—Substrates, e.g. flexible substrates
- H10K77/111—Flexible substrates
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- 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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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
- H10K59/10—OLED displays
- H10K59/12—Active-matrix OLED [AMOLED] displays
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- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
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- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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Abstract
The invention relates to a preparation method of a flexible material, and provides a method for preparing a flexible substrate material capable of adsorbing lanthanum oxide by using a mantis shrimp membrane, aiming at the problem that common chitin hardly adsorbs lanthanide metal oxide. And transferring the filter residue into an acetic acid solution, performing ultrasonic treatment, centrifuging, taking supernatant, and evaporating to remove water to obtain the flexible substrate material. According to the invention, chitin is modified to add a large number of amino and carboxyl functional groups, and the adsorption capacity of the flexible substrate material prepared from the modified chitin on lanthanum oxide is greatly improved, so that powerful support is provided for the development and application of the flexible substrate material in flexible screens such as AMOLED (active matrix organic light emitting diode) containing lanthanide metal oxide.
Description
Technical Field
The invention relates to a preparation method of a flexible material, in particular to a method for preparing a flexible substrate material capable of adsorbing lanthanum oxide by using a oratosquillas diaphragm.
Background
The flexible display screen is light and thin in volume, good in flexibility and good in development prospect. The substrate of the flexible display screen is generally made of flexible chemical plastics, one of the problems of the chemical plastics is that the chemical plastics is not easy to decompose and damage the environment, and the other is that the material for preparing the substrate of the flexible display screen needs to have high light transmittance, high thermal stability and high tensile strength, and the chemical plastics are usually high in price. Chitin is a natural polymer with a second content to cellulose in nature, and widely exists in natural resources such as crustaceans, fungi, insects, mollusks and the like. The chitin has good biocompatibility and degradability, can be prepared into a chitin film with certain flexibility and transparency, and can be used for replacing chemical plastics to prepare a substrate of a flexible display screen.
Lanthanide series oxide is resistant to acid and alkali corrosion, stable in high-temperature physical and chemical properties, and widely focused in the fields of semiconductors, luminescent materials and the like. The lanthanide series metal oxide TFT technology independently developed by China southern China university is reported to be the first time of successfully developing a color flexible AMOLED (active matrix organic light emitting diode, the most advanced flexible screen technology at present) display screen technology in China, and breaks the technical barrier of foreign countries. Therefore, the method has great significance for preparing the flexible screen with excellent properties by greatly improving the adsorption capacity of the lanthanide series metal oxide. However, the common chitin hardly adsorbs lanthanide metal oxides, and thus an ideal technical structure is needed to solve the above problems.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention provides the method for preparing the flexible substrate material capable of adsorbing the lanthanum oxide by using the oratosquillas diaphragm, the prepared flexible substrate material is biodegradable and environment-friendly, the adsorption capacity of the flexible substrate material on the lanthanide series metal oxide is up to 107.8 mg/g of chitin, and powerful support is provided for the development and application of the flexible substrate material in flexible screens such as AMOLED (active matrix organic light emitting diode) containing the lanthanide series metal oxide.
In order to achieve the purpose, the invention adopts the following technical scheme: a method for preparing a flexible substrate material capable of adsorbing lanthanum oxide by using a mantis shrimp membrane is characterized in that the dried mantis shrimp membrane is firstly crushed into micro-nano-scale membrane powder, then the membrane powder is added into an amino-triethyl acid solution, N-dimethylaniline, potassium persulfate and hydrogen peroxide are added, the mixture is sealed and continuously stirred at normal temperature for 8 to 12 hours, a product is filtered, filter residues are washed to be neutral by water, and the vacuum drying is carried out. And transferring filter residues into an acetic acid solution, performing ultrasonic treatment and then centrifuging, taking supernate, and evaporating water to obtain the flexible substrate material.
The content of chitin in the diaphragm of the Oratosquilla is very high, which accounts for about 82.8% of the total mass, and the residual impurities comprise minerals (mainly calcium carbonate), crude protein, grease and the like, the mass percent of the minerals is only 8.6%, and the mass percent of the protein is also only 7.2%. Because the mineral content and the protein content are low, the high-purity chitin (the ash content is less than 1%) can be obtained only by processing a small amount of low-concentration amino-triethyl-acid solution when extracting effective components, so the Mantis oralis diaphragm is adopted as a raw material, the processing steps are simple, and the reagent consumption is low; the flexible substrate material prepared from the oratosquillas diaphragm belongs to waste utilization, the raw materials are cheap, and the solid waste treatment cost of the oratosquillas diaphragm is reduced; the diaphragm of the oratosquillas is an ecological material, and the flexible substrate material prepared from the diaphragm of the oratosquillas is degradable and environment-friendly. The method comprises the steps of modifying chitin by taking N, N-dimethylaniline as a modifier and potassium persulfate and hydrogen peroxide as initiators, adding a large number of amino and carboxyl functional groups to the chitin, and preparing the flexible substrate material after a series of purification treatments such as acetic acid solution dissolution, ultrasound, centrifugation and the like, wherein the adsorption capacity of the flexible substrate material on lanthanum oxide is greatly improved.
Preferably, the concentration of the solution of the amino-triethanoic acid is 10-25% (w: v).
Preferably, the material-liquid ratio of the membrane powder to the amino-triethyl acid solution is 1g (20-50) mL.
Preferably, the addition amounts of potassium persulfate and hydrogen peroxide are each 0.1 to 10% (w: v) of the aqueous solution of iminodisuccinic acid sodium salt.
Preferably, the feed-liquid ratio of the filter residue to the acetic acid solution is 1g (30-50) mL.
Preferably, the sonication is carried out at 900W under ice bath for 1-2 hours.
Preferably, the centrifugation is carried out at 12000 rpm and 4 ℃ for 30 min.
Therefore, the invention has the following beneficial effects: (1) the raw material oratosquillas diaphragm disclosed by the invention is high in chitin content, high-purity chitin can be obtained only by treating a small amount of low-concentration aminotrietic acid solution, the treatment steps are simple, the reagent consumption is low, and the method is convenient and environment-friendly; (2) the flexible substrate material prepared from the oratosquillas diaphragm belongs to waste utilization, the raw materials are cheap, and the solid waste treatment cost of the oratosquillas diaphragm is reduced; (3) the flexible substrate material prepared from chitin is degradable and environment-friendly; (4) the chitin is modified to add a large number of amino and carboxyl functional groups, the adsorption capacity of the flexible substrate material prepared from the modified chitin on lanthanum oxide is greatly improved, and powerful support is provided for development and application of the flexible substrate material in flexible screens such as AMOLED containing lanthanide metal oxide.
Drawings
Fig. 1 is a graph showing the adsorption amount of lanthanum oxide to the flexible base materials of example 1 and comparative example.
Fig. 2 is an SEM image of the flexible base material of the comparative example after adsorbing lanthanum oxide.
Fig. 3 is an SEM image of the flexible substrate material of example 1 after adsorbing lanthanum oxide.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
In the present invention, unless otherwise specified, all the raw materials and equipment used are commercially available or commonly used in the art, and the methods in the examples are conventional in the art unless otherwise specified.
Example 1
Firstly, crushing a dried mantis shrimp diaphragm into micro-nano diaphragm powder by using an ultrafine crusher, then adding 10g of diaphragm powder into 200mL of amino-triethyl-acid solution, wherein the concentration of the amino-triethyl-acid solution is 15% (w: v), then adding 10g of N, N-dimethylaniline, 10g of potassium persulfate and 10g of hydrogen peroxide, sealing, continuously stirring for 12 hours at normal temperature, filtering a product, washing filter residues to be neutral by using water, and carrying out vacuum drying. And transferring the filter residue into an acetic acid solution with the pH value equal to 3, continuously performing ultrasonic treatment for 1 hour in an ice bath environment by using a 900W ultrasonic cell disruptor, then centrifuging for 30 min at the rotation speed of 12000 rpm and the temperature of 4 ℃, taking supernatant, and evaporating water to dryness in an oil bath at the temperature of 100 ℃ to obtain the flexible substrate material.
Example 2
Firstly crushing the dried mantis shrimp diaphragm into micro-nano diaphragm powder by using a superfine crusher, then adding 10g of diaphragm powder into 500mL of aminotriethanoic acid solution, wherein the concentration of the aminotriethanoic acid solution is 25% (w: v), then adding 50g of N, N-dimethylaniline, 50g of potassium persulfate and 0.5g of hydrogen peroxide, sealing, continuously stirring for 8 hours at normal temperature, filtering the product, washing filter residues to be neutral by using water, and drying in vacuum. And transferring the filter residue into an acetic acid solution with the pH value equal to 2, continuously performing ultrasonic treatment for 2 hours in an ice bath environment by using a 900W ultrasonic cell disruptor, centrifuging for 50 minutes at the rotation speed of 12000 rpm and the temperature of 0 ℃, taking supernatant, and evaporating water to dryness in an oil bath at the temperature of 100 ℃ to obtain the flexible substrate material.
Example 3
Firstly crushing the dried squilla oratoria into micro-nano-scale membrane powder by using a superfine crusher, then adding 10g of membrane powder into 300mL of aminotriacetic acid solution, wherein the concentration of the aminotriacetic acid solution is 10% (w: v), continuously adding 15g of N, N-dimethylaniline, 0.3g of potassium persulfate and 30g of hydrogen peroxide, sealing, continuously stirring for 10 hours at normal temperature, filtering the product, washing filter residues to be neutral by using water, and drying in vacuum. And transferring the filter residue into an acetic acid solution with the pH value equal to 3, continuously performing ultrasonic treatment for 1 hour in an ice bath environment by using a 900W ultrasonic cell disruptor, centrifuging for 20 min at the rotation speed of 12000 rpm and the temperature of 4 ℃, taking supernatant, and evaporating water to dryness in an oil bath at the temperature of 100 ℃ to obtain the flexible substrate material.
Comparative example
10g of the membrane powder prepared in example 1 was added to 200mL of an aminotrietric acid solution having a concentration of 15% (w: v), sealed, stirred continuously at room temperature for 12 hours, the product was filtered, the filter residue was washed with water to neutrality, and dried in vacuo. And transferring the filter residue into an acetic acid solution with the pH value equal to 3, continuously performing ultrasonic treatment for 1 hour in an ice bath environment by using a 900W ultrasonic cell disruption instrument, centrifuging for 30 min at the rotation speed of 12000 rpm and the temperature of 4 ℃, taking supernatant, and evaporating water to dryness in an oil bath at the temperature of 100 ℃ to obtain the flexible substrate material.
The comparative example, which has a modification step less than example 1 and the other treatments are identical, has a layer of lanthanum oxide coated on their respective products, and the effect of the modification step on the properties of the flexible material can be seen by characterization. As shown in FIG. 1, the flexible substrate material made of unmodified chitin has no adsorption capacity to lanthanum oxide basically, while the flexible substrate material made of modified chitin has an adsorption capacity to lanthanum as high as 91.9mg/g chitin (107.8 mg/g chitin after being converted into lanthanum oxide). In addition, as shown in fig. 2 and 3, after the lanthanide oxide is adsorbed, no lanthanum oxide particles can be found on the surface of the unmodified chitin; a large amount of lanthanum oxide particles are distributed on the surface of the modified chitin, which shows that the adsorption capacity of the modified chitin on lanthanide metal oxide is greatly improved. The material provides powerful support for development and application of the material in flexible screens such as AMOLED containing lanthanide metal oxides.
The raw material mantis shrimp diaphragm of the invention has high chitin content, and high-purity chitin can be obtained only by treating a small amount of low-concentration amino-triethyl acid solution, so that the treatment steps are simple, the reagent consumption is low, and the method is convenient and environment-friendly; the flexible substrate material prepared from the oratosquillas diaphragm belongs to waste utilization, the raw materials are cheap, and the solid waste treatment cost of the oratosquillas diaphragm is reduced; the flexible substrate material prepared from chitin is degradable and environment-friendly; the chitin is modified to add a large number of amino and carboxyl functional groups, the adsorption capacity of the flexible substrate material prepared from the modified chitin to lanthanum oxide is greatly improved, and powerful support is provided for development and application of the flexible substrate material in flexible screens such as AMOLED (active matrix organic light emitting diode) containing lanthanide metal oxide.
Claims (6)
1. The method for preparing the flexible substrate material capable of adsorbing the lanthanum oxide by using the mantis shrimp membrane is characterized in that the dried mantis shrimp membrane is firstly crushed into micro-nano-scale membrane powder, then the membrane powder is added into an amino-triethyl acid solution, N-dimethylaniline, potassium persulfate and hydrogen peroxide are added, the mixture is sealed and continuously stirred at normal temperature for 8-12 hours, a product is filtered, filter residues are washed to be neutral by water, the mixture is dried in vacuum, the filter residues are transferred into an acetic acid solution, the material-liquid ratio of the filter residues to the acetic acid solution is 1g (30-50) mL, the mixture is subjected to ultrasonic treatment and centrifugation, supernatant is taken, and water is evaporated to obtain the flexible substrate material.
2. The method for preparing a flexible substrate material capable of adsorbing lanthanum oxide from mantis shrimp membranes as claimed in claim 1, wherein the concentration of the amino-acetic acid solution is 10-25% (w: v).
3. The method for preparing the flexible substrate material capable of adsorbing the lanthanum oxide from the mantis shrimp membranes as claimed in claim 1, wherein the feed-liquid ratio of the membrane powder to the amino-triethyl acid solution is 1g (20-50) mL.
4. The method for preparing a flexible substrate material capable of adsorbing lanthanum oxide from a mantis shrimp membrane as claimed in claim 1, 2 or 3, wherein the addition amount of potassium persulfate and hydrogen peroxide is 0.1-10% (w: v) of the amino-triethyl-acid solution.
5. The method for preparing the flexible substrate material capable of adsorbing the lanthanum oxide by using the mantis shrimp membrane as claimed in claim 1, wherein the ultrasonic condition is 900W, and the continuous ultrasonic treatment is carried out for 1-2 hours in an ice bath.
6. The method for preparing the flexible substrate material capable of adsorbing the lanthanum oxide from the mantis shrimp membranes as claimed in claim 1, wherein the centrifugation is performed at 12000 rpm and 4 ℃ for 30 min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103342821A (en) * | 2013-07-10 | 2013-10-09 | 南京林业大学 | Method for preparing chitin nanofibre by using shrimp and crab shells |
| CN109225157A (en) * | 2018-10-26 | 2019-01-18 | 浙江海洋大学 | A kind of preparation method of lanthanum ion adsorbent |
| CN109824797A (en) * | 2018-10-26 | 2019-05-31 | 浙江海洋大学 | A method of preparing chitin |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103342821A (en) * | 2013-07-10 | 2013-10-09 | 南京林业大学 | Method for preparing chitin nanofibre by using shrimp and crab shells |
| CN109225157A (en) * | 2018-10-26 | 2019-01-18 | 浙江海洋大学 | A kind of preparation method of lanthanum ion adsorbent |
| CN109824797A (en) * | 2018-10-26 | 2019-05-31 | 浙江海洋大学 | A method of preparing chitin |
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