CN115260723B - Preparation method of degradable fluorescent film of aminated carbon quantum dot - Google Patents
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229920000747 poly(lactic acid) Polymers 0.000 claims abstract description 36
- 239000004626 polylactic acid Substances 0.000 claims abstract description 36
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 21
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- -1 amino carbon quantum dot Chemical compound 0.000 claims abstract description 14
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 12
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- 238000000576 coating method Methods 0.000 claims abstract description 9
- 239000010453 quartz Substances 0.000 claims abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000004729 solvothermal method Methods 0.000 claims abstract description 8
- 238000002390 rotary evaporation Methods 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 6
- QOSSAOTZNIDXMA-UHFFFAOYSA-N Dicylcohexylcarbodiimide Chemical group C1CCCCC1N=C=NC1CCCCC1 QOSSAOTZNIDXMA-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 5
- AGGKEGLBGGJEBZ-UHFFFAOYSA-N tetramethylenedisulfotetramine Chemical group C1N(S2(=O)=O)CN3S(=O)(=O)N1CN2C3 AGGKEGLBGGJEBZ-UHFFFAOYSA-N 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 13
- 229910052799 carbon Inorganic materials 0.000 abstract description 11
- 239000002131 composite material Substances 0.000 abstract description 3
- 238000010791 quenching Methods 0.000 abstract description 3
- 230000000171 quenching effect Effects 0.000 abstract description 3
- 239000003381 stabilizer Substances 0.000 abstract description 3
- 230000004048 modification Effects 0.000 description 7
- 238000012986 modification Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 239000007822 coupling agent Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 4
- 239000006087 Silane Coupling Agent Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 3
- 238000002189 fluorescence spectrum Methods 0.000 description 3
- 125000000524 functional group Chemical group 0.000 description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 3
- 238000007112 amidation reaction Methods 0.000 description 2
- 238000005576 amination reaction Methods 0.000 description 2
- 229960005070 ascorbic acid Drugs 0.000 description 2
- 235000010323 ascorbic acid Nutrition 0.000 description 2
- 239000011668 ascorbic acid Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000000295 emission spectrum Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000000695 excitation spectrum Methods 0.000 description 2
- DPBLXKKOBLCELK-UHFFFAOYSA-N pentan-1-amine Chemical group CCCCCN DPBLXKKOBLCELK-UHFFFAOYSA-N 0.000 description 2
- 229920006381 polylactic acid film Polymers 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 230000009435 amidation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000011852 carbon nanoparticle Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002059 diagnostic imaging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229940100684 pentylamine Drugs 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
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Abstract
The invention discloses a preparation method of an aminated carbon quantum dot degradable fluorescent film, which comprises the following steps: s1: adding pentaerythritol and oleylamine into absolute ethyl alcohol, performing ultrasonic dispersion for 7min to uniformly mix the materials, transferring the materials into a polytetrafluoroethylene-lined reaction kettle, performing solvothermal reaction at 120-150 ℃ for 4-8h, performing rotary evaporation, dissolving the obtained dark brown product into acetone, adding a catalyst, stirring and dissolving to obtain an amino carbon quantum dot solution; s2: and dissolving carboxyl-terminated polylactic acid in dichloromethane to prepare a polylactic acid solution with the weight percent of 5%, dropwise adding an amino carbon quantum dot solution into the polylactic acid solution, stirring and reacting for 1-3h, coating the polylactic acid solution on a quartz plate, and naturally airing to obtain the amino carbon quantum dot degradable fluorescent film. According to the invention, the quaternium is used as a carbon source for the first time, the oleylamine is used as a stabilizer to prepare the aminated carbon quantum dot, and the aminated carbon quantum dot is grafted to the long chain end of the polylactic acid, so that the composite stability of the quaternium and the oleylamine is improved, the fluorescence quenching of the carbon quantum dot is inhibited, and the fluorescence stability of the carbon quantum dot is improved.
Description
Technical Field
The invention belongs to the field of fluorescent film preparation, and particularly relates to a preparation method of an aminated carbon quantum dot degradable fluorescent film.
Background
The carbon quantum dots (CarbonQuantumDots, CQDs), also called carbon dots or carbon nano dots, are zero-dimensional carbon nano materials with remarkable fluorescence performance, are composed of ultrafine, dispersed, quasi-spherical carbon nano particles with the size lower than 10nm, and have good application prospects in many fields of medical imaging technology, environment monitoring, chemical analysis, catalyst preparation, energy development and the like. The existing preparation method of the carbon quantum dots comprises two main types: top-down (top-down) and bottom-up (bottom-up) respectively, the "top-down" method includes: arc discharge, laser ablation, electrochemical; the "bottom-up" method includes: hydrothermal method, chemical oxidation method, microwave synthesis method, and template method. When preparing the carbon quantum dots from top to bottom, the carbon sources used are carbon nanotubes, carbon fibers, graphite rods, carbon ash, active carbon and the like. The chemical structure and optical properties of the carbon quantum dots are various due to different preparation methods and different carbon source types of CQDs, so that the carbon quantum dots can better meet the needs of various practical applications.
The CQDs fluorescent film is formed by compounding carbon quantum dots and a polymer film forming agent, but due to poor compatibility of inorganic matters of the carbon quantum dots and an organic polymer, the stability and mechanical property of the CQDs fluorescent film are poor, and in order to change the current situation, researchers adopt a coupling agent to carry out surface modification on the CQDs so as to enable the CQDs fluorescent film to carry out cross-linking with the polymer, but the modification effect of the coupling agent causes the surface of the CQDs to be covered or coated with a layer of non-luminous coupling agent medium, so that the fluorescence property of the CQDs fluorescent film is affected.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of an amino carbon quantum dot degradable fluorescent film.
The technical scheme of the invention is summarized as follows:
the preparation method of the degradable fluorescent film of the aminated carbon quantum dot comprises the following steps:
s1: adding pentaerythritol and oleylamine into absolute ethanol, performing ultrasonic dispersion for 7min to uniformly mix the materials, transferring the materials into a polytetrafluoroethylene-lined reaction kettle, performing solvothermal reaction at 120-150 ℃ for 4-8h, performing rotary evaporation to remove absolute ethanol solvent, and performing rotary evaporation to obtain the product
Dissolving the obtained dark brown product in acetone, adding a catalyst, stirring and dissolving to obtain an aminated carbon quantum dot solution;
s2: and dissolving carboxyl-terminated polylactic acid in dichloromethane to prepare a polylactic acid solution with the weight percent of 5%, dropwise adding an amino carbon quantum dot solution into the polylactic acid solution, stirring and reacting for 1-3h, coating the polylactic acid solution on a quartz plate, and naturally airing to obtain the amino carbon quantum dot degradable fluorescent film.
Preferably, the catalyst is dicyclohexylcarbodiimide.
Preferably, the dosage ratio of the pentaerythritol, the oleylamine, the absolute ethyl alcohol, the acetone and the catalyst is (0.1-0.5) g (0.18-0.8) g, 100mL:10mL (0.01-0.02) g.
Preferably, the volume ratio of the aminated carbon quantum dot solution to the 5wt% polylactic acid solution is 1: (1-4). The invention has the beneficial effects that:
according to the invention, the quaternary tetramine is used as a carbon source and the oleylamine is used as a stabilizer for the first time, the amination carbon quantum dot is prepared by a solvothermal method, under the catalysis of dicyclohexylcarbodiimide, an amino functional group rich in the surface of the amino functional group reacts with carboxyl-terminated polylactic acid in an amidation manner, and then the fluorescent carbon quantum dot is grafted to the long chain end of the polylactic acid, and is stably embedded in the polylactic acid film in a chemical bond manner, so that the composite stability of the two is improved, meanwhile, the fluorescence quenching of the carbon quantum dot is effectively inhibited, the fluorescence stability of the carbon quantum dot is improved, compared with the traditional silane coupling agent modification mode, the surface modification of a non-luminous intermediate is not needed, the fluorescent amination carbon quantum dot is directly connected with the polylactic acid in a covalent manner, the absorption of non-luminous silane coupling agent to fluorescence is avoided, and the fluorescence efficiency is greatly improved.
Drawings
FIG. 1 is an ultraviolet-visible absorption spectrum, an excitation spectrum and an emission spectrum of the aminated carbon quantum dot prepared in example 1;
FIG. 2 is a fluorescence spectrum of the carbon quantum dot degradable fluorescent film prepared in examples 1-4 and comparative example;
FIG. 3 is a flow chart of a preparation method of the degradable fluorescent film of the aminated carbon quantum dot.
Detailed Description
The present invention is described in further detail below with reference to examples to enable those skilled in the art to practice the same by referring to the description.
The invention discloses a preparation method of an amino carbon quantum dot degradable fluorescent film, which comprises the following steps:
s1: adding pentaerythritol and oleylamine into absolute ethyl alcohol, performing ultrasonic dispersion for 7min to uniformly mix the materials, transferring the materials into a polytetrafluoroethylene-lined reaction kettle, performing solvothermal reaction at 120-150 ℃ for 4-8h, performing rotary evaporation to remove absolute ethyl alcohol solvent, dissolving the obtained dark brown product into acetone, adding a catalyst dicyclohexylcarbodiimide, and stirring and dissolving to obtain an aminated carbon quantum dot solution; the dosage ratio of the quaternary tetramine, the oleylamine, the absolute ethyl alcohol, the acetone and the catalyst is (0.1-0.5) g (0.18-0.8) g:100mL:10mL (0.01-0.02) g;
s2: dissolving carboxyl-terminated polylactic acid in dichloromethane to prepare a polylactic acid solution with the weight percent of 5%, dropwise adding an amino carbon quantum dot solution into the polylactic acid solution, stirring and reacting for 1-3h, coating the mixture on a quartz plate, and naturally airing the mixture to obtain the amino carbon quantum dot degradable fluorescent film; the volume ratio of the aminated carbon quantum dot solution to the 5wt% polylactic acid solution is 1: (1-4).
Example 1
The preparation method of the degradable fluorescent film of the aminated carbon quantum dot comprises the following steps:
s1: adding 0.1g of pentaerythritol and 0.18g of oleylamine into 100mL of absolute ethyl alcohol, performing ultrasonic dispersion for 7min to uniformly mix the materials, transferring the materials into a polytetrafluoroethylene-lined reaction kettle, performing solvothermal reaction at 130 ℃ for 8h, performing rotary evaporation until absolute ethyl alcohol solvent is removed, dissolving the obtained dark brown product (showing strong blue light under a 365nm ultraviolet lamp and indicating the formation of fluorescent aminated carbon quantum dots) into 10mL of acetone, adding 0.01g of catalyst dicyclohexylcarbodiimide, and stirring and dissolving to obtain an aminated carbon quantum dot solution;
s2: 3.4737g of carboxyl-terminated polylactic acid is dissolved in 50mL of dichloromethane to prepare a 5wt% polylactic acid solution;
and then, dropwise adding 10mL of the aminated carbon quantum dot solution into 10mL of the 5wt% polylactic acid solution, stirring and reacting for 1h, coating the solution on a quartz plate, and naturally airing to obtain the aminated carbon quantum dot degradable fluorescent film.
Fig. 1 is an ultraviolet-visible absorption spectrum, an excitation spectrum and an emission spectrum of the aminated carbon quantum dot prepared in example 1: as can be seen from fig. 1, the absorption peak of the ultraviolet-visible absorption spectrum of the aminated carbon quantum dot at 340nm belongs to N-pi transition of-n=n-, and is colorless and transparent under natural light, and shows strong blue light under 365nm ultraviolet light; in the fluorescence spectrum, the carbon quantum dot has a maximum emission peak at 515nm under 435nm excitation.
Example 2 is identical to example 1, except that: and S2, dropwise adding 10mL of the aminated carbon quantum dot solution into 20mL of the 5wt% polylactic acid solution, stirring and reacting for 1h, coating on a quartz plate, and naturally airing to obtain the aminated carbon quantum dot degradable fluorescent film.
Example 3 is identical to example 1, except that: and S2, dropwise adding 10mL of the aminated carbon quantum dot solution into 30mL of the 5wt% polylactic acid solution, stirring and reacting for 1h, coating on a quartz plate, and naturally airing to obtain the aminated carbon quantum dot degradable fluorescent film.
Example 4 is identical to example 1, except that: and S2, dropwise adding 10mL of the aminated carbon quantum dot solution into 40mL of the 5wt% polylactic acid solution, stirring and reacting for 1h, coating on a quartz plate, and naturally airing to obtain the aminated carbon quantum dot degradable fluorescent film.
The comparative example uses ascorbic acid as a carbon source and N-beta- (aminoethyl) -gamma-aminopropyl trimethoxy silane as a coupling agent to prepare a fluorescent film, and the preparation method comprises the following steps:
s1: adding 0.1g of ascorbic acid and 0.18g of oleylamine into 100mL of absolute ethyl alcohol, performing ultrasonic dispersion for 7min to uniformly mix the two materials, transferring the two materials into a polytetrafluoroethylene-lined reaction kettle, performing solvothermal reaction at 130 ℃ for 8h, performing rotary evaporation until absolute ethyl alcohol solvent is removed, mixing and stirring the obtained dark brown product with 0.1g of N-beta- (aminoethyl) -gamma-aminopropyl trimethoxysilane for 0.5h, dissolving the obtained mixture into 10mL of acetone, adding 0.01g of catalyst dicyclohexylcarbodiimide, and stirring and dissolving the mixture to obtain a silane modified carbon quantum dot solution;
s2: 3.4737g of carboxyl-terminated polylactic acid is dissolved in 50mL of dichloromethane to prepare a 5wt% polylactic acid solution;
and then, dropwise adding 10mL of silane modified carbon quantum dot solution into 10mL of 5wt% polylactic acid solution, stirring and reacting for 1h, coating on a quartz plate, and naturally airing to obtain the carbon quantum dot degradable fluorescent film.
Fig. 2 is a fluorescence spectrum of the carbon quantum dot degradable fluorescent film prepared in examples 1 to 4 and comparative example: as can be seen from FIG. 2, the carbon quantum dot solutions of examples 1-4 are unchanged, under the excitation of 435nm wavelength light, the fluorescence intensity is gradually decreased along with the increase of the dichloromethane solution ratio of the carboxyl-terminated polylactic acid, and meanwhile, the fluorescent film of example 1 is far higher than that of the comparative example as compared with the patterns of comparative example 1, because the coupling agent absorbs fluorescence in the aminosilane modified carbon quantum dot of the comparative example, and the aminated carbon quantum dot prepared by taking the quaternium as a carbon source of example 1 is directly combined with the carboxyl-terminated polylactic acid, so that the structural stability of the film is solved, and the fluorescence performance of the film is greatly ensured.
In the embodiment 1-4, the quaternary pentylamine is used as a carbon source and the oleylamine is used as a stabilizer for the first time, the solvothermal method is used for preparing the aminated carbon quantum dot, the amino functional group rich in the surface of the aminated carbon quantum dot and the carboxyl-terminated polylactic acid are subjected to amidation reaction under the catalysis of dicyclohexylcarbodiimide, and then the fluorescent carbon quantum dot is grafted to the tail end of a long chain of the polylactic acid, and is stably embedded in the polylactic acid film in a chemical bond mode, so that the composite stability of the two is improved, meanwhile, the fluorescence quenching of the carbon quantum dot is effectively inhibited, the fluorescence stability of the carbon quantum dot is improved, compared with the traditional silane coupling agent modification mode, the surface modification of a non-luminous intermediate is not needed, the fluorescent aminated carbon quantum dot is directly connected with the polylactic acid in a covalent mode, the absorption of the non-luminous silane coupling agent to fluorescence is avoided, and the fluorescence efficiency is greatly improved.
Although embodiments of the present invention have been disclosed above, it is not limited to the use of the description and embodiments, it is well suited to various fields of use for the invention, and further modifications may be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the particular details without departing from the general concepts defined in the claims and the equivalents thereof.
Claims (4)
1. The preparation method of the degradable fluorescent film of the aminated carbon quantum dot is characterized by comprising the following steps of:
s1: adding pentaerythritol and oleylamine into absolute ethyl alcohol, performing ultrasonic dispersion for 7min to uniformly mix the materials, transferring the materials into a polytetrafluoroethylene-lined reaction kettle, performing solvothermal reaction at 120-150 ℃ for 4-8h, performing rotary evaporation to remove absolute ethyl alcohol solvent, dissolving the obtained dark brown product into acetone, adding a catalyst, stirring and dissolving to obtain an aminated carbon quantum dot solution;
s2: and dissolving carboxyl-terminated polylactic acid in dichloromethane to prepare a polylactic acid solution with the weight percent of 5%, dropwise adding an amino carbon quantum dot solution into the polylactic acid solution, stirring and reacting for 1-3h, coating the polylactic acid solution on a quartz plate, and naturally airing to obtain the amino carbon quantum dot degradable fluorescent film.
2. The method for preparing the degradable fluorescent film of the aminated carbon quantum dot according to claim 1, wherein the catalyst is dicyclohexylcarbodiimide.
3. The preparation method of the degradable fluorescent film for the aminated carbon quantum dots, which is characterized in that the dosage ratio of the quaternary tetramine to the oleylamine to the anhydrous ethanol to the acetone to the catalyst is (0.1-0.5) g (0.18-0.8) g to 100mL to 10mL (0.01-0.02) g.
4. The method for preparing the degradable fluorescent film of the aminated carbon quantum dots according to claim 1, wherein the volume ratio of the aminated carbon quantum dot solution to the 5wt% polylactic acid solution is 1: (1-4).
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104371730A (en) * | 2014-10-23 | 2015-02-25 | 云南民族大学 | Poly-a-hydroxy acid modified CdTe quantum dot and preparation method thereof |
| CN109054820A (en) * | 2018-07-11 | 2018-12-21 | 苏州星烁纳米科技有限公司 | The preparation method of carbon quantum dot |
| CN109097038A (en) * | 2018-09-29 | 2018-12-28 | 太原理工大学 | A kind of solid yellow fluorescent carbon quantum dot and preparation method thereof |
| CN110157422A (en) * | 2019-04-25 | 2019-08-23 | 云南大学 | A kind of preparation method of amination carbon quantum dot |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104371730A (en) * | 2014-10-23 | 2015-02-25 | 云南民族大学 | Poly-a-hydroxy acid modified CdTe quantum dot and preparation method thereof |
| CN109054820A (en) * | 2018-07-11 | 2018-12-21 | 苏州星烁纳米科技有限公司 | The preparation method of carbon quantum dot |
| CN109097038A (en) * | 2018-09-29 | 2018-12-28 | 太原理工大学 | A kind of solid yellow fluorescent carbon quantum dot and preparation method thereof |
| CN110157422A (en) * | 2019-04-25 | 2019-08-23 | 云南大学 | A kind of preparation method of amination carbon quantum dot |
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