CN108530346A - A kind of preparation method of N-serve and its preparation method of catalyst and catalyst - Google Patents
A kind of preparation method of N-serve and its preparation method of catalyst and catalyst Download PDFInfo
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- CN108530346A CN108530346A CN201810425361.9A CN201810425361A CN108530346A CN 108530346 A CN108530346 A CN 108530346A CN 201810425361 A CN201810425361 A CN 201810425361A CN 108530346 A CN108530346 A CN 108530346A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/61—Halogen atoms or nitro radicals
-
- 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
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0277—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides comprising ionic liquids, as components in catalyst systems or catalysts per se, the ionic liquid compounds being used in the molten state at the respective reaction temperature
- B01J31/0292—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides comprising ionic liquids, as components in catalyst systems or catalysts per se, the ionic liquid compounds being used in the molten state at the respective reaction temperature immobilised on a substrate
- B01J31/0295—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides comprising ionic liquids, as components in catalyst systems or catalysts per se, the ionic liquid compounds being used in the molten state at the respective reaction temperature immobilised on a substrate by covalent attachment to the substrate, e.g. silica
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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
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0277—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides comprising ionic liquids, as components in catalyst systems or catalysts per se, the ionic liquid compounds being used in the molten state at the respective reaction temperature
- B01J31/0298—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides comprising ionic liquids, as components in catalyst systems or catalysts per se, the ionic liquid compounds being used in the molten state at the respective reaction temperature the ionic liquids being characterised by the counter-anions
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Pyridine Compounds (AREA)
- Catalysts (AREA)
Abstract
A kind of preparation method of 2 chlorine, 6 trichloromethyl pyridine and its preparation method of catalyst and catalyst, belong to and prepare 2 chlorine, 6 trichloromethyl pyridine field.A kind of catalyst being used to prepare 2 chlorine, 6 trichloromethyl pyridine comprising carrier and iron content pyridine chloride salt ions liquid, iron content pyridine chloride salt ions fluid load is on carrier.This catalyst is by carrier, substantially increasing the contact area of catalyst and reactant, can improve the preparation efficiency of 2 chlorine, 6 trichloromethyl pyridine iron content pyridine chloride salt ions fluid load.In addition the invention further relates to a kind of preparation method preparing the above-mentioned catalyst for being used to prepare 2 chlorine, 6 trichloromethyl pyridine and a kind of preparation method of 2 chlorine, 6 trichloromethyl pyridine, overcome tradition prepare 2 chlorine, 6 trichloromethyl pyridine method there are reaction temperatures it is excessively high, product yield is low and catalyst inactivation is not easy to regenerate the shortcomings of.
Description
Technical field
The present invention relates to prepare N-serve field, and the chloro- 6- trichloromethyls of more particularly to a kind of 2-
The preparation method and its catalyst of pyridine and the preparation method of catalyst.
Background technology
N-serve is a kind of important nitrification inhibitor, can efficiently inhibit to nitrify in soil thin
The activity of bacterium, to alleviate the reaction speed that soil ammonium-state is converted into nitrate nitrogen.Ammonium nitrogen can by soil colloid adsorb and
It not easily runs off, to improve the utilization ratio of fertilizer.But under the conditions of Soil ventilation, ammonium nitrogen can under microbial action
To be converted into nitrate nitrogen, but nitrate nitrogen has been lost in, and the utilization rate of nitrogenous fertilizer is caused to decline.Therefore, N-serve is made
There is very important practical value in agricultural production for nitrification inhibitor use.
Traditional catalyst prepare N-serve method that there are reaction temperatures is excessively high, product yield is low and
Catalyst inactivation is not easy the shortcomings of regenerating.
Invention content
The first object of the present invention is to provide a kind of catalyst being used to prepare N-serve, this is urged
Agent can improve the preparation efficiency for preparing N-serve.
The second object of the present invention is to provide a kind of preparation for the catalyst being used to prepare N-serve
Method, be used to prepare made from this preparation method N-serve catalyst can be used in catalyzing and synthesizing 2- it is chloro-
The reaction of 6- trichloromethyl pyridines.
The third object of the present invention is to provide a kind of preparation method of N-serve, this preparation method
Simplicity, being capable of the chloro- 6- trichloromethyls pyrroles of the obtained 2- of high efficiency.
The present invention solves its technical problem using following technical scheme to realize.
The present invention proposes a kind of catalyst being used to prepare N-serve comprising carrier and iron content pyrrole
Pyridine chloride salt ions liquid, for iron content pyridine chloride salt ions fluid load on carrier, the structure of iron content pyridine chloride salt ions liquid is logical
Formula is as follows:
Wherein R1And R2It is alkyl.
The present invention also proposes a kind of preparation side preparing the above-mentioned catalyst for being used to prepare N-serve
Method is used to prepare urging for N-serve by the way that iron content pyridine chloride salt ions fluid load to be made on carrier
Agent.
The present invention also proposes a kind of preparation method of N-serve, and the chloro- 6- of 2- are used to prepare using above-mentioned
N-serve is obtained by the reaction in the catalyst 2- picolines and nitrogen of trichloromethyl pyridine.
The advantageous effect of the embodiment of the present invention is:
A kind of catalyst being used to prepare N-serve provided by the invention, this catalyst will be by that will contain
Iron pyridine chloride salt ions fluid load substantially increases the contact area of catalyst and reactant, can improve system on carrier
For the preparation efficiency of N-serve, high product yield and its chlorination reaction temperature is reduced, and this catalyst is one
Kind long catalytic life and renewable free of contamination green catalyst.
A kind of preparation side preparing the above-mentioned catalyst for being used to prepare N-serve provided by the invention
Method, the obtained catalyst for being used to prepare N-serve that this preparation method can be easy are chloro- for synthesis 2-
6- trichloromethyl pyridines are significant.
A kind of preparation method of N-serve provided by the invention overcomes tradition and prepares the chloro- 6- of 2- tri-
The method of chloromethylpyridine there are reaction temperatures it is excessively high, product yield is low and catalyst inactivation is not easy to regenerate the shortcomings of, this preparation
Method is easy, and product yield is high, and chlorination reaction temperature is relatively low.
Specific implementation mode
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, builds according to normal condition or manufacturer
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Preparation method to a kind of N-serve of the embodiment of the present invention and its catalyst and catalysis below
The preparation method of agent is specifically described.
A kind of catalyst being used to prepare N-serve is provided in the embodiment of the present invention comprising carrier
With iron content pyridine chloride salt ions liquid, iron content pyridine chloride salt ions fluid load is on carrier, iron content pyridine chloride salt ions liquid
General structure it is as follows:
Wherein R1And R2It is alkyl.
Further, in a preferred embodiment of the present invention, the load capacity of carrier is 0.1~5.0wt%.Carrier includes molecule
Sieve, molecular sieve include arbitrary several in MCM-41, MCM-22, ZSM-5, ZSM-11, ZSM-22, SAPO-34 and Beta or one
Kind.
A kind of preparation method for the catalyst being used to prepare N-serve is provided in the embodiment of the present invention,
By the catalyst that iron content pyridine chloride salt ions fluid load is prepared to N-serve on carrier.
Further, in a preferred embodiment of the present invention, by molecular sieve, iron content pyridine chloride salt ions liquid and absolute ethyl alcohol
It is added to three-necked flask mixing, the mass ratio of the molecular sieve of addition, iron content pyridine chloride salt ions liquid and absolute ethyl alcohol is
1:(0.001~0.053):Then three-necked flask equipped with mixture is put into and has children outside the state plan ultrasound in device by (1~2), and dipping 12~
After for 24 hours, the catalyst for being used to prepare N-serve is obtained after dry 6~12h at 50~100 DEG C.
A kind of preparation method of N-serve is provided in the embodiment of the present invention, is used to prepare using above-mentioned
The catalyst 2- picolines and chlorine reaction of N-serve obtain N-serve.
Further, in a preferred embodiment of the present invention, first 2- picoline aqueous solution Liquid sample introductions pump is passed into
Gasifier gasification, the molar ratio of 2- picolines and water is 1 in 2- picoline aqueous solutions:(5~20), then by the 2- after gasification
With 10~100h after picoline aqueous solution, chlorine and inert gas mixing-1Volume space velocity be passed into be placed with and be used to prepare
It in the fixed bed reactors of the catalyst of N-serve, reacts at 180~240 DEG C, collects condensation production
Object carries out chromatography, and tail gas is passed through sodium hydrate aqueous solution, and the chloro- 6- trichloromethyl pyridines of 2- are made.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
A kind of preparation method for the catalyst being used to prepare N-serve is provided in the present embodiment.
MCM-41 molecular sieves, iron content pyridine chloride salt ions liquid and absolute ethyl alcohol are added to three-necked flask to be mixed,
The mass ratio of the MCM-41 molecular sieves of addition, iron content pyridine chloride salt ions liquid and absolute ethyl alcohol is 1:0.001:1, it then will dress
There is the three-necked flask of mixture to be put into ultrasound in excusing from death device, after impregnating 12h, obtains being used to prepare 2- after dry 12h at 80 DEG C
The load capacity of the catalyst of chloro- 6- trichloromethyl pyridines, MCM-41 molecular sieves is 0.1wt%.
Embodiment 2
A kind of preparation method for the catalyst being used to prepare N-serve is provided in the present embodiment.
Beta molecular sieves, iron content pyridine chloride salt ions liquid and absolute ethyl alcohol are added to three-necked flask to be mixed, added
The mass ratio of the Beta molecular sieves, iron content pyridine chloride salt ions liquid and the absolute ethyl alcohol that enter is 1:0.053:1, it then will be equipped with mixed
The three-necked flask for closing object is put into ultrasound in excusing from death device, after impregnating 12h, obtains after dry 12h being used to prepare 2- at 80 DEG C chloro-
The load capacity of the catalyst of 6- trichloromethyl pyridines, Beta molecular sieves is 5.0wt%.
Embodiment 3
A kind of preparation method for the catalyst being used to prepare N-serve is provided in the present embodiment.
ZSM-5 molecular sieve, iron content pyridine chloride salt ions liquid and absolute ethyl alcohol are added to three-necked flask to be mixed, added
The mass ratio of the ZSM-5 molecular sieve, iron content pyridine chloride salt ions liquid and the absolute ethyl alcohol that enter is 1:0.048:2, then it will be equipped with
The three-necked flask of mixture is put into ultrasound in excusing from death device, after impregnating for 24 hours, obtains being used to prepare 2- after dry 12h at 80 DEG C
The load capacity of the catalyst of chloro- 6- trichloromethyl pyridines, ZSM-5 molecular sieve is 4.6wt%.
Embodiment 4
A kind of preparation method for the catalyst being used to prepare N-serve is provided in the present embodiment.
ZSM-11 molecular sieves, iron content pyridine chloride salt ions liquid and absolute ethyl alcohol are added to three-necked flask to be mixed,
The mass ratio of the ZSM-11 molecular sieves of addition, iron content pyridine chloride salt ions liquid and absolute ethyl alcohol is 1:0.032:1, it then will dress
There is the three-necked flask of mixture to be put into ultrasound in excusing from death device, after impregnating 18h, obtains being used to prepare 2- after dry 12h at 50 DEG C
The load capacity of the catalyst of chloro- 6- trichloromethyl pyridines, ZSM-11 molecular sieves is 3.5wt%.
Embodiment 5
A kind of preparation method for the catalyst being used to prepare N-serve is provided in the present embodiment.
SAPO-34 molecular sieves, iron content pyridine chloride salt ions liquid and absolute ethyl alcohol are added to three-necked flask to be mixed,
The mass ratio of the SAPO-34 molecular sieves of addition, iron content pyridine chloride salt ions liquid and absolute ethyl alcohol is 1:0.024:1, then will
Three-necked flask equipped with mixture is put into ultrasound in excusing from death device, after impregnating 12h, is used to prepare after dry 6h at 100 DEG C
The load capacity of the catalyst of N-serve, SAPO-34 molecular sieves is 3.2wt%.
Embodiment 6
A kind of preparation method of N-serve is provided in the present embodiment.
First 2- picoline aqueous solution Liquid sample introductions are pumped and are passed into gasifier gasification, 2- in 2- picoline aqueous solutions
The molar ratio of picoline and water is 1:10, then will be after 2- picolines aqueous solution, chlorine and the inert gas mixing after gasification
With 10h-1Volume space velocity be passed into the fixed bed reaction for being placed with the catalyst that 1g is used to prepare N-serve
It in device, reacts at 180 DEG C, collects condensed product, carry out chromatography, tail gas is passed through sodium hydrate aqueous solution, and 2- is made
Chloro- 6- trichloromethyl pyridines, N-serve yield are 83.5%.
Embodiment 7
A kind of preparation method of N-serve is provided in the present embodiment.
First 2- picoline aqueous solution Liquid sample introductions are pumped and are passed into gasifier gasification, 2- in 2- picoline aqueous solutions
The molar ratio of picoline and water is 1:10, then will be after 2- picolines aqueous solution, chlorine and the inert gas mixing after gasification
With 80h-1Volume space velocity be passed into the fixed bed reaction for being placed with the catalyst that 1g is used to prepare N-serve
It in device, reacts at 240 DEG C, collects condensed product, carry out chromatography, tail gas is passed through sodium hydrate aqueous solution, and 2- is made
Chloro- 6- trichloromethyl pyridines, N-serve yield are 88.7%.
Embodiment 8
A kind of preparation method of N-serve is provided in the present embodiment.
First 2- picoline aqueous solution Liquid sample introductions are pumped and are passed into gasifier gasification, 2- in 2- picoline aqueous solutions
The molar ratio of picoline and water is 1:10, then will be after 2- picolines aqueous solution, chlorine and the inert gas mixing after gasification
With 100h-1Volume space velocity be passed into be placed with the catalyst that 1g is used to prepare N-serve fixed bed it is anti-
It answers in device, reacts at 240 DEG C, collect condensed product, carry out chromatography, tail gas is passed through sodium hydrate aqueous solution, is made
N-serve, N-serve yield are 85.8%.
Embodiment 9
A kind of preparation method of N-serve is provided in the present embodiment.
First 2- picoline aqueous solution Liquid sample introductions are pumped and are passed into gasifier gasification, 2- in 2- picoline aqueous solutions
The molar ratio of picoline and water is 1:5, then after 2- picolines aqueous solution, chlorine and the inert gas after gasification are mixed with
80h-1Volume space velocity be passed into the fixed bed reactors for being placed with the catalyst that 1g is used to prepare N-serve
In, it reacts at 240 DEG C, collects condensed product, carry out chromatography, tail gas is passed through sodium hydrate aqueous solution, and it is chloro- that 2- is made
6- trichloromethyl pyridines, N-serve yield are 89.4%.
Embodiment 10
A kind of preparation method of N-serve is provided in the present embodiment.
First 2- picoline aqueous solution Liquid sample introductions are pumped and are passed into gasifier gasification, 2- in 2- picoline aqueous solutions
The molar ratio of picoline and water is 1:20, then will be after 2- picolines aqueous solution, chlorine and the inert gas mixing after gasification
With 80h-1Volume space velocity be passed into the fixed bed reaction for being placed with the catalyst that 1g is used to prepare N-serve
It in device, reacts at 200 DEG C, collects condensed product, carry out chromatography, tail gas is passed through sodium hydrate aqueous solution, and 2- is made
Chloro- 6- trichloromethyl pyridines, N-serve yield are 81.4%.
In conclusion a kind of catalyst being used to prepare N-serve of the embodiment of the present invention, this catalysis
Agent by the way that iron content pyridine chloride salt ions fluid load on carrier, is substantially increased the contact area of catalyst and reactant,
The preparation efficiency for preparing N-serve, high product yield can be improved and reduce its chlorination reaction temperature, and this
Catalyst is a kind of long catalytic life and renewable free of contamination green catalyst.
A kind of preparation side preparing the above-mentioned catalyst for being used to prepare N-serve of the embodiment of the present invention
Method, the obtained catalyst for being used to prepare N-serve that this preparation method can be easy are chloro- for synthesis 2-
6- trichloromethyl pyridines are significant.
A kind of preparation method of N-serve of the embodiment of the present invention overcomes tradition and prepares the chloro- 6- of 2-
The method of trichloromethyl pyridine there are reaction temperatures it is excessively high, product yield is low and catalyst inactivation is not easy to regenerate the shortcomings of, this system
Preparation Method is easy, and product yield is high, and chlorination reaction temperature is relatively low.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of catalyst being used to prepare N-serve, which is characterized in that it includes carrier and iron content pyridine
Chloride salt ions liquid, the iron content pyridine chloride salt ions fluid load on the carrier, the iron content pyridine chloride salt ions liquid
The general structure of body is as follows:
Wherein R1And R2It is alkyl.
2. the catalyst according to claim 1 for being used to prepare N-serve, which is characterized in that described
The load capacity of carrier is 0.1~5.0wt%.
3. the catalyst according to claim 1 for being used to prepare N-serve, which is characterized in that described
Carrier includes molecular sieve, and the molecular sieve includes MCM-41, MCM-22, ZSM-5, ZSM-11, ZSM-22, SAPO-34 and Beta
In it is arbitrary several or a kind of.
4. a kind of prepare as claims 1 to 3 any one of them is used to prepare the catalyst of N-serve
Preparation method, which is characterized in that by the way that the use is made in the iron content pyridine chloride salt ions fluid load on the carrier
In the catalyst for preparing N-serve.
5. the preparation method of the catalyst according to claim 4 for being used to prepare N-serve, feature
It is comprising after the iron content pyridine chloride salt ions liquid, the carrier and solvent are mixed, it is ultrasonically treated,
It is dried to obtain the catalyst for being used to prepare N-serve.
6. the preparation method of the catalyst according to claim 5 for being used to prepare N-serve, feature
It is comprising after the iron content pyridine chloride salt ions liquid, the carrier and absolute ethyl alcohol are mixed, carry out at ultrasound
After reason, then 12 are impregnated~for 24 hours, it then obtains described being used to prepare chloro- tri- chloromethanes of 6- of 2- after dry 6~12h at 50~100 DEG C
The catalyst of yl pyridines.
7. the preparation method of the catalyst according to claim 6 for being used to prepare N-serve, feature
It is, when the carrier, the absolute ethyl alcohol and the iron content pyridine chloride salt ions liquid are mixed, the carrier, institute
The mass ratio for stating absolute ethyl alcohol and the iron content pyridine chloride salt ions liquid is followed successively by 1:(0.001~0.053):(1~2).
8. a kind of preparation method of N-serve, which is characterized in that using such as any one of claim 1~2 institute
The catalyst 2- picolines for being used to prepare N-serve and chlorine reaction stated obtain the chloro- 6- of 2- tri-
Chloromethylpyridine.
9. the preparation method of N-serve according to claim 8, which is characterized in that it includes by gas
2- picolines aqueous solution, chlorine and inert gas after change, which are passed through to be placed with, described is used to prepare the chloro- 6- trichloromethyls pyrroles of 2-
In the reactor of the catalyst of pyridine, collects condensed product and the N-serve is made.
10. the preparation method of N-serve according to claim 9, which is characterized in that reaction temperature is
180~240 DEG C, the molar ratio of 2- picolines and water described in the 2- picolines aqueous solution is 1:(5~20), gaseous mixture
The volume space velocity of body is 10~100h-1。
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Cited By (2)
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CN108658847A (en) * | 2018-05-07 | 2018-10-16 | 盐城工学院 | A kind of iron content pyridine chloride salt ions liquid and its preparation method and application |
CN109694346A (en) * | 2018-10-30 | 2019-04-30 | 浙江埃森化学有限公司 | The method that 2- picoline liquid phase Light chlorimation prepares N-serve |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108658847A (en) * | 2018-05-07 | 2018-10-16 | 盐城工学院 | A kind of iron content pyridine chloride salt ions liquid and its preparation method and application |
CN109694346A (en) * | 2018-10-30 | 2019-04-30 | 浙江埃森化学有限公司 | The method that 2- picoline liquid phase Light chlorimation prepares N-serve |
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