CN110511459A - A kind of fibre framework materials dipping solution, preparation method and dipping method - Google Patents
A kind of fibre framework materials dipping solution, preparation method and dipping method Download PDFInfo
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- CN110511459A CN110511459A CN201910822586.2A CN201910822586A CN110511459A CN 110511459 A CN110511459 A CN 110511459A CN 201910822586 A CN201910822586 A CN 201910822586A CN 110511459 A CN110511459 A CN 110511459A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
- C08L9/10—Latex
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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- Chemical Kinetics & Catalysis (AREA)
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- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a kind of fibre framework materials dipping solution, preparation method and dipping methods.Dipping solution includes 100 parts by weight of deionized water;Polyamines 1-5 parts by weight;Polyphenol 1-20 parts by weight;Sodium hydroxide 0.1-2 parts by weight;Latex 50-120 parts by weight;Impregnation fluid solid content is 10-30%.Preparation method is that polyamines, polyphenol and deionized water are added in reaction vessel, and sodium hydroxide is added and adjusts reaction solution pH, and mixed liquor is stirred to react under normal temperature conditions, and latex is added after reaction and continues to stir evenly, obtains the fibre framework materials dipping solution.Dipping method is the coating that fibre framework materials carry out dipping solution by the method for a bath dipping or two bath dippings, is then dried and is heat-treated.The present invention effectively substitutes the use of toxic raw material and intermediate in traditional RFL impregnation system, reduces the harm to human body and environment.
Description
Technical field
The invention belongs to impregnation technical fields, more particularly to a kind of fibre framework materials dipping solution, preparation method and leaching
Stain method.
Background technique
Fiber rubber composite material is composed of reinforcing fiber framework material and rubber matrix, and wherein rubber matrix is good
Good elasticity is used to the large deformation for bearing to generate when composite material stress, and fibre framework materials are because of its higher strength and stiffness
For resisting the destruction that stress generates composite material.Fiber rubber composite material is widely used in the high load automobile/aircraft wheel of high speed
Tire, anti-high pressure special type sebific duct and high-tenacity specific rubber conveyer belt etc..Interfacial adhesion performance between fiber and rubber matrix is determined
Determine the key that high-performance fiber enhancing plays stress transfer efficiency, the quality of bond properties, is directly related to rubber between the two
The safety and service life of product in use
In rubber industry production, in order to be glued between polarity and rigid difference very big fiber and rubber matrix
It closes, most common processing means are exactly to be carried out at traditional Resorcin-Formaldehyde-Latex (RFL) dipping to fibre framework materials
Reason.In RFL rubber shoe latex layer, functional group can be in conjunction with the polar group on fiber surface on RF resin, while RF resin is handed over
Rubber latex component in connection reticular structure can be acted on by co-vulcanization to be crosslinked with rubber matrix, so that fiber and rubber-based
Bonding transition zone is formed between body;Although RFL dipping technique is comparable mature and has lower production cost, face
Urgent need is protected to increasingly harsh environment, develops fiber novel environment friendly impregnation technology, substitution is industrially widely used
, poisonous and hazardous Resorcin-Formaldehyde-Latex (RFL) dipping technique is imminent.Formaldehyde was ground in 2009 by international cancer
Studying carefully center and being classified as leads to one of chemicals of leukaemia.In recent years, isophthalic was gone with regard to fibre framework materials impregnation system both at home and abroad
The research of diphenol and formolation has carried out a large amount of report.
International monopoly WO2014/175844A2 discloses a kind of environmentally friendly adhesive formula system, for bonding curtain
Cloth and rubber.The binding system component includes the acrylic resin containing carboxyl, epoxy resin, polyfunctionality enclosed type isocyanide
Acid esters or molecular weight 1000-10000g/mol base polyurethane prepolymer for use as and rubber latex, described in above for peel adhesion energy
The above for peel adhesion energy of slightly above RFL dipping fiber.
United States Patent (USP) 2015/0314644A1 discloses a kind of more for polyether-type by rubber latex, epoxide and main chain
The bonding formula of amine composition.The binding system overcomes influence of the amine to system stability.Without containing harmful in impregnation system
The ingredients such as resorcinol and formaldehyde, and reached RFL through the binding system adhesive strength that treated between fiber and rubber
The level of adhesion of dipping process.
United States Patent (USP) US4472463 discloses a kind of impregnation system formulation, for inactive polyester fiber two bath dipping
Processing.First by one or two kinds of acrylic monomers and a small amount of styrene copolymerized obtained acrylic resin, with this acrylic resin
Impregnation formula is mixed to prepare with latex.When for inactive polyester fiber, need by a traditional bath epoxide and/
Or blocked isocyanate activates fiber, two baths use novel acrylic resin-latex system impregnation, place
H extraction force outline between the fiber and rubber of reason is higher than the fiber of RFL dipping.
United States Patent (USP) US 2015/0259560A1 discloses one kind by acrylic resin, epoxide, polyisocyanates
With the fibre framework materials impregnation formula of latex composition.This method is used to improve adhesiveness between synthetic fibers and rubber,
And the formula composition is environment-protecting and non-poisonous.Bonding effect between its fiber and rubber for handling can reach traditional RFL processing
Level.
Therefore, the fiber dipping process system for developing novel environment friendly has become necessity, to replace in traditional RFL impregnation system
Resorcinol and toxic, the carcinogenic composition such as formaldehyde.
Summary of the invention
For the use for solving the problems, such as toxic component in tradition RFL system, the present invention provides a kind of leachings of fibre framework materials
Glue preparation method and dipping method.Before it can guarantee to meet the bond properties between fibre framework materials and rubber matrix
It puts, effectively substitutes the use of toxic raw material and intermediate in tradition RFL impregnation system, reduce the danger to human body and environment
Evil.
Dipping solution of the invention can effectively substitute the ingredients such as resorcinol and formaldehyde toxic in RFL impregnation system, together
When can satisfy bond properties between fibre framework materials and rubber matrix;On the one hand the process flow of this impregnation system is simple,
It does not need significantly to change prior art, on the other hand the dipping solution can store at room temperature, and preparation time is short, can
Carry out heavy industrialization application.The present invention is mixed to prepare fibre framework materials leaching using polyamines, polyphenol, sodium hydroxide and latex
Glue carries out impregnation to fibre framework materials using the dipping solution, enable to fibre framework materials and rubber matrix it
Between obtain preferable bond properties.
The purpose of the present invention is realized by following technical proposals:
An object of the present invention is to provide a kind of fibre framework materials dipping solution, including by weight with the following group
Point:
Existing all polyamines, preferably diethylenetriamine, dipropylenetriamine, octamethylenediamine, triethylene four can be used in polyamines
One or more of combinations of amine, tetraethylenepentamine, pentaethylene hexamine, polyethyleneimine or polyetheramine.
Polyphenol be preferably one of catechol, pyrogallol, gallic acid, tannic acid, catechin or anthocyanidin or
Several combinations.
Latex is preferably vinyl pyridine latex, styrene-butadiene latex, butadiene styrene vinyl pyridine latex, carboxylic styrene butadiene latex, carboxyl butyronitrile glue
The combination of one or more of cream, chlorosulfonated polyethylene latex, polychloroprene latex, NBR latex or hydrogenated butyronitrile latex.Latex
Solid content be preferably 20-50%.
Fibre framework materials are preferably cotton fiber, artificial silk, nylon 66 fiber, nylon 6 fiber, polyester PET fiber, polyester
One or more of PEN fiber, aramid fiber or ultra high molecular weight polyethylene fiber;The form of fiber is monofilament, cotton rope, sail
Cloth or cord.
Impregnation fluid solid content is 10-30%.
The second object of the present invention is to provide the preparation method of fibre framework materials dipping solution described above, method
Are as follows: polyamines, polyphenol and deionized water are added in reaction vessel, it is 8.0-12.0 that sodium hydroxide, which is added, and adjusts reaction solution pH,
1-5h is reacted under room temperature, rubber latex is added, and is continued to stir 0.5-6h under room temperature, is obtained the fibre framework materials dipping solution.
The third object of the present invention is to provide the dipping method of fibre framework materials dipping solution described above, method
Are as follows: fibre framework materials carry out the coating of dipping solution by the method for a bath dipping or two bath dippings, then carry out drying and heat
Processing.Drying temperature is 120-180 DEG C, and heat treatment temperature is 180-250 DEG C;Heat treatment time is 1-8min.
It is preferred that fibre framework materials are placed in the composition such as epoxide or epoxide and blocked isocyanate first
Activator in pre-process, drying heat treatment after, then impregnated again.
Have through fibre framework materials handled by environmentally friendly dipping solution of the invention with natural rubber and synthetic rubber
Higher adhesive strength, synthetic rubber include: butadiene-styrene rubber, butadiene rubber, nitrile rubber, ethylene propylene diene rubber, acrylate
Rubber, butyl rubber etc..
The preparation method of the environmentally friendly dipping solution of fibre framework materials, preparation method step by weight
It is as follows: polyamines, polyphenol and deionized water to be added in reaction vessel, it is 8.0- that sodium hydroxide, which is added, and adjusts reaction solution pH
12.0,1-5h is reacted under room temperature, rubber latex is added, continues to stir 0.5-6h under room temperature, obtains the fibre framework materials leaching
Glue makes final impregnation fluid solid content 10-30%.
The impregnation technology of the environmentally friendly fibre framework materials dipping solution: fibre framework materials by one bath dipping or
The method of two bath dippings carries out the coating of dipping solution, is then dried and is heat-treated, dried under the conditions of 120-180 DEG C,
1-8min is heat-treated under the conditions of 180-250 DEG C, fibre framework materials are directly placed in the one of said components when impregnating by a bath
Bathe impregnation in dipping solution.
Further, it can use conventional methods first: fibre framework materials are placed in epoxide or epoxidation
It closes and is pre-processed in the activator of object and blocked isocyanate composition, dried after being heat-treated, then soaked with dipping solution of the invention
Stain finally carries out drying heat treatment.
Prepared by the fibre framework materials of the environmentally friendly dipping solution impregnation and the composite material of rubber: by rubber
Item is put into mold ditch, then the fibre framework materials of impregnation are put into the ditch vertical with adhesive tape and fix upper end, lower end
The weight for hanging up 50g, is then covered with adhesive tape on fibre framework materials, covers die cover, is vulcanized on vulcanizing press.
Compared with prior art, the beneficial effects of the present invention are:
1, impregnation formula of liquid of the invention realizes no resorcinol and formaldehydeless use, not only drastically reduces to ring
The harm in border and human body, and dipping solution preparation and fiber impregnation simple process, the reaction time is short, is conducive to industrial production.
2, polyamines and polyphenol that the present invention mentions, one side polyamines and polyphenol can form network structure, polarity by reaction
Group can be with fiber-reactive;Rubber latex particle in another aspect network structure can participate in rubber matrix co-vulcanization, thus
Make have better bond properties between fibre framework materials and rubber.
3, dipping solution of the invention is placed viscosity for a long time at room temperature and not will increase dramatically, and is conducive to fiber skeleton material
The long term storage of dipping solution, is conducive to industrial applications in material dipping production process.
Specific embodiment
The present invention is further illustrated combined with specific embodiments below.
Embodiment 1
One bath uses traditional impregnation method.Component and its parts by weight are as follows: 92.4 parts of deionized waters, 3.2 parts of closings
Isocyanates, 1.3 parts of epoxy resin.
Two bath components and its parts by weight are as follows:
Preparation method are as follows: the deionized water of the above number, polyethyleneimine, pyrogallol and sodium hydroxide are added anti-
It answers in container, mixed liquor reacts 1.5h under normal temperature conditions, is uniformly mixed it, sufficiently reacts;Latex is continuously added, under room temperature
Continue to stir 2h, obtains the fibre framework materials dipping solution.
Wherein, fibre framework materials by one bath dipping or two bath dipping method carry out dipping solution coating, then into
Row drying and heat treatment.Drying temperature is 120 DEG C, and heat treatment temperature is 200 DEG C;Heat treatment time is 1min.It is first before dipping
First fibre framework materials are placed in the activator of the compositions such as epoxide or epoxide and blocked isocyanate and are located in advance
Then reason is impregnated again after drying heat treatment.
Embodiment 2
One bath uses traditional impregnation method;Component and its parts by weight are as follows: 92.4 parts of deionized waters, 3.2 parts of closings
Isocyanates, 1.3 parts of epoxy resin.
Two bath components and its parts by weight are as follows:
Preparation method are as follows: the deionized water of the above number, polyethyleneimine, pyrogallol and sodium hydroxide are added anti-
It answers in container, mixed liquor reacts 1h under normal temperature conditions, is uniformly mixed it, sufficiently reacts;Continuously add latex, under room temperature after
Continuous stirring 3h, obtains the fibre framework materials dipping solution.
Wherein, fibre framework materials by one bath dipping or two bath dipping method carry out dipping solution coating, then into
Row drying and heat treatment.Drying temperature is 120 DEG C, and heat treatment temperature is 230 DEG C;Heat treatment time is 1min.It is first before dipping
First fibre framework materials are placed in the activator of the compositions such as epoxide or epoxide and blocked isocyanate and are located in advance
Then reason is impregnated again after drying heat treatment.
Embodiment 3
One bath uses traditional impregnation method;Component and its parts by weight are as follows: 92.4 parts of deionized waters, 3.2 parts of closings
Isocyanates, 1.3 parts of epoxy resin.
Two bath components and its parts by weight are as follows:
Preparation method are as follows: the deionized water of the above number, polyethyleneimine, pyrogallol and sodium hydroxide are added anti-
It answers in container, mixed liquor reacts 2h under normal temperature conditions, is uniformly mixed it, sufficiently reacts;Continuously add latex, under room temperature after
Continuous stirring 4h, obtains the fibre framework materials dipping solution.
Wherein, fibre framework materials by one bath dipping or two bath dipping method carry out dipping solution coating, then into
Row drying and heat treatment.Drying temperature is 150 DEG C, and heat treatment temperature is 200 DEG C;Heat treatment time is 2min.It is first before dipping
First fibre framework materials are placed in the activator of the compositions such as epoxide or epoxide and blocked isocyanate and are located in advance
Then reason is impregnated again after drying heat treatment.
Embodiment 4
One bath uses traditional impregnation method;Component and its parts by weight are as follows: 92.4 parts of deionized waters, 3.2 parts of closings
Isocyanates, 1.3 parts of epoxy resin.
Two bath components and its parts by weight are as follows:
Preparation method are as follows: the deionized water of the above number, polyethyleneimine, pyrogallol and sodium hydroxide are added anti-
It answers in container, mixed liquor reacts 1.5h under normal temperature conditions, is uniformly mixed it, sufficiently reacts;Latex is continuously added, under room temperature
Continue to stir 2h, obtains the fibre framework materials dipping solution.
Wherein, fibre framework materials by one bath dipping or two bath dipping method carry out dipping solution coating, then into
Row drying and heat treatment.Drying temperature is 150 DEG C, and heat treatment temperature is 250 DEG C;Heat treatment time is 2min.It is first before dipping
First fibre framework materials are placed in the activator of the compositions such as epoxide or epoxide and blocked isocyanate and are located in advance
Then reason is impregnated again after drying heat treatment.
Embodiment 5
One bath uses traditional impregnation method;Component and its parts by weight are as follows: 92.4 parts of deionized waters, 3.2 parts of closings
Isocyanates, 1.3 parts of epoxy resin.
Two bath components and its parts by weight are as follows:
Preparation method are as follows: the deionized water of the above number, polyethyleneimine, pyrogallol and sodium hydroxide are added anti-
It answers in container, mixed liquor reacts 1h under normal temperature conditions, is uniformly mixed it, sufficiently reacts;Continuously add latex, under room temperature after
Continuous stirring 1h, obtains the fibre framework materials dipping solution.
Wherein, fibre framework materials by one bath dipping or two bath dipping method carry out dipping solution coating, then into
Row drying and heat treatment.Drying temperature is 120 DEG C, and heat treatment temperature is 250 DEG C;Heat treatment time is 2min.It is first before dipping
First fibre framework materials are placed in the activator of the compositions such as epoxide or epoxide and blocked isocyanate and are located in advance
Then reason is impregnated again after drying heat treatment.
Experimental data is shown in Table 1
Table 1
H extraction test is carried out to embodiment 1-5 and comparative example 1, standard GB/T/T2942-2009 is pressed in the test of H bonding force
In method tested.It is as follows (by weight to prepare the formula of standard rubbers used in H bonding force test sample
Meter): 100 parts of natural rubber (smoke sheet rubber), 40 parts of carbon black N330 (top grade product), 4 parts of zinc oxide (top grade product), sulphur (top grade product)
2.5 parts, 0.8 part of captax (top grade product), 2 parts of stearic acid (top grade product), 3 parts of aromatic naphtha (top grade product), antioxidant 4020 is (excellent
Grade product) 1.5 parts.It is 136 ± 2 DEG C that H, which extracts used curing temperature when prepared by sample out, and sulfurizing mould pressure is 3MPa, vulcanization
Time is 50min.Peel strength is by the method in the stripping methods such as Chang Meiying measurement 66 impregnation single cord bonding force document of polyamide fibre
It is tested, prepares standard rubbers used in peel strength test sample and be formulated (by weight) as follows: natural rubber
100 parts of glue (smoke sheet rubber), 40 parts of semi-reinforcing hydrocarbon black, 4 parts of zinc oxide, 2.5 parts of sulphur, 0.8 part of captax, 2 parts of stearic acid, pine
3 parts of tar, 0.75 part of antioxidant A, 0.75 part of antioxidant D.Used curing temperature is 160 when the preparation of peel strength sample
DEG C, sulfurizing mould pressure is 2.354MPa, vulcanization time 20min.
As seen from the results in Table 1, after different embodiments above is handled, the H of embodiment 1-2 is bonded p-aramid fiber cord fabric thread
Power is not much different with comparative example 1, and quite, the H bonding force of embodiment 4-5 is than comparative example 1 for the H bonding force and comparative example 1 of embodiment 3
It is slightly higher.Peel strength of the peel strength of embodiment 1-2 lower than comparative example, a little higher than comparative example of the peel strength of embodiment 3-4,
And the peel strength of embodiment 5 and comparative example maintain an equal level.This illustrates that dipping solution prepared by the present invention is not changing any bonding and object
In the case where rationality energy, the RFL impregnation formula of liquid containing pollution and carcinogenic resorcinol, formaldehyde harmful substance can be substituted and existed
It is used in the two-bath gum dipping system of p-aramid fiber.The results show that dipping solution prepared by the present invention can effectively promote polyester fibre
The bond properties for tieing up framework material and rubber, can reach traditional Resorcin-Formaldehyde-Latex (RFL) impregnation system substantially
Bonding effect, and green non-pollution.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of fibre framework materials dipping solution, which is characterized in that the dipping solution includes following components by weight:
2. fibre framework materials dipping solution according to claim 1, which is characterized in that the solid content of latex is 20-50%;
The solid content of dipping solution is 10-30%.
3. fibre framework materials dipping solution according to claim 1, which is characterized in that the polyamines be diethylenetriamine,
Dipropylenetriamine, octamethylenediamine, polyethylene polyamine, triethylene tetramine, tetraethylenepentamine, pentaethylene hexamine, polyethyleneimine or poly-
One or more of combinations of ether amines.
4. fibre framework materials dipping solution according to claim 2, which is characterized in that the latex is vinylpyridine glue
Cream, styrene-butadiene latex, butadiene styrene vinyl pyridine latex, carboxylic styrene butadiene latex, carboxylic acrylonitrile butadiene rubber latex, chlorosulfonated polyethylene latex, polychloroprene latex, fourth
The combination of one or more of nitrile latex or hydrogenated butyronitrile latex.
5. fibre framework materials dipping solution according to claim 1, which is characterized in that the polyphenol is catechol, neighbour
The combination of one or more of benzenetriol, gallic acid, tannic acid, catechin or anthocyanidin.
6. fibre framework materials dipping solution according to claim 1, which is characterized in that fibre framework materials be cotton fiber,
Artificial silk, nylon 66 fiber, nylon 6 fiber, polyester PET fiber, polyester PEN fiber, aramid fiber or superhigh molecular weight polyethylene
One or more of alkene fiber.
7. fibre framework materials dipping solution according to claim 6, which is characterized in that the form of fiber be monofilament, cotton rope,
Canvas or cord.
8. the preparation method of -7 any fibre framework materials dipping solutions according to claim 1, which is characterized in that will be more
Amine, polyphenol and deionized water are added in reaction vessel as reaction solution, are added sodium hydroxide and are adjusted reaction solution, make reaction solution
PH be 8.0-12.0, then at normal temperature react 1-5h after latex is added, continue under room temperature stir 0.5-6h, obtain fiber bone
Frame material dipping solution.
9. the dipping method of -7 any fibre framework materials dipping solutions according to claim 1, which is characterized in that fiber bone
Frame material carries out the coating of dipping solution by the method for a bath dipping or two bath dippings, is then dried and is heat-treated;Drying
Temperature is 110-180 DEG C, and heat treatment temperature is 180-250 DEG C, heat treatment time 1-8min.
10. the dipping method of fibre framework materials dipping solution according to claim 9, which is characterized in that first by fiber
Framework material is placed in the activator of epoxide or epoxide and blocked isocyanate composition and pre-processes, at drying heat
After reason, then impregnated again.
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CN112160169A (en) * | 2020-09-30 | 2021-01-01 | 北京化工大学 | Environment-friendly fiber dipping solution, preparation method and application |
CN112411196A (en) * | 2020-11-05 | 2021-02-26 | 陕西同华机电有限公司 | High-performance TPU coated fabric and preparation method thereof |
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CN113957717A (en) * | 2021-11-15 | 2022-01-21 | 安徽华烨特种材料有限公司 | Ultra-high molecular weight polyethylene fiber reinforced material and preparation method thereof |
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