CN106884322A - A kind of preparation method of flame-resistant polyacrylonitrile fiber - Google Patents
A kind of preparation method of flame-resistant polyacrylonitrile fiber Download PDFInfo
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- CN106884322A CN106884322A CN201710221478.0A CN201710221478A CN106884322A CN 106884322 A CN106884322 A CN 106884322A CN 201710221478 A CN201710221478 A CN 201710221478A CN 106884322 A CN106884322 A CN 106884322A
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- fiber
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- flame
- polyacrylonitrile
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Classifications
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
- D06M14/18—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation
- D06M14/26—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin
- D06M14/28—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/68—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
- D06M11/70—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/402—Amides imides, sulfamic acids
- D06M13/432—Urea, thiourea or derivatives thereof, e.g. biurets; Urea-inclusion compounds; Dicyanamides; Carbodiimides; Guanidines, e.g. dicyandiamides
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
- D06M2101/28—Acrylonitrile; Methacrylonitrile
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a kind of preparation method of flame-resistant polyacrylonitrile fiber.Its preparation process is:Polyacrylonitrile fibre is placed in the acetone soln containing benzophenone (BP) and is impregnated, taking-up is placed on two-sided cross-fire under ultraviolet lamp, removal excess surface BP is cleaned after fiber sample is taken out with acetone soln, then fiber sample is placed in N hydroxymethyl acrylamide solutions and is impregnated, taking-up is placed on two-sided cross-fire under ultraviolet lamp, N NMAs is grafted to polyacrylonitrile fibre surface;Polyacrylonitrile fibre after grafting is placed in phosphoric acid solution and is reacted, cleaned and dried with distilled water after taking-up, obtain flame-resistant polyacrylonitrile fiber.The present invention is with benzophenone as initiator, N NMAs are grafted to polyacrylonitrile fibre surface using ultraviolet radiation graft technology, recycle chemical modification carries out phosphatizing treatment to polyacrylonitrile fibre, fiber is obtained good fire resistance, more meets actual production demand.
Description
Technical field
The present invention relates to textile product technical field, and in particular to a kind of preparation side of flame-resistant polyacrylonitrile fiber
Method.
Background technology
Fire frequently occurs in world wide, the serious safety of life and property for threatening people, and textile has turned into and draws
The main hidden danger of inside fire is sent out, in order to ensure the security of the lives and property, flame-retardancy requirements is proposed to textile all over the world, while
The standard and regulation of correlation are formulated, with the hair of international trade, entertainment industry, national defense construction, public fire protection and labourer safety
Exhibition, people are increasingly harsh to the use scope and flame-retardancy requirements of textile.Polyacrylonitrile fibre is former as a kind of important weaving
Material, has many advantages, such as:, warmth retention property good, bright in colour, soft to chemical reagent good stability, dyeability is good, but its
Flame retardant effect is not good, and limited oxygen index is minimum in synthetic fibers, therefore preparation flame-resistant polyacrylonitrile fiber has far-reaching meaning
Justice.
Chinese invention patent application number is flame-resistant polyacrylonitrile fiber and its manufacture method disclosed in the A of CN 1566421, is incited somebody to action
The fire retardant for preparing and the inorganic spinning dope blending of polyacrylonitrile, are configured to co-blended spinning stoste, and silk of respinning obtains poly- third
Alkene nitrile fiber, wherein fire retardant are APP (APP), or processed by silane coupler or titanate coupling agent
APP.The method use inorganic additive flame retardant APP is cheap and easy to get, non-toxic efficient, but in the spinning solution in add new thing
Matter, and addition is larger, is easily caused product and loses original excellent properties.
In order to solve the above problems, a kind of preparation method of flame-resistant polyacrylonitrile fiber is designed particularly necessary.
The content of the invention
For not enough present on prior art, the present invention seeks to be to provide a kind of system of flame-resistant polyacrylonitrile fiber
Preparation Method, flame-resistant polyacrylonitrile fiber is prepared using grafting by the way of chemical modification is combined, and keeps it former to greatest extent
Some premium properties, good flame retardation effect more meets the demand of actual production, it is easy to promote the use of.
To achieve these goals, the present invention is to realize by the following technical solutions:A kind of fire-retardant polyacrylonitrile is fine
The preparation method of dimension, its preparation process is:
(1) grafting process:Polyacrylonitrile fibre is placed in the acetone soln containing benzophenone (BP) is first impregnated, take out fiber
After sample, the min of two-sided cross-fire 5~60 under ultraviolet lamp is placed on, is cleaned with acetone soln after fiber sample is taken out
Remove the BP of excess surface;Then fiber sample is placed in certain density N hydroxymethyl acrylamide solution and is impregnated, taken out
After fiber sample, the min of two-sided cross-fire 5~60 under ultraviolet lamp is placed on, is grafted to N hydroxymethyl acrylamide
Polyacrylonitrile fibre surface;
(2) chemical modification process:Polyacrylonitrile fibre after grafting is placed in the certain density of the urea containing certain mass
Certain hour is reacted in phosphoric acid solution, is cleaned and is dried with distilled water after taking out fiber sample, obtain flame-resistant polyacrylonitrile fiber.
Preferably, the acetone soln containing BP in described step (1), wherein BP contents are 0.5~5%, fiber sample exists
Dip time in acetone soln containing BP is 1~10h.
Preferably, in the N hydroxymethyl acrylamide solution of described step (1) N hydroxymethyl acrylamide content
It is 10~60 %, dip time of the fiber sample in N hydroxymethyl acrylamide solution is 1~10h.
Preferably, phosphorus acid content is 10~60 wt%, phosphorylation in phosphatizing treatment maceration extract in described step (2)
At 30~60 DEG C, the reaction time is 1~10h for the reaction temperature control for the treatment of.
Preferably, the urea and the mass ratio of phosphoric acid in described step (2) are 10:1~1:1, phosphatizing treatment leaching
Phosphorus acid content is 10~60wt% in stain liquid.
Beneficial effects of the present invention:The mode being combined using crosslinking technology and chemical modification technique, phosphorus, nitrogen are drawn
Fiber surface is entered, fiber is obtained good fire resistance, excellent performance, flame-resistant polyacrylonitrile fiber tool prepared by the method
There is profound significance.
Specific embodiment
For technological means, creation characteristic, reached purpose and effect for making present invention realization are easy to understand, with reference to
Specific embodiment, is expanded on further the present invention.
This specific embodiment uses following technical scheme:A kind of preparation method of flame-resistant polyacrylonitrile fiber, its preparation
Step is:
(1) grafting process:Polyacrylonitrile fibre is placed in first 1~10 is impregnated in the acetone soln that BP contents are 0.5~5 %
H, after taking out fiber sample, is placed on the min of two-sided cross-fire 5~60 under ultraviolet lamp, with third after fiber sample is taken out
The BP of ketone solution cleaning removal excess surface;Then it is 10~60 % fiber sample to be placed in into N hydroxymethyl acrylamide content
1~10 h is impregnated in the aqueous solution, after taking out fiber sample, being placed under ultraviolet lamp carries out two-sided cross-fire 5~60
Min, makes N hydroxymethyl acrylamide be grafted to polyacrylonitrile fibre surface.
(2) chemical modification process:Phosphatizing treatment is carried out to fiber sample, its step is:At a temperature of 30~60 DEG C,
1~10 h of reaction in the phosphoric acid solution that phosphorus acid content is 10~60 % will be placed in by the fiber sample of grafting, takes out fiber-like
Cleaned and dried with distilled water after product, obtain flame-resistant polyacrylonitrile fiber.
This specific embodiment with benzophenone as initiator, using ultraviolet radiation graft technology by N hydroxymethyl acrylamide
Polyacrylonitrile fibre surface is grafted to, the method for recycling chemical modification carries out phosphatizing treatment to polyacrylonitrile fibre, so that
Flame-resistant polyacrylonitrile fiber is obtained, fiber is obtained good fire resistance, the method has wide market application foreground.
Embodiment 1:A kind of preparation method of flame-resistant polyacrylonitrile fiber, its preparation process is:
(1) grafting process:Polyacrylonitrile fibre is placed in first 1 h is impregnated in the acetone soln that BP contents are 1 %, take out fiber
After sample, the min of two-sided cross-fire 10 under ultraviolet lamp is placed on, is cleaned with acetone soln after fiber sample is taken out
Except the BP of excess surface;Then fiber sample is placed in the N hydroxymethyl acrylamide that N hydroxymethyl acrylamide content is 20 %
Impregnate 2h in solution, after taking out fiber sample, being placed under ultraviolet lamp carries out two-sided cross-fire 10min, makes N- hydroxyl first
Base acrylamide graft is to polyacrylonitrile fibre surface.
(2) chemical modification process:Phosphatizing treatment is carried out to fiber sample, its step is:At a temperature of 50 DEG C, will pass through
The fiber sample of grafting is placed in and 1h is reacted in the phosphoric acid solution that phosphorus acid content is 30%, is cleaned with distilled water after taking out fiber sample
And dry, obtain flame-resistant polyacrylonitrile fiber.
Embodiment 2:A kind of preparation method of flame-resistant polyacrylonitrile fiber, its preparation process is:
(1) grafting process:Polyacrylonitrile fibre is placed in first 1h is impregnated in the acetone soln that BP contents are 1 %, take out fiber
After sample, two-sided cross-fire 20min under ultraviolet lamp is placed on, cleans removal after fiber sample is taken out with acetone soln
The BP of excess surface;Then fiber sample is placed in the N hydroxymethyl acrylamide that N hydroxymethyl acrylamide content is 30 % molten
Impregnate 2h in liquid, after taking out fiber sample, being placed under ultraviolet lamp carries out two-sided cross-fire 20min, makes N- methylols
Acrylamide graft is to polyacrylonitrile fibre surface.
(2) chemical modification process:Phosphatizing treatment is carried out to fiber sample, its step is:At a temperature of 50 DEG C, will pass through
The fiber sample of grafting is placed in and 1h is reacted in the phosphoric acid solution that phosphorus acid content is 30%, is cleaned with distilled water after taking out fiber sample
And dry, obtain flame-resistant polyacrylonitrile fiber.
Embodiment 3:A kind of preparation method of flame-resistant polyacrylonitrile fiber, its preparation process is:
(1) grafting process:Polyacrylonitrile fibre is placed in first 1h is impregnated in the acetone soln that BP contents are 1 %, take out fiber
After sample, the min of two-sided cross-fire 20 under ultraviolet lamp is placed on, is cleaned with acetone soln after fiber sample is taken out
Except the BP of excess surface;Then fiber sample is placed in the N hydroxymethyl acrylamide that N hydroxymethyl acrylamide content is 30 %
Impregnate 2h in solution, after taking out fiber sample, being placed under ultraviolet lamp carries out two-sided cross-fire 20min, makes N- hydroxyl first
Base acrylamide graft is to polyacrylonitrile fibre surface.
(2) chemical modification process:Phosphatizing treatment is carried out to fiber sample, its step is:At a temperature of 50 DEG C, will pass through
The fiber sample of grafting is placed in and 1h is reacted in the phosphoric acid solution that phosphorus acid content is 40%, is cleaned with distilled water after taking out fiber sample
And dry, obtain flame-resistant polyacrylonitrile fiber.
General principle of the invention and principal character and advantages of the present invention has been shown and described above.The technology of the industry
Personnel it should be appreciated that the present invention is not limited to the above embodiments, simply explanation described in above-described embodiment and specification this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appending claims and its
Equivalent thereof.
Claims (9)
1. a kind of preparation method of flame-resistant polyacrylonitrile fiber, it is characterised in that its preparation process is:
(1) grafting process:Polyacrylonitrile fibre is placed in the acetone soln containing benzophenone (BP) is first impregnated, take out fiber
Sample, is placed on the min of two-sided cross-fire 5~60 under ultraviolet lamp, is cleaned with acetone soln after fiber sample is taken out
Except the BP of excess surface;Then fiber sample is placed in certain density N hydroxymethyl acrylamide solution and is impregnated, take out fine
Dimension sample, is placed on the min of two-sided cross-fire 5~60 under ultraviolet lamp, N hydroxymethyl acrylamide is grafted to poly- third
Alkene nitrile fiber surface;
(2) chemical modification process:Polyacrylonitrile fibre after grafting is placed in the certain density of the urea containing certain mass
Certain hour is reacted in phosphoric acid solution, is cleaned and is dried with distilled water after taking out fiber sample, obtain flame-resistant polyacrylonitrile fiber.
2. a kind of preparation method of flame-resistant polyacrylonitrile fiber according to claim 1, it is characterised in that described step
(1) acetone soln containing BP in, wherein BP contents are 0.5~5%, dip time of the fiber sample in the acetone soln containing BP
It is 1~10h.
3. a kind of preparation method of flame-resistant polyacrylonitrile fiber according to claim 1, it is characterised in that described step
(1) content of N hydroxymethyl acrylamide is 10~60 % in N hydroxymethyl acrylamide solution, and fiber sample is in N- hydroxyl first
Dip time in base acrylamide solution is 1~10h.
4. a kind of preparation method of flame-resistant polyacrylonitrile fiber according to claim 1, it is characterised in that described step
(2) phosphorus acid content is 10~60 wt% in phosphatizing treatment maceration extract in.
5. a kind of preparation method of flame-resistant polyacrylonitrile fiber according to claim 1, it is characterised in that described step
(2) phosphatizing treatment in, at 30~60 DEG C, the reaction time is 1~10h to the control of its reaction temperature.
6. a kind of preparation method of flame-resistant polyacrylonitrile fiber according to claim 1, it is characterised in that described step
(2) urea and the mass ratio of phosphoric acid in are 10:1~1:1, phosphorus acid content is 10~60wt% in phosphatizing treatment maceration extract.
7. the preparation method of a kind of flame-resistant polyacrylonitrile fiber according to claim 1-6, it is characterised in that it prepares step
Suddenly it is:
(1) grafting process:Polyacrylonitrile fibre is placed in first 1 h is impregnated in the acetone soln that BP contents are 1 %, take out fiber
After sample, the min of two-sided cross-fire 10 under ultraviolet lamp is placed on, is cleaned with acetone soln after fiber sample is taken out
Except the BP of excess surface;Then fiber sample is placed in the N hydroxymethyl acrylamide that N hydroxymethyl acrylamide content is 20 %
Impregnate 2h in solution, after taking out fiber, being placed under ultraviolet lamp carries out two-sided cross-fire 10min, makes N- methylols third
Acrylamide is grafted to polyacrylonitrile fibre surface;
(2) chemical modification process:Phosphatizing treatment is carried out to fiber sample, its step is:At a temperature of 50 DEG C, will be by grafting
Fiber be placed in 1h reacted in the phosphoric acid solution that phosphorus acid content is 30%, cleaned and dried with distilled water after taking out fiber sample, obtain
To flame-resistant polyacrylonitrile fiber.
8. the preparation method of a kind of flame-resistant polyacrylonitrile fiber according to claim 1-6, it is characterised in that it prepares step
Suddenly it is:
(1) grafting process:Polyacrylonitrile fibre is placed in first 1h is impregnated in the acetone soln that BP contents are 1 %, take out fiber
After sample, two-sided cross-fire 20min under ultraviolet lamp is placed on, cleans removal after fiber sample is taken out with acetone soln
The BP of excess surface;Then fiber sample is placed in the N hydroxymethyl acrylamide that N hydroxymethyl acrylamide content is 30 % molten
Impregnate 2h in liquid, after taking out fiber sample, being placed under ultraviolet lamp carries out two-sided cross-fire 20min, makes N- methylols
Acrylamide graft is to polyacrylonitrile fibre surface;
(2) chemical modification process:Phosphatizing treatment is carried out to fiber sample, its step is:At a temperature of 50 DEG C, will be by grafting
Fiber sample be placed in 1h reacted in the phosphoric acid solution that phosphorus acid content is 30%, cleaned and dried with distilled water after taking out fiber sample
It is dry, obtain flame-resistant polyacrylonitrile fiber.
9. the preparation method of a kind of flame-resistant polyacrylonitrile fiber according to claim 1-6, it is characterised in that it prepares step
Suddenly it is:
(1) grafting process:Polyacrylonitrile fibre is placed in first 1h is impregnated in the acetone soln that BP contents are 1 %, take out fiber
After sample, the min of two-sided cross-fire 20 under ultraviolet lamp is placed on, is cleaned with acetone soln after fiber sample is taken out
Except the BP of excess surface;Then fiber sample is placed in the N hydroxymethyl acrylamide that N hydroxymethyl acrylamide content is 30 %
Impregnate 2h in solution, after taking out fiber sample, being placed under ultraviolet lamp carries out two-sided cross-fire 20min, makes N- hydroxyl first
Base acrylamide graft is to polyacrylonitrile fibre surface;
(2) chemical modification process:Phosphatizing treatment is carried out to fiber sample, its step is:At a temperature of 50 DEG C, will be by grafting
Fiber sample be placed in 1h reacted in the phosphoric acid solution that phosphorus acid content is 40%, cleaned and dried with distilled water after taking out fiber sample
It is dry, obtain flame-resistant polyacrylonitrile fiber.
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Citations (4)
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JPH03292351A (en) * | 1990-04-11 | 1991-12-24 | Asahi Chem Ind Co Ltd | Highly light-resistant and flame-retardant resin composition |
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CN101831804A (en) * | 2010-04-28 | 2010-09-15 | 北京化工大学 | Durable flame-retardant after-finishing method for fabric |
CN104610794A (en) * | 2013-11-01 | 2015-05-13 | 中国科学技术大学先进技术研究院 | Phosphor-nitrogen intumescent flame retardant, and synthetic method and applications thereof |
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2017
- 2017-04-06 CN CN201710221478.0A patent/CN106884322A/en active Pending
Patent Citations (4)
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JPH03292351A (en) * | 1990-04-11 | 1991-12-24 | Asahi Chem Ind Co Ltd | Highly light-resistant and flame-retardant resin composition |
CN101353863A (en) * | 2007-07-27 | 2009-01-28 | 中国石油化工股份有限公司 | Method for preparing flame-retardant anti-dripping fibre or fabric and flame-retardant anti-dripping fibre or fabric |
CN101831804A (en) * | 2010-04-28 | 2010-09-15 | 北京化工大学 | Durable flame-retardant after-finishing method for fabric |
CN104610794A (en) * | 2013-11-01 | 2015-05-13 | 中国科学技术大学先进技术研究院 | Phosphor-nitrogen intumescent flame retardant, and synthetic method and applications thereof |
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Title |
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