CN108486686A - A kind of preparation process of High-performance graphene Nanowire vinylon and cotton blend - Google Patents
A kind of preparation process of High-performance graphene Nanowire vinylon and cotton blend Download PDFInfo
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- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
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Abstract
A kind of preparation process of High-performance graphene Nanowire vinylon and cotton blend of the present invention, steps are as follows:Prepare macromolecule spinning solution;Graphene stoste is added into macromolecule spinning solution and is mixed, forms composite spinning stoste after mixing;Composite spinning stoste inputs in the nozzle of spray gun;The composite spinning stoste is sprayed from nozzle using spray gun and enters wire drawing chamber, and the composite spinning stoste drop is drawn into a diameter of 100nm Nanowire vinylon and cotton blends below using the high temperature and pressure air that HTHP air generator generates.Special macromolecule spinning solution formula and preparation process can greatly improve the performance of spinning solution by unique complex antimicrobials and composite antioxidant, reinforce the anti-microbial property and antioxygen property of final products graphene nano fiber cotton.
Description
Technical field
The present invention relates to a kind of preparation processes of High-performance graphene Nanowire vinylon and cotton blend.
Background technology
Graphene(Graphene)It is a kind of two dimension that hexangle type being formed in honeycomb lattice with sp2 hybridized orbits by carbon atom
Carbon nanomaterial.Graphene has excellent optics, electricity, mechanical characteristic, in materialogy, micro-nano technology, the energy, biomedicine
It is with important application prospects with drug delivery etc., it is considered to be a kind of future revolutionary material.
Nanofiber refers to a diameter of nanoscale and the larger filamentary material with certain draw ratio of length, in addition,
Nano particle is filled into general fibre, nanofiber is also referred to as to the fiber that it is modified.It says in the narrow sense, nanofiber
Diameter between 1nm to 100nm, but in a broad sense, fiber of the fibre diameter less than 1000nm is referred to as nanofiber.It will
Graphene is combined in nanofiber, can obtain high intensity, big thermal coefficient, high conduction performance, and bigger serface etc. is excellent
Performance.Therefore develop it is a kind of can develop a kind of graphene be applied to the preparation process of Nanowire vinylon and cotton blend production increasingly by
To the concern of people.
Invention content
The present invention proposes the preparation process that a kind of high-performance is added to graphene nano fiber cotton regarding to the issue above.
Specific technical solution is as follows:
A kind of preparation process of High-performance graphene Nanowire vinylon and cotton blend, which is characterized in that preparation process is as follows:
(1)Prepare macromolecule spinning solution;
(2)Graphene stoste is added into macromolecule spinning solution and is mixed, forms composite spinning stoste after mixing;
(3)Composite spinning stoste inputs in the nozzle of spray gun;
(4)The composite spinning stoste is sprayed from nozzle using spray gun and enters wire drawing chamber, and is occurred using high temperature and pressure air
The composite spinning stoste drop is drawn into a diameter of 100nm Nanowire vinylon and cotton blends below by the high temperature and pressure air that device generates.
Further, the mixing quality ratio of the graphene stoste and the macromolecule spinning solution is 3-6:17-25.
Further, the preparation process of the graphene stoste is as follows:
(1)Graphite powder is taken to be mixed at normal temperatures with Strong oxdiative mixed liquor, mixing quality ratio is graphite powder:Strong oxdiative mixed liquor=
1:3,20~30min of incorporation time, stir speed (S.S.) 88r/min stand 1H after mixing, obtain primary liquid:
(2)Hydrogen peroxide will be added in primary liquid and stir evenly, the volume ratio of primary liquid and hydrogen peroxide is 7:5, mixing time is
30~60min, stir speed (S.S.) 110r/min stand 2~3H after the completion of stirring, obtain secondary liquid;
(3)Potassium permanganate powder will be added in secondary liquid, the mass ratio of secondary liquid and potassium permanganate is 3:1, it is stirred 25
~55min, temperature is maintained at 45~50 DEG C when mixing, and mixing rate is 135r/min, carries out after mixing for the first time
Ultrasonic oscillation, concussion time are 30~40min, and ultrasonic frequency is 40~60kHZ, obtains three-level liquid;
(4)Chlorine will be passed through in three-level liquid, the volume ratio of three-level liquid and chlorine is 10:13, the reaction time is 30~90min, instead
2H should be stood after the completion, second of ultrasonic oscillation is carried out after standing, and the concussion time is 60~90min, ultrasonic frequency 50
~77kHZ;Then centrifugal treating is carried out, deionized water is used in combination to wash out lower sediment, obtains graphene stoste.
Further, the grain size of the potassium permanganate powder is the mesh of 100 mesh~80.
Further, the grain size of the graphite powder is 10~100nm.
Further, Strong oxdiative mixed liquor is the mixed liquor of concentrated nitric acid solution and concentrated sulfuric acid solution, sulphur in concentrated sulfuric acid solution
The mass percent of acid is 85%, the mass percent position 75% of sulfuric acid, concentrated sulfuric acid solution and concentrated nitric acid solution in concentrated nitric acid solution
Mixed volume ratio be 4~9:5~11.
Further, the macromolecule spinning solution is by poly- the four of the mass parts of the 4 of 11~18 mass parts, 4 '-MDI, 5~7
Hydrogen furans ether glycol, the polyether triol of 1~2 mass parts, the polyoxypropylene diamine of 5~7 mass parts, the Isosorbide-5-Nitrae-of 2~3 mass parts
The antioxidant of butanediol, the antiseptic of 4~7 mass parts, 1~1.5 mass parts reacts 0.5~1.0 hour at 89~97 DEG C;
It is cooled to the sodium carboxymethylcellulose that 3~5 mass parts are added after room temperature, the polyvinylpyrrolidone of 6~8 mass parts, stirring is simultaneously
It can be obtained the macromolecule spinning solution after dispersion.
Further, the antiseptic is by dodecyl dimethyl benzyl ammonium bromide, myristyl benzyl dimethyl chlorination
Ammonium, stearyl dimethyl benzyl ammonium chloride, 2- n-octyl -4- isothiazoline -3- ketone are with mass ratio 3:4:1:7 ratio
It mixes.
Further, the antioxidant is by β-(4- hydroxyl -3,5- di-tert-butyl-phenyls)The positive octadecyl ester of propionic acid, four (β-(3,
5- di-tert-butyl-hydroxy phenyls)Propionic acid) pentaerythritol ester, phosphorous acid(Three nonyl phenyl)Ester is with mass ratio 3-4:1-4:3-6
Ratio mix.
Beneficial effects of the present invention are:
Special macromolecule spinning solution formula and preparation process, by unique complex antimicrobials and composite antioxidant,
The performance of spinning solution can be greatly improved, the anti-microbial property and antioxygen of final products graphene nano fiber cotton are reinforced
Performance.
The graphene stoste of special preparation, using multiple oxidation reaction, graphene stoste made from the method for fractional steps is oxidation stone
Black alkene stoste can be good at use in nanofiber making, containing abundant oxygen functional group, such as carboxyl, hydroxyl, epoxy group
It is easy to use Deng, this kind of stoste in use, direct plungeing into macromolecule spinning solution when nanofiber production.And energy
Nanofiber intensity, thermal coefficient, electric conductivity are enough increased substantially, using effect is good.
Specific implementation mode
It is clear to make technical scheme of the present invention be more clear, below the present invention is described further, it is any to this
The technical characteristic of inventive technique scheme carries out the scheme that equivalencing is obtained with conventional reasoning and each falls within the scope of the present invention.
Embodiment 1
A kind of preparation process of High-performance graphene Nanowire vinylon and cotton blend, preparation process are as follows:
(1)Antioxidant is prepared, by β-(4- hydroxyl -3,5- di-tert-butyl-phenyls)The positive octadecyl ester of propionic acid, four (β-(3,5- bis- tertiary fourths
Base -4- hydroxy phenyls)Propionic acid) pentaerythritol ester, phosphorous acid(Three nonyl phenyl)Ester is with mass ratio 3:1:3 ratio mixing, system
Obtain antioxidant;
(2)Antiseptic is prepared, by dodecyl dimethyl benzyl ammonium bromide, myristyl benzyl dimethyl ammonium chloride, octadecane
Base dimethyl benzyl ammonium chloride, 2- n-octyl -4- isothiazoline -3- ketone are with mass ratio 3:4:1:7 ratio mixing, is made
Antiseptic;
(3)Prepare macromolecule spinning solution;By the polytetrahydrofuran ether glycol of the mass parts of the 4 of 11 mass parts, 4 '-MDI, 5,1 matter
The polyether triol of amount part, the polyoxypropylene diamine of 5 mass parts, the 1,4-butanediol of 2 mass parts, the antiseptic of 4 mass parts, 1
The antioxidant of mass parts reacts 0.5 hour at 89 DEG C;It is cooled to the sodium carboxymethylcellulose that 3 mass parts are added after room temperature, 6 matter
The polyvinylpyrrolidone for measuring part, stirs and can be obtained the macromolecule spinning solution after disperseing;
(4)Graphene stoste is prepared, graphite powder is taken to be mixed at normal temperatures with Strong oxdiative mixed liquor, the grain size of the graphite powder is
10nm, Strong oxdiative mixed liquor are the mixed liquor of concentrated nitric acid solution and concentrated sulfuric acid solution, the quality percentage of sulfuric acid in concentrated sulfuric acid solution
Than being 85%, the mass percent position 75% of sulfuric acid, the mixed volume ratio of concentrated sulfuric acid solution and concentrated nitric acid solution in concentrated nitric acid solution
It is 4:5;Mixing quality ratio is graphite powder:Strong oxdiative mixed liquor=1:3, incorporation time 20min, stir speed (S.S.) 88r/min,
1H is stood after mixing, obtains primary liquid:Hydrogen peroxide will be added in primary liquid and stirs evenly, the body of primary liquid and hydrogen peroxide
Product is than being 7:5, mixing time 30min, stir speed (S.S.) 110r/min stand 2H after the completion of stirring, obtain secondary liquid;It will be secondary
Potassium permanganate powder is added in grade liquid, the grain size of potassium permanganate powder is 100 mesh;The mass ratio of secondary liquid and potassium permanganate is
3:1, it is stirred 25min, temperature is maintained at 45 DEG C when mixing, and mixing rate is 135r/min, is carried out after mixing
First time ultrasonic oscillation, concussion time are 30min, and ultrasonic frequency 40kHZ obtains three-level liquid;It will be passed through in three-level liquid
The volume ratio of chlorine, three-level liquid and chlorine is 10:13, reaction time 30min stand 2H, are carried out after standing after the completion of reaction
Second of ultrasonic oscillation, concussion time are 60min, ultrasonic frequency 50kHZ;Then carry out centrifugal treating, and spend from
Sub- water washes out lower sediment, obtains graphene stoste;
(5)With the mixing 3 of graphene stoste and the macromolecule spinning solution:17 mass ratio adds graphene stoste
Enter in macromolecule spinning solution and mixed, forms composite spinning stoste after mixing;
(6)Composite spinning stoste inputs in the nozzle of spray gun;
(7)The composite spinning stoste is sprayed from nozzle using spray gun and enters wire drawing chamber, and is occurred using high temperature and pressure air
The composite spinning stoste drop is drawn into a diameter of 100nm Nanowire vinylon and cotton blends below by the high temperature and pressure air that device generates.
Embodiment 2
A kind of preparation process of High-performance graphene Nanowire vinylon and cotton blend, preparation process are as follows:
(1)Antioxidant is prepared, by β-(4- hydroxyl -3,5- di-tert-butyl-phenyls)The positive octadecyl ester of propionic acid, four (β-(3,5- bis- tertiary fourths
Base -4- hydroxy phenyls)Propionic acid) pentaerythritol ester, phosphorous acid(Three nonyl phenyl)Ester is with mass ratio 4:4:6 ratio mixing, system
Obtain antioxidant;
(2)Antiseptic is prepared, by dodecyl dimethyl benzyl ammonium bromide, myristyl benzyl dimethyl ammonium chloride, octadecane
Base dimethyl benzyl ammonium chloride, 2- n-octyl -4- isothiazoline -3- ketone are with mass ratio 3:4:1:7 ratio mixing, is made
Antiseptic;
(3)Prepare macromolecule spinning solution;By the polytetrahydrofuran ether glycol of the mass parts of the 4 of 18 mass parts, 4 '-MDI, 5~7,
The polyether triol of 2 mass parts, the polyoxypropylene diamine of 7 mass parts, the 1,4-butanediol of 3 mass parts, the antibacterial of 7 mass parts
The antioxidant of agent, 1.5 mass parts reacts 1.0 hours at 97 DEG C;It is cooled to the carboxymethyl cellulose that 5 mass parts are added after room temperature
Sodium, the polyvinylpyrrolidone of 8 mass parts stir and can be obtained the macromolecule spinning solution after disperseing;
(4)Graphite powder is taken to be mixed at normal temperatures with Strong oxdiative mixed liquor, the grain size of the graphite powder is 100nm, Strong oxdiative mixing
Liquid is the mixed liquor of concentrated nitric acid solution and concentrated sulfuric acid solution, and the mass percent of sulfuric acid is 85% in concentrated sulfuric acid solution, and concentrated nitric acid is molten
The mixed volume ratio of the mass percent position 75% of sulfuric acid in liquid, concentrated sulfuric acid solution and concentrated nitric acid solution is 9:11;Mixing quality ratio
Example is graphite powder:Strong oxdiative mixed liquor=1:3, incorporation time 30min, stir speed (S.S.) 88r/min stand 1H after mixing,
Obtain primary liquid:Hydrogen peroxide will be added in primary liquid and stir evenly, the volume ratio of primary liquid and hydrogen peroxide is 7:5, when stirring
Between be 60min, stir speed (S.S.) 110r/min, stirring after the completion of stand 3H, obtain secondary liquid;High violent acid will be added in secondary liquid
The grain size of potassium powder, potassium permanganate powder is 80 mesh;The mass ratio of secondary liquid and potassium permanganate is 3:1, it is stirred
55min, temperature is maintained at 50 DEG C when mixing, and mixing rate is 135r/min, carries out first time ultrasonic wave after mixing
Concussion, concussion time are 40min, and ultrasonic frequency 60kHZ obtains three-level liquid;To be passed through chlorine in three-level liquid, three-level liquid with
The volume ratio of chlorine is 10:13, reaction time 90min stand 2H, second of ultrasonic wave shake are carried out after standing after the completion of reaction
It swings, the concussion time is 90min, ultrasonic frequency 77kHZ;Then centrifugal treating is carried out, is used in combination deionized water by lower sediment
It washes out, obtains graphene stoste;
(5)With the mixing 6 of graphene stoste and the macromolecule spinning solution:25 mass ratio adds graphene stoste
Enter in macromolecule spinning solution and mixed, forms composite spinning stoste after mixing;
(6)Composite spinning stoste inputs in the nozzle of spray gun;
(7)The composite spinning stoste is sprayed from nozzle using spray gun and enters wire drawing chamber, and is occurred using high temperature and pressure air
The composite spinning stoste drop is drawn into a diameter of 100nm Nanowire vinylon and cotton blends below by the high temperature and pressure air that device generates.
Embodiment 3
A kind of preparation process of High-performance graphene Nanowire vinylon and cotton blend, preparation process are as follows:
(1)Antioxidant is prepared, by β-(4- hydroxyl -3,5- di-tert-butyl-phenyls)The positive octadecyl ester of propionic acid, four (β-(3,5- bis- tertiary fourths
Base -4- hydroxy phenyls)Propionic acid) pentaerythritol ester, phosphorous acid(Three nonyl phenyl)Ester is with mass ratio 3:2:5 ratio mixing, system
Obtain antioxidant;
(2)Antiseptic is prepared, by dodecyl dimethyl benzyl ammonium bromide, myristyl benzyl dimethyl ammonium chloride, octadecane
Base dimethyl benzyl ammonium chloride, 2- n-octyl -4- isothiazoline -3- ketone are with mass ratio 3:4:1:7 ratio mixing, is made
Antiseptic;
(3)Prepare macromolecule spinning solution;By the polytetrahydrofuran ether glycol of the mass parts of the 4 of 14 mass parts, 4 '-MDI, 6,1 matter
The polyether triol of amount part, the polyoxypropylene diamine of 6 mass parts, the 1,4-butanediol of 2 mass parts, the antiseptic of 5 mass parts, 1
The antioxidant of mass parts reacts 0.7 hour at 93 DEG C;It is cooled to the sodium carboxymethylcellulose that 4 mass parts are added after room temperature, 7 matter
The polyvinylpyrrolidone for measuring part, stirs and can be obtained the macromolecule spinning solution after disperseing;
(4)Graphite powder is taken to be mixed at normal temperatures with Strong oxdiative mixed liquor, the grain size of the graphite powder is 44nm, Strong oxdiative mixed liquor
For the mixed liquor of concentrated nitric acid solution and concentrated sulfuric acid solution, the mass percent of sulfuric acid is 85% in concentrated sulfuric acid solution, concentrated nitric acid solution
In sulfuric acid mass percent position 75%, the mixed volume ratio of concentrated sulfuric acid solution and concentrated nitric acid solution is 5:7;Mixing quality ratio
For graphite powder:Strong oxdiative mixed liquor=1:3, incorporation time 25min, stir speed (S.S.) 88r/min stand 1H, obtain after mixing
To primary liquid;Hydrogen peroxide will be added in primary liquid and stir evenly, the volume ratio of primary liquid and hydrogen peroxide is 7:5, mixing time
For 45min, stir speed (S.S.) 110r/min, 2.5H is stood after the completion of stirring, obtains secondary liquid;High violent acid will be added in secondary liquid
The grain size of potassium powder, potassium permanganate powder is 88 mesh;The mass ratio of secondary liquid and potassium permanganate is 3:1, it is stirred
38min, temperature is maintained at 48 DEG C when mixing, and mixing rate is 135r/min, carries out first time ultrasonic wave after mixing
Concussion, concussion time are 35min, and ultrasonic frequency 46kHZ obtains three-level liquid;To be passed through chlorine in three-level liquid, three-level liquid with
The volume ratio of chlorine is 10:13, reaction time 65min stand 2H, second of ultrasonic wave shake are carried out after standing after the completion of reaction
It swings, the concussion time is 78min, ultrasonic frequency 65kHZ;Then centrifugal treating is carried out, is used in combination deionized water by lower sediment
It washes out, obtains graphene stoste;
(5)With the mixing 5 of graphene stoste and the macromolecule spinning solution:19 mass ratio adds graphene stoste
Enter in macromolecule spinning solution and mixed, forms composite spinning stoste after mixing;
(6)Composite spinning stoste inputs in the nozzle of spray gun;
(7)The composite spinning stoste is sprayed from nozzle using spray gun and enters wire drawing chamber, and is occurred using high temperature and pressure air
The composite spinning stoste drop is drawn into a diameter of 100nm Nanowire vinylon and cotton blends below by the high temperature and pressure air that device generates.
Beneficial effects of the present invention are:
Special macromolecule spinning solution formula and preparation process, by unique complex antimicrobials and composite antioxidant,
The performance of spinning solution can be greatly improved, the anti-microbial property and antioxygen of final products graphene nano fiber cotton are reinforced
Performance.
The graphene stoste of special preparation, using multiple oxidation reaction, graphene stoste made from the method for fractional steps is oxidation stone
Black alkene stoste can be good at use in nanofiber making, containing abundant oxygen functional group, such as carboxyl, hydroxyl, epoxy group
It is easy to use Deng, this kind of stoste in use, direct plungeing into macromolecule spinning solution when nanofiber production.And energy
Nanofiber intensity, thermal coefficient, electric conductivity are enough increased substantially, using effect is good.
Claims (9)
1. a kind of preparation process of High-performance graphene Nanowire vinylon and cotton blend, which is characterized in that preparation process is as follows:
Prepare macromolecule spinning solution;
Graphene stoste is added into macromolecule spinning solution and is mixed, forms composite spinning stoste after mixing;
Composite spinning stoste inputs in the nozzle of spray gun;
The composite spinning stoste is sprayed from nozzle using spray gun and enters wire drawing chamber, and is given birth to using HTHP air generator
At high temperature and pressure air the composite spinning stoste drop is drawn into a diameter of 100nm Nanowire vinylon and cotton blends below.
2. a kind of preparation process of High-performance graphene Nanowire vinylon and cotton blend as described in claim 1, which is characterized in that the stone
The mixing quality ratio of black alkene stoste and the macromolecule spinning solution is 3-6:17-25.
3. a kind of preparation process of High-performance graphene Nanowire vinylon and cotton blend as described in claim 1, which is characterized in that the stone
The preparation process of black alkene stoste is as follows:
(1)Graphite powder is taken to be mixed at normal temperatures with Strong oxdiative mixed liquor, mixing quality ratio is graphite powder:Strong oxdiative mixed liquor=
1:3,20~30min of incorporation time, stir speed (S.S.) 88r/min stand 1H after mixing, obtain primary liquid:
(2)Hydrogen peroxide will be added in primary liquid and stir evenly, the volume ratio of primary liquid and hydrogen peroxide is 7:5, mixing time is
30~60min, stir speed (S.S.) 110r/min stand 2~3H after the completion of stirring, obtain secondary liquid;
(3)Potassium permanganate powder will be added in secondary liquid, the mass ratio of secondary liquid and potassium permanganate is 3:1, it is stirred 25
~55min, temperature is maintained at 45~50 DEG C when mixing, and mixing rate is 135r/min, carries out after mixing for the first time
Ultrasonic oscillation, concussion time are 30~40min, and ultrasonic frequency is 40~60kHZ, obtains three-level liquid;
(4)Chlorine will be passed through in three-level liquid, the volume ratio of three-level liquid and chlorine is 10:13, the reaction time is 30~90min, instead
2H should be stood after the completion, second of ultrasonic oscillation is carried out after standing, and the concussion time is 60~90min, ultrasonic frequency 50
~77kHZ;Then centrifugal treating is carried out, deionized water is used in combination to wash out lower sediment, obtains graphene stoste.
4. a kind of preparation process of High-performance graphene Nanowire vinylon and cotton blend as claimed in claim 3, which is characterized in that the height
The grain size of violent acid potassium powder is the mesh of 100 mesh~80.
5. a kind of preparation process of High-performance graphene Nanowire vinylon and cotton blend as claimed in claim 3, which is characterized in that the stone
The grain size of ink powder is 10~100nm.
6. a kind of preparation process of High-performance graphene Nanowire vinylon and cotton blend as claimed in claim 3, which is characterized in that Strong oxdiative
Mixed liquor is the mixed liquor of concentrated nitric acid solution and concentrated sulfuric acid solution, and the mass percent of sulfuric acid is 85% in concentrated sulfuric acid solution, dense nitre
The mixed volume ratio of the mass percent position 75% of sulfuric acid in acid solution, concentrated sulfuric acid solution and concentrated nitric acid solution is 4~9:5~11.
7. a kind of preparation process of High-performance graphene Nanowire vinylon and cotton blend as described in claim 1, which is characterized in that the height
Molecule spinning solution is by the polytetrahydrofuran ether glycol of the mass parts of the 4 of 11~18 mass parts, 4 '-MDI, 5~7,1~2 mass parts
Polyether triol, the polyoxypropylene diamine of 5~7 mass parts, the 1,4-butanediol of 2~3 mass parts, the antibacterial of 4~7 mass parts
The antioxidant of agent, 1~1.5 mass parts reacts 0.5~1.0 hour at 89~97 DEG C;3~5 mass are added after being cooled to room temperature
The sodium carboxymethylcellulose of part, the polyvinylpyrrolidone of 6~8 mass parts stir and can be obtained the macromolecule after disperseing
Spinning solution.
8. a kind of preparation process of High-performance graphene Nanowire vinylon and cotton blend as claimed in claim 7, which is characterized in that described anti-
Microbial inoculum is by dodecyl dimethyl benzyl ammonium bromide, myristyl benzyl dimethyl ammonium chloride, octadecyl dimethyl benzyl chlorine
Change ammonium, 2- n-octyl -4- isothiazoline -3- ketone with mass ratio 3:4:1:7 ratio mixes.
9. a kind of preparation process of High-performance graphene Nanowire vinylon and cotton blend as claimed in claim 7, which is characterized in that described anti-
Oxygen agent is by β-(4- hydroxyl -3,5- di-tert-butyl-phenyls)The positive octadecyl ester of propionic acid, four (β-(3,5- di-tert-butyl-hydroxy phenyls)
Propionic acid) pentaerythritol ester, phosphorous acid(Three nonyl phenyl)Ester is with mass ratio 3-4:1-4:The ratio of 3-6 mixes.
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