CN107903592A - A kind of high temperature resistant polyethylene terephthalate composite material and preparation method thereof - Google Patents
A kind of high temperature resistant polyethylene terephthalate composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of high temperature resistant polyethylene terephthalate composite material and preparation method thereof, including following parts by weight raw material to be prepared:50 60 parts of polyethylene terephthalate, 8 12 parts of nano-aluminum hydroxide, 5 10 parts of modifying agent, 20 35 parts of polyimides, 0.3 0.8 parts of coupling agent, 25 parts of crosslinking agent, 5 10 parts of triethyl phosphite, 38 parts of zinc stearate;The present invention is for composite by the nano-aluminum hydroxide Jing Guo specific aim modification and polyethylene terephthalate, and nano-aluminum hydroxide is set to be dispersed in polyethylene terephthalate system, obtained polyethylene terephthalate composite material resistance to elevated temperatures is excellent, is conducive to application of the polyethylene terephthalate in more areas.
Description
Technical field
The present invention relates to modified material field, and in particular to a kind of high temperature resistant polyethylene terephthalate composite material and
Its preparation method.
Background technology
Polyethylene terephthalate be exchanged by dimethyl terephthalate (DMT) with glycol ester or with terephthalic acid (TPA) with
Ethylene glycol esterification first synthesizes bishydroxyethyl terephthalate, then carries out polycondensation reaction again and is made, and belongs to crystal type saturated polyester, is
Milky or light yellow, highly crystalline polymer.With excellent mechanical performance, rigidity is high, hardness is big, and water imbibition is small, ruler
Very little stability is good, good toughness, impact resistance, rub resistance, creep resistance, and chemical resistance is good.In industries such as automobile, aviation, electronics, machineries
In be used widely.
With the continuous improvement that people require material resistance to elevated temperatures, the poly terephthalic acid second without heat resist modification
Diester has been difficult to meet demand, thus, heat resist modification is carried out to polyethylene terephthalate and is necessitated.Now to poly- pair
The heat resist modification processing method species of polyethylene terephthalate is various, and modified effect is also fine, especially with nano material
Appearance and application, polyethylene terephthalate heat-resisting quantity increase significant effect, enable polyethylene terephthalate
Largely used in more areas, but there is also deficiency.Although nano material has, high temperature resistant enhancing effect is good, small excellent of additive amount
Point, but there is also difficulties in dispersion, it is of high cost the defects of.During heat resist modification is carried out, nano material disperses uneven meeting shadow
Its high-temperature resistant result is rung, obtained modified material heat-resisting quantity is relatively low, and the production and application to modified material adversely affect.
The content of the invention
The defects of it is an object of the invention to overcome existing polyethylene terephthalate composite material heat-resisting quantity poor,
A kind of high temperature resistant polyethylene terephthalate composite material and preparation method thereof is provided;The present invention will pass through at specific aim modification
The nano-aluminum hydroxide of reason and polyethylene terephthalate are for composite, and it is poly- to benzene to be dispersed in nano-aluminum hydroxide
In dioctyl phthalate second diester system, obtained polyethylene terephthalate composite material resistance to elevated temperatures is excellent, is conducive to poly- pair
Application of the polyethylene terephthalate in more areas.
In order to realize foregoing invention purpose, the present invention provides a kind of high temperature resistant polyethylene terephthalate composite wood
Material, including following parts by weight raw material are prepared:50-60 parts of polyethylene terephthalate, 8-12 parts of nanometer hydrogen-oxygen
Change aluminium, 5-10 parts of modifying agent, 20-35 parts of polyimides, 0.3-0.8 parts of coupling agent, 2-5 parts of crosslinking agent, 5-10 parts
Triethyl phosphite, 3-8 parts of zinc stearate.
A kind of above-mentioned high temperature resistant polyethylene terephthalate composite material, can increase according to nano-aluminum hydroxide and crosslinking
The basic principle of resin material heat-resisting quantity, not only by targetedly screening modifying agent, coupling agent and the species of crosslinking agent, comes
The compatibility between nano-aluminum hydroxide and polyethylene terephthalate is improved, and makes nano-aluminum hydroxide in poly- terephthaldehyde
Disperse in sour second diester evenly, make nano-aluminum hydroxide to the heat-resisting quantity humidification of polyethylene terephthalate more
It is good, modified polyethylene terephthalate composite material is also made by controlling the degree of polymerization of polyethylene terephthalate
Reach optimum balance relation between heat-resisting quantity and processability, so that the polyethylene terephthalate composite material made
Under conditions of with excellent heat-resisting quantity, it may have excellent processability, allows it to be applied in more areas.
A kind of above-mentioned high temperature resistant polyethylene terephthalate composite material, wherein, the nano-aluminum hydroxide particle diameter
For 10-80nm;Nano-aluminum hydroxide particle diameter is smaller, and dispersiveness is poorer, and nano-aluminum hydroxide particle diameter is bigger, to poly terephthalic acid
The high temperature resistant humidification of second diester is poorer;Preferably, the nano-aluminum hydroxide particle diameter is 30-50nm;Most preferably, institute
The nano-aluminum hydroxide particle diameter stated is 40nm.
A kind of above-mentioned high temperature resistant polyethylene terephthalate composite material, wherein, the modifying agent is the acid of glycerine three
The mixture of ester and dimethyl mercaptosuccinic acid esters composition;The modifying agent can improve nano-aluminum hydroxide with poly- to benzene two
The compatibility of formic acid second diester, and polar group can be formed on nano-aluminum hydroxide surface, beneficial to scattered;Preferably, it is described
The ratio between amount of material of triglyceride and dimethyl mercaptosuccinic acid esters is 1 ︰ 1 in modifying agent.
A kind of above-mentioned high temperature resistant polyethylene terephthalate composite material, wherein, the degree of polymerization of polyimides is bigger, then
The heat-resisting quantity of polyethylene terephthalate composite material is poorer after crosslinking, and processability is better, and the polymer of polyimides is got over
Small, then the heat-resisting quantity of polyethylene terephthalate composite material is better after being crosslinked, and processability is poorer, and therefore, selection is reasonable
The polyimides degree of polymerization, be the important means for balancing heat-resisting quantity and processability.The degree of polymerization of the polyimides is
120-180;Preferably, the degree of polymerization of the polyimides is 140-160;It is optimal, the degree of polymerization of the polyimides
For 150;By preferred, obtained polyethylene terephthalate composite material both has excellent heat-resisting quantity, it may have compared with
Good processability, is adapted to the application in more areas.
Wherein, the polyethylene terephthalate degree of polymerization is 800-1200;Preferably, the poly terephthalic acid
The degree of polymerization of second diester is 900-1100;Most preferably, the degree of polymerization of the polyethylene terephthalate is 1000;Pass through
It is preferred that obtained polyethylene terephthalate composite material both has excellent heat-resisting quantity, it may have preferable processability.
A kind of above-mentioned high temperature resistant polyethylene terephthalate composite material, wherein, the coupling agent is different for aluminic acid three
Propyl ester coupling agent;Three isopropyl ester of aluminic acid can increase between nano-aluminum hydroxide and polyethylene terephthalate and modifying agent
Compatibility, improves the performance of polyethylene terephthalate composite material.
Wherein, the crosslinking agent is aluminium isopropoxide, which can be by the polymer raw materials of two kinds of different polymerization degrees
Appropriate crosslinking, improves the heat-resisting quantity of polyethylene terephthalate composite material.
A kind of above-mentioned high temperature resistant polyethylene terephthalate composite material, wherein, its raw material further includes dispersant, increases
Mould one or more auxiliary agents in agent, antistatic additive, coloring agent, brightener;Above-mentioned auxiliary agent can improve poly terephthalic acid second
The processability of diester composite material, increases the effect such as its feature, so as to increase its applicability.
In order to realize foregoing invention purpose, further, present invention also offers a kind of high temperature resistant poly terephthalic acid second
The preparation method of diester composite material, comprises the following steps:
(1)Nano-aluminum hydroxide is handled with coupling agent;
(2)Nano-aluminum hydroxide Jing Guo coupling agent treatment is subjected to cladding processing with modifying agent;
(3)The place for composite in the electric field after mixing by the nano-aluminum hydroxide after cladding and polyethylene terephthalate
Reason, obtains mixture;
(4)By mixture and polyimides, crosslinking agent, zinc stearate, triethyl phosphite after mixing at place for composite
Reason, obtains high temperature resistant polyethylene terephthalate composite material.
A kind of preparation method of high temperature resistant polyethylene terephthalate composite material, first with coupling agent to nanometer hydroxide
Aluminium carries out coupling processing, increase nano-aluminum hydroxide and modifying agent, the compatibility of polyethylene terephthalate;Modifying agent is used again
Processing is modified to nano-aluminum hydroxide, and polar group is formed on its surface;Finally make a nanometer hydroxide using external electric field
Polar group polarization in aluminium surface and polyethylene terephthalate chain, it is powered, pass through repelling each other between electric charge or attracting original
Reason, also can be bonded with the polar group on polyethylene terephthalate chain while making nano-aluminum hydroxide dispersed, from
And the high temperature resistant enhancing effect of nano-aluminum hydroxide is farthest embodied, so as to get modification poly terephthalic acid second
Diester heat-resisting quantity significantly improves;The preparation method is simple and reliable, and it is compound to be suitable for high temperature resistant polyethylene terephthalate
Extensive, the industrialized production of material.
A kind of preparation method of above-mentioned high temperature resistant polyethylene terephthalate composite material, wherein, it is preferred that step 1
Carry out ultrasonic wave being used to aid in during coupling processing;Shaken by the high speed of ultrasonic wave, make nano-aluminum hydroxide dispersed
More preferably, and to coupling processing there is facilitation.
A kind of preparation method of above-mentioned high temperature resistant polyethylene terephthalate composite material, wherein, described in step 3
Electric field energy produces polarization to group, makes group powered, so as to promote the scattered and bonded effect of nano-aluminum hydroxide, carries
The heat-resisting quantity of the modified polyethylene terephthalate of height.
Preferably, the electric field strength is 1.5-2.5kv/m;Electric field strength is too small, and polarization effect is weak, to nanometer hydrogen-oxygen
The dispersion effect for changing aluminium is poor;Electric field strength is excessive, and polarization effect is too strong, and intermolecular force is too big, and strand produces orientation and moves
It is dynamic, arrangement and the bonded performance for having an impact, may be decreased polyethylene terephthalate composite material to strand;It is optimal
Choosing, the electric field strength is 1.8-2.0kv/m.
Wherein, it is preferred that the electric field is the constant parallel electric field of direction of an electric field;The constant parallel electric field of direction of an electric field
Best to the polarization effect of polar group, group intermolecular forces are stablized, and the scattered and bonded promotion to nano-aluminum hydroxide is made
Use best results.
Compared with prior art, beneficial effects of the present invention:
1st, polyethylene terephthalate composite material of the present invention targetedly screens the kind of modifying agent, coupling agent and crosslinking agent
Class, makes the compatibility between nano-aluminum hydroxide and polyethylene terephthalate more preferable, in polyethylene terephthalate
Dispersiveness it is more preferable, nano-aluminum hydroxide is more preferable to the heat-resisting quantity humidification of polyethylene terephthalate.
2nd, polyethylene terephthalate composite material of the present invention is sub- by controlling polyethylene terephthalate and polyamides
The degree of polymerization of amine makes the modified polyethylene terephthalate composite material reach most between heat-resisting quantity and processability
Good equilibrium relation, so as to get polyethylene terephthalate composite material under conditions of with excellent heat-resisting quantity,
With excellent processability.
3rd, the preparation method of polyethylene terephthalate composite material of the present invention, utilizes the polarization of external electric field, energy
Promote nano-aluminum hydroxide scattered and bonded in polyethylene terephthalate system, the high temperature resistant of nano-aluminum hydroxide increases
Potent fruit is more preferable, the heat-resisting quantity higher of obtained polyethylene terephthalate composite material.
4th, the preparation method of polyethylene terephthalate composite material of the present invention is simple, reliable, and suitable high temperature resistant is gathered pair
Extensive, the industrialized production of polyethylene terephthalate composite material.
Embodiment
With reference to test example and embodiment, the present invention is described in further detail.But this should not be understood
Following embodiment is only limitted to for the scope of the above-mentioned theme of the present invention, it is all that this is belonged to based on the technology that present invention is realized
The scope of invention.
Embodiment 1
(1)10 parts of nano-aluminum hydroxide is handled with 0.6 part of three isopropyl ester of aluminic acid;
(2)By the nano-aluminum hydroxide Jing Guo coupling agent treatment 3.5 parts of triglyceride and 3.5 parts of dimethyl sulfydryl amber
Amber acid esters carries out cladding processing;
(3)Nano-aluminum hydroxide after cladding is uniformly mixed with the polyethylene terephthalate that 55 parts of the degree of polymerization is 1000
Extruded afterwards in the constant parallel electric field of the direction of an electric field that electric field strength is 2.0kv/m, obtain mixture;
(4)The polyimides, 4 parts of aluminium isopropoxides, 8 parts of phosphorous that the mixture that step 3 is obtained and 28 parts of the degree of polymerization are 150
Triethylenetetraminehexaacetic acid ester, 5 parts of zinc stearate are extruded after mixing, obtain high temperature resistant polyethylene terephthalate composite wood
Material.
Embodiment 2
(1)8 parts of nano-aluminum hydroxide is handled with 0.3 part of three isopropyl ester of aluminic acid;
(2)By the nano-aluminum hydroxide Jing Guo coupling agent treatment 2.5 parts of triglyceride and 2.5 parts of dimethyl sulfydryl amber
Amber acid esters carries out cladding processing;
(3)Nano-aluminum hydroxide after cladding is uniformly mixed with the polyethylene terephthalate that 50 parts of the degree of polymerization is 1200
Extruded afterwards in the electric field for being 2.5kv/m in electric field strength, obtain mixture;
(4)The polyimides, 2 parts of aluminium isopropoxides, 5 parts of phosphorous that the mixture that step 3 is obtained and 20 parts of the degree of polymerization are 120
Triethylenetetraminehexaacetic acid ester, 3 parts of zinc stearate are extruded after mixing, obtain high temperature resistant polyethylene terephthalate composite wood
Material.
Embodiment 3
(1)12 parts of nano-aluminum hydroxide is handled with 0.8 part of three isopropyl ester of aluminic acid;
(2)By the nano-aluminum hydroxide Jing Guo coupling agent treatment 5 parts of triglyceride and 4 parts of dimethyl mercapto succinic acid
Ester carries out cladding processing;
(3)Nano-aluminum hydroxide after cladding is uniformly mixed with the polyethylene terephthalate that 60 parts of the degree of polymerization is 800
Extruded afterwards in the constant parallel electric field of the direction of an electric field that electric field strength is 1.5kv/m, obtain mixture;
(4)The polyimides, 5 parts of aluminium isopropoxides, 10 parts of Asia that the mixture that step 3 is obtained and 35 parts of the degree of polymerization are 180
Triethyl phosphate, 8 parts of zinc stearate are extruded after mixing, obtain high temperature resistant polyethylene terephthalate composite wood
Material.
Comparative example 1
(1)10 parts of nano-aluminum hydroxide is handled with 0.6 part of three isopropyl ester of aluminic acid;
(2)By the nano-aluminum hydroxide Jing Guo coupling agent treatment and 7 parts of dispersant, 55 parts of the degree of polymerization be 1000 it is poly- to benzene
Dioctyl phthalate second diester is extruded in the constant parallel electric field of the direction of an electric field that electric field strength is 1.2kv/m after mixing,
Obtain mixture;
(3)The polyimides, 4 parts of aluminium isopropoxides, 8 parts of phosphorous that the mixture that step 2 is obtained and 28 parts of the degree of polymerization are 150
Triethylenetetraminehexaacetic acid ester, 5 parts of zinc stearate are extruded after mixing, obtain polyethylene terephthalate composite material.
Comparative example 2
(1)10 parts of nano-aluminum hydroxide is handled with 0.6 part of three isopropyl ester of aluminic acid;
(2)By the nano-aluminum hydroxide Jing Guo coupling agent treatment 3.5 parts of triglyceride and 3.5 parts of dimethyl sulfydryl amber
Amber acid esters carries out cladding processing;
(3)By polyethylene terephthalate that the nano-aluminum hydroxide after cladding and 55 parts of the degree of polymerization are 1000,28 parts
The degree of polymerization is uniformly mixed laggard for 150 polyimides, 4 parts of aluminium isopropoxides, 8 parts of triethyl phosphite, 5 parts of zinc stearate
Row extrusion, obtains polyethylene terephthalate composite material.
Comparative example 3
(1)10 parts of nano-aluminum hydroxide is handled with 0.6 part of three isopropyl ester of aluminic acid;
(2)By the nano-aluminum hydroxide Jing Guo coupling agent treatment 3.5 parts of polystyrene and 3.5 parts of dimethyl mercaptosuccinic
Acid esters carries out cladding processing;
(3)Nano-aluminum hydroxide after cladding is uniformly mixed with the polyethylene terephthalate that 55 parts of the degree of polymerization is 1000
Extruded afterwards in the constant parallel electric field of the direction of an electric field that electric field strength is 2.0kv/m, obtain mixture;
(4)The polyimides, 4 parts of aluminium isopropoxides, 8 parts of phosphorous that the mixture that step 3 is obtained and 28 parts of the degree of polymerization are 150
Triethylenetetraminehexaacetic acid ester, 5 parts of zinc stearate are extruded after mixing, obtain polyethylene terephthalate composite material.
Comparative example 4
(1)10 parts of nano-aluminum hydroxide is handled with 0.6 part of three isopropyl ester of aluminic acid;
(2)By the nano-aluminum hydroxide Jing Guo coupling agent treatment 3.5 parts of triglyceride and 3.5 parts of dimethyl sulfydryl amber
Amber acid esters carries out cladding processing;
(3)By polyimides that the nano-aluminum hydroxide after cladding and 28 parts of the degree of polymerization are 150,4 parts of aluminium isopropoxides, 8 parts
Triethyl phosphite, 5 parts of zinc stearate, the polyethylene terephthalate that 55 parts of the degree of polymerization is 1000 exist after mixing
Electric field strength is to be extruded in the constant parallel electric field of the direction of an electric field of 2.0kv/m, obtains polyethylene terephthalate and answers
Condensation material.
Comparative example 5
(1)10 parts of nano-aluminum hydroxide is handled with 0.6 part of three isopropyl ester of aluminic acid;
(2)By the nano-aluminum hydroxide Jing Guo coupling agent treatment 3.5 parts of triglyceride and 3.5 parts of dimethyl sulfydryl amber
Amber acid esters carries out cladding processing;
(3)Nano-aluminum hydroxide after cladding is uniformly mixed with the polyethylene terephthalate that 55 parts of the degree of polymerization is 700
Extruded afterwards in the constant parallel electric field of the direction of an electric field that electric field strength is 2.0kv/m, obtain mixture;
(4)Polyimides that the mixture that step 3 is obtained and 28 parts of the degree of polymerization are 100,4 parts of triethyl phosphite, 5 parts
Zinc stearate, 8 parts of aluminium isopropoxides extruded after mixing, obtain polyethylene terephthalate composite material.
By the polyethylene terephthalate composite material in above-described embodiment 1-3 and comparative example 1-5, performance inspection is carried out
Survey, record data are as follows:
Performance | Heat distortion temperature(℃) | Processability |
Embodiment 1 | 122 | ++++ |
Embodiment 2 | 121 | ++++ |
Embodiment 3 | 122 | ++++ |
Comparative example 1 | 108 | ++++ |
Comparative example 2 | 109 | ++++ |
Comparative example 3 | 112 | ++++ |
Comparative example 4 | 115 | ++++ |
Comparative example 5 | 123 | ++ |
Polyethylene terephthalate | 98 | +++ |
Note:"+" is more, illustrates that performance is better.
Above-mentioned analysis of experimental data is understood, the high temperature resistant poly terephthalic acid of the present invention being prepared in embodiment 1-3
Second diester composite material, nano-aluminum hydroxide are uniformly dispersed, good with the compatibility of polyethylene terephthalate, poly- terephthaldehyde
Sour second diester composite material heat-resisting quantity is good, and processability is good;And in comparative example 1, be not used modifying agent to nano-aluminum hydroxide into
Row modification, although adding dispersant, nano-aluminum hydroxide dispersion effect is poor, the phase with polyethylene terephthalate
Capacitive is poor, and the heat-resisting quantity of polyethylene terephthalate composite material significantly reduces;Do not answered in the electric field in comparative example 2
Conjunction is handled, and nano-aluminum hydroxide dispersion effect is poor, and the heat-resisting quantity of polyethylene terephthalate composite material significantly reduces;It is right
Modifying agent is not the application defined in ratio 3, and nano-aluminum hydroxide dispersion effect is poor, and polyethylene terephthalate is compound
The heat-resisting quantity of material significantly reduces;Cross-linking reaction equally carries out in the electric field in comparative example 4, and electric field produces not cross-linking reaction
Profit influence, so as to get polyethylene terephthalate composite material heat-resisting quantity reduce;What is used in comparative example 5 is poly- to benzene
Dioctyl phthalate second diester and the polyimides degree of polymerization are too small, although heat-resisting quantity increased after compound, its processability significantly drops
It is low, it is unfavorable for the application of polyethylene terephthalate composite material.
Claims (10)
1. a kind of high temperature resistant polyethylene terephthalate composite material, it is characterised in that including following parts by weight raw material system
It is standby to obtain:50-60 parts of polyethylene terephthalate, 8-12 parts of nano-aluminum hydroxide, 5-10 parts of modifying agent, 20-35
The polyimides, 0.3-0.8 parts of coupling agent, 2-5 parts of crosslinking agent, 5-10 parts of triethyl phosphite, 3-8 parts of tristearin of part
Sour zinc;The mixture that the modifying agent forms for triglyceride with dimethyl mercaptosuccinic acid esters;The coupling agent is aluminic acid
Three isopropyl ester coupling agents, the crosslinking agent are aluminium isopropoxide;The degree of polymerization of the polyimides is 120-180;It is described poly- to benzene
The dioctyl phthalate second diester degree of polymerization is 800-1200.
2. composite material according to claim 1, it is characterised in that triglyceride and dimethyl mercapto in the modifying agent
The ratio between amount of material of base succinate is 1 ︰ 1.
3. composite material according to claim 1, it is characterised in that the degree of polymerization of the polyimides is 140-160.
4. composite material according to claim 3, it is characterised in that the degree of polymerization of the polyimides is 150.
5. composite material according to claim 1, it is characterised in that the polyethylene terephthalate degree of polymerization is
900-1100。
6. composite material according to claim 5, it is characterised in that the polyethylene terephthalate degree of polymerization is
1000。
7. a kind of preparation method of the composite material as described in claim any one of 1-6, it is characterised in that comprise the following steps:
(1)Nano-aluminum hydroxide is handled with coupling agent;
(2)Nano-aluminum hydroxide Jing Guo coupling agent treatment is subjected to cladding processing with modifying agent;
(3)The place for composite in the electric field after mixing by the nano-aluminum hydroxide after cladding and polyethylene terephthalate
Reason, obtains mixture;(4)Mixture and polyimides, crosslinking agent, zinc stearate, triethyl phosphite are existed after mixing
Processing for composite, obtains high temperature resistant polyethylene terephthalate composite material.
8. preparation method according to claim 7, it is characterised in that step(3)Middle electric field strength is 1.5-2.5kv/m.
9. preparation method according to claim 8, it is characterised in that step(3)Middle electric field strength is 1.8-2.0kv/m.
10. preparation method according to claim 7, it is characterised in that step(3)Middle electric field is put down for direction of an electric field is constant
Row electric field.
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CN111073234A (en) * | 2019-12-30 | 2020-04-28 | 浙江新力新材料股份有限公司 | Heat-resistant flame-retardant PET composite material, preparation method thereof and application thereof in preparation of patch board |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111073234A (en) * | 2019-12-30 | 2020-04-28 | 浙江新力新材料股份有限公司 | Heat-resistant flame-retardant PET composite material, preparation method thereof and application thereof in preparation of patch board |
CN111073234B (en) * | 2019-12-30 | 2022-04-08 | 浙江新力新材料股份有限公司 | Heat-resistant flame-retardant PET composite material, preparation method thereof and application thereof in preparation of patch board |
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