CN103613931B - A kind of antistatic silicone gel for heat-conducting pad and preparation method thereof - Google Patents

A kind of antistatic silicone gel for heat-conducting pad and preparation method thereof Download PDF

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CN103613931B
CN103613931B CN201310497048.3A CN201310497048A CN103613931B CN 103613931 B CN103613931 B CN 103613931B CN 201310497048 A CN201310497048 A CN 201310497048A CN 103613931 B CN103613931 B CN 103613931B
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vinyl
viscosity
resin
preparation
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CN103613931A (en
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陈维
张丽娅
王建斌
陈田安
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Yantai Darbond Technology Co Ltd
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YANTAI DEBANG ADVANCED SILICON MATERIALS CO Ltd
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Abstract

The present invention relates to a kind of antistatic silicone gel for heat-conducting pad and preparation method thereof, be that the component A of 1:1 and B component form by weight proportion, described component A is made up of the raw material of following weight part: base-material 95 ~ 99.84 parts, catalyzer 0.1 ~ 1 part, caking agent 0.05 ~ 2 part, 0.01 ~ 2 part, static inhibitor; Described B component is made up of the raw material of following weight part: base-material 84 ~ 94.9 parts, linking agent 5 ~ 15 parts, 0.1 ~ 1 part, inhibitor; Silicon gel good fluidity prepared by the present invention, has excellent cementability, holds viscosity and static resistance after sulfuration.

Description

A kind of antistatic silicone gel for heat-conducting pad and preparation method thereof
Technical field
The present invention relates to a kind of antistatic silicone gel for heat-conducting pad and preparation method thereof, belong to organic silicon electronic field of material technology.
Background technology
Heat-conducting pad is mainly used to fill the clearance between heater members and radiator element or metab, cover very irregular surface, make heat be transmitted to metal shell or diffuser plate from discrete device or whole PCB, improve the efficiency of heating electronic package and extend its work-ing life.
At present, the material be applied on heat-conducting pad is by selecting suitable resin, and then add certain heat conductive filler, fire retardant, pigment, softening agent and scorch retarder etc. get a desired effect.The resin of usual selection has epoxy resin, one or more in acrylic resin and silicone resin; The temperature tolerance of epoxy resin is poor, easily ftractures, shock proof weak effect; Acrylic resin cost is high, and condition of cure is harsh, and technique is loaded down with trivial details; Silicone resin class generally adopts silicon gel.Silica hydrogel is applied on heat-conducting pad, can fit well with contact surface, gives full play to its good elasticity and restorative, adapts to pressure change and temperature fluctuation.There are some defects in the domestic silicon gel that can be applied in this field, cementability is inadequate, and it is not good to hold viscosity, and antistatic effect is poor.Low cementability can have a strong impact on the combination between colloid and base material in using for a long time, causes polluting and destroying.Polymkeric substance due to resistance own very large, surface easily savings electrostatic and causing danger, and antistatic compounds can make electrostatic leak in time.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of antistatic silicone gel for heat-conducting pad and preparation method thereof, silicon gel prepared by the present invention is that the control of a kind of surface viscosity is proper, and good to substrate adherence, lasting adhesion property is desirable, cementability is strong, antistatic.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of antistatic silicone gel for heat-conducting pad, is that the component A of 1:1 and B component form, wherein by weight proportion
Described component A is made up of the raw material of following weight part: base-material 95 ~ 99.84 parts, catalyzer 0.1 ~ 1 part, caking agent 0.05 ~ 2 part, 0.01 ~ 2 part, static inhibitor;
Described B component is made up of the raw material of following weight part: base-material 84 ~ 94.9 parts, linking agent 5 ~ 15 parts, 0.1 ~ 1 part, inhibitor;
Wherein, described in A and B, base-material is the mixture of the organopolysiloxane containing vinyl and the silicone resin containing vinyl.
On the basis of technique scheme, the present invention can also do following improvement.
Further, the described organopolysiloxane containing vinyl is that vinyl bonds is combined in polysiloxane molecule chain end, molecular chain side chain or is bonded in molecule chain end and side chain.Vinyl polysiloxane is the organopolysiloxane or its mixture that at least contain two vinyl.
Further, the above-mentioned organopolysiloxane containing vinyl is the raw material of low volatile content, at fugitive constituent 150 DEG C 2 hours, and mass loss is less than 0.03%, and viscosity is 100 ~ 10000 centipoises, and the content of vinyl is 0.1 ~ 10wt%, specifically sees structural formula (1);
R 1for-Vi, work as R 2during for-Me, wherein n 1>=10, n 2>=10.
R 1, R 2for-Vi, wherein n 1>=10, n 2>=10.
The beneficial effect of above-mentioned further scheme is adopted to be: by the adjustment to matrix material viscosity, consumption, to realize the control to viscosity and intensity.
Further, the resin containing vinyl is vinyl MQ resin or the MDT resin containing vinyl.
Further, vinyl MQ resin is the raw material of low volatile content, and at fugitive constituent 150 DEG C, mass loss in 2 hours is less than 0.5%, and viscosity is 500 ~ 10000 centipoises, and the content of vinyl is 0.01 ~ 5wt%, and molecular formula is as follows:
(Me 3siO 0.5) a(ViMe 2siO 0.5) b(SiO 2) molecular formula 1
Wherein, a=0 ~ 1.5, b=0 ~ 1.5
Further, the MDT resin of vinyl is the raw material of low volatile content, and at volatile matter 150 DEG C, mass loss in 2 hours is less than 0.5%, and viscosity is 500 ~ 10000 centipoises, and the content of vinyl is 0.01 ~ 5wt%, and molecular formula is as follows:
(Me 3siO 0.5) a(ViMe 2siO 0.5) b(Me 2siO) (MeSiO 1.5) molecular formula 2
Wherein, a=0 ~ 1.5, b=0 ~ 1.5
The beneficial effect of above-mentioned further scheme is adopted to be: the MQ resin containing vinyl and the MDT resin containing vinyl are a kind of well organosilicon supporting materials, the functions such as it also has thickening, toughness reinforcing, wear-resisting, weather-proof.
Further, described linking agent is the hydrogen containing siloxane of hydrogen content 0.01 ~ 2wt%, viscosity is 10 ~ 100 centipoises, described linking agent is the organic hydrogen polysiloxanes being bonded to the hydrogen atom in hydrogen containing siloxane molecule on Siliciumatom containing two or more, specifically comprise, the organic hydrogen polysiloxanes that Si-H is bonded in the organic hydrogen polysiloxanes of hydrogen containing siloxane molecule chain end, Si-H is bonded in hydrogen containing siloxane molecular chain side chain, Si-H are bonded in one or more the mixture in the organic hydrogen polysiloxanes of hydrogen containing siloxane molecule chain end and side chain.Described hydrogen containing siloxane is the raw material of refining rank; Specifically see structural formula (2)
K 1, K 2for-Me or-H, wherein has one at least for-H, n 1>=0, n 2>=10.
Adopt the beneficial effect of above-mentioned further scheme to be: the molecular structure of organic hydrogen polysiloxanes can provide the active hydrogen of certain mass mark, contribute to the hardness regulating Silica hydrogel, modulus and vulcanization rate etc.The organic hydrogen polysiloxanes of active hydrogen end-blocking is a kind of chainextender, regulates its consumption can adjust the intensity of Silica hydrogel, toughness and viscosity, changes the mechanical property of Silica hydrogel.
Further, described catalyzer is platinum vinyl siloxane complex, and consumption is account for component A gross weight 0.1 ~ 1.0%, and platinum content is 1000 ~ 10000ppm, be preferably platinum (0)-2,4,6,8-tetramethyl--2,4,6,8-tetravinyl cyclotetrasiloxane complex solution;
Further, described caking agent is one or more the mixture in the organopolysiloxane of following structure, concrete as shown in structural formula (3), (4), (5), (6):
Wherein, n >=5,
Wherein, n >=5,
Wherein, n >=5,
Wherein, n >=5.
Adopt the beneficial effect of above-mentioned further scheme to be: to adopt caking agent can improve the surface viscosity of Silica hydrogel, increase the bonding force with base material, reduce internal stress.
Further, described inhibitor is alkynes alcohols material; Inhibitor consumption is account for B component gross weight 0.1 ~ 1.0%.
Further, described alkynes alcohols material is the one in 3-methyl isophthalic acid-butine-3-alcohol, 1-ethynylcyclohexanol, 3-propyl group-ethyl acetylene-3-alcohol, 3-octyl group-ethyl acetylene-3-alcohol, is preferably 1-ethynylcyclohexanol;
Adopt the beneficial effect of above-mentioned further scheme to be extend working hour of Silica hydrogel adding of inhibitor, and the package stability of Silica hydrogel is improved;
Further, described static inhibitor is one or more the mixture in the organopolysiloxane of following structure, concrete as shown in structural formula (7) and (8):
Wherein, n >=10,
Wherein, n >=10.
Adopt the beneficial effect of above-mentioned further scheme to be that static inhibitor can reduce surface resistivity and electric charge enrichment, improve its antistatic property, avoid the disaster that presence of fire etc. is unnecessary.
The invention has the beneficial effects as follows:
1) after sulfuration to the adhesivity of base material and hold tack splendid, good sealing effect;
2) static resistance after sulfuration is strong;
The invention provides a kind of preparation method of the above-mentioned antistatic silicone gel for heat-conducting pad, comprising:
The preparation of component A: under 25 DEG C of conditions, by the base-material of 95 ~ 99.84 weight parts, the catalyzer of 0.1 ~ 1 weight part and the caking agent of 0.05 ~ 2 weight part, the static inhibitor of 0.01 ~ 2 weight part, joins successively in stirrer, mixes, and obtains described component A;
The preparation of B component: under 25 DEG C of conditions, by the base-material of 84 ~ 94.9 weight parts, the linking agent of 5 ~ 15 weight parts, the inhibitor of 0.1 ~ 1 weight part, joins successively in stirrer, mixes, and obtains described B component;
Under 25 DEG C of conditions, component A and B component are mixed by the weight proportion of 1:1, in the middle of the mixing raw material system sizing material of mixing being placed in heat-conducting pad, deaeration 10 ~ 40 minutes under 0.05 ~-0.1MPa vacuum, 100 ~ 150 DEG C of heating solidification in 0.4 ~ 2 hour.
On the basis of technique scheme, the present invention can also do following improvement.
Further, described vacuum condition is 0.09MPa;
Further, described inclined heated plate is 20 minutes, specifically determines according to the inclined heated plate of heat-conducting pad material system;
Further, described in the condition that is heating and curing be 125 DEG C, 30 minutes, concrete set time adjusted according to the actual condition of cure of heat-conducting pad;
The beneficial effect of the preparation method of silicon gel of the present invention is:
The preparation method of silicon gel of the present invention is simple to operate, process stabilizing, and operable time is long, and cementability is good, and be heating and curing fast, antistatic effect is good, excellent storage stability.
Embodiment
Be described principle of the present invention and feature below, example, only for explaining the present invention, is not intended to limit scope of the present invention.
In this manual, viscosity number refers to and adopt TA rheometer, the numerical value recorded under the condition of rotating speed 60/S at 25 DEG C.The resin of A and B component and silicone oil are the raw material of refining rank.
Embodiment 1
The preparation of component A: take viscosity be 10000 centipoises as structural formula (1), wherein R 1for-Vi, R 2for both-end vinyl polysiloxane (contents of ethylene 0.1wt%) 46.95g of-Me, viscosity be 100 centipoises as structural formula (1), wherein R 1, R 2for end, side vinyl polysiloxane (contents of ethylene 10wt%) 15.0g of-Vi, vinyl MQ resin such as molecular formula 1(viscosity is 500 centipoises, contents of ethylene 5wt%) 35g, add caking agent as structural formula (3), n=5,0.05g, add static inhibitor, as structural formula (7), n=10,2.0g, catalyst platinum (0)-2,4,6,8-tetramethyl--2,4,6,8-tetravinyl cyclotetrasiloxane complex solution 1.0g, platinum content 1000ppm, adds in stirrer successively, mixing and stirring, obtains described component A;
The preparation of B component: take viscosity be 500 centipoises as structural formula (1), wherein R 1for-Vi, R 2for both-end vinyl polysiloxane (contents of ethylene 0.5wt%) 79.9g of-Me, vinyl MQ resin such as molecular formula 1(viscosity is 10000 centipoises, contents of ethylene=0.01wt%) 15.0g, hydrogen containing siloxane as structural formula (2), K 1for-Me and K 2for-H, viscosity is 10 centipoises, and hydrogen richness is 2.0wt%, 5.0g, 1-ethynylcyclohexanol 0.1g, adds successively in stirrer, mixing and stirring, obtains described B component;
During use, component A, B component are mixed by weight for the proportioning of 1:1, in the middle of the mixing raw material being placed in heat-conducting pad, vacuum 0.05MPa, deaeration 40 minutes, and in 125 DEG C of heating 0.5 hour.
Embodiment 2
The preparation of component A: take viscosity be 2000 centipoises as structural formula (1), wherein R 1for-Vi, R 2for both-end vinyl polysiloxane (contents of ethylene 0.2wt%) 77.89g of-Me, vinyl MDT resin such as molecular formula 2(viscosity is 500 centipoises, contents of ethylene 5wt%) 20.0g, add caking agent as structural formula (4), n=10,2.0g, add static inhibitor, as structural formula (8), n=20,0.01g, catalyst platinum (0)-2,4,6,8-tetramethyl--2,4,6,8-tetravinyl cyclotetrasiloxane complex solution 0.1g, platinum content 10000ppm, adds in stirrer successively, mixing and stirring, obtains described component A;
The preparation of B component: take viscosity be 500 centipoises as structural formula (1), wherein R 1for-Vi, R 2for both-end vinyl polysiloxane (contents of ethylene 0.5wt%) 64.0g of-Me, vinyl MDT resin such as molecular formula 2(viscosity is 10000 centipoises, contents of ethylene 0.01wt%) 20.0g, hydrogen containing siloxane as structural formula (2), K 1and K 2for-H, hydrogen content is 1.0wt%, and viscosity is 100 centipoises, and 15.0g, 3-methyl isophthalic acid-butine-3-alcohol 1.0g, adds successively in stirrer, mixing and stirring, obtain described B component;
During use, component A, B component are mixed by weight for the proportioning of 1:1, in the middle of the mixing raw material being placed in heat-conducting pad, vacuum-0.1MPa, deaeration deaeration 10 minutes, and in 125 DEG C of heating 0.5 hour.
Embodiment 3
The preparation of component A: take viscosity be 1000 centipoises as structural formula (1), wherein R 1for-Vi, R 2for both-end vinyl polysiloxane (contents of ethylene 0.3wt%) 62.2g of-Me, viscosity be 2000 centipoises as structural formula (1), wherein R 1, R 2for end, side vinyl polysiloxane (contents of ethylene 8wt%) 15.0g of-Vi, vinyl MDT resin such as molecular formula 2(viscosity is 5000 centipoises, contents of ethylene 3.6wt%) 20.0g, add caking agent as structural formula (5), n=15,1.0g, add static inhibitor, as structural formula (7), n=20,1.2g, catalyst platinum (0)-2,4,6,8-tetramethyl--2,4,6,8-tetravinyl cyclotetrasiloxane complex solution 0.6g, platinum content 5000ppm, adds in stirrer successively, mixing and stirring, obtains described component A;
The preparation of B component: take viscosity be 500 centipoises as structural formula (1), wherein R 1for-Vi, R 2for both-end vinyl polysiloxane (contents of ethylene 0.5wt%) 64.5g of-Me, vinyl MQ resin such as molecular formula 1(viscosity is 5000 centipoises, contents of ethylene 3.6wt%) 25.0g, hydrogen containing siloxane as structural formula (2), K 1for-H, K 2for-Me, viscosity is 30 centipoises, and hydrogen content is 0.01wt%, 4.0g, hydrogen containing siloxane as structural formula (2), K 1for-Me and K 2for-H, viscosity is 10 centipoises, and hydrogen content is, 2.0wt%, 6.0g, 3-propyl group-ethyl acetylene-3-alcohol 0.5g, adds successively in stirrer, mixing and stirring, obtain described B component;
During use, component A, B component are mixed by weight for the proportioning of 1:1, in the middle of the mixing raw material being placed in heat-conducting pad, vacuum 0.09MPa, deaeration 20 minutes, and in 125 DEG C of heating 0.5 hour.
Comparative example 1
The preparation of component A: take viscosity be 10000 centipoises as structural formula (1), wherein R 1for-Vi, R 2for both-end vinyl polysiloxane (contents of ethylene 0.1wt%) 47.0g of-Me, viscosity be 100 centipoises as structural formula (1), wherein R 1, R 2for end, side vinyl polysiloxane (contents of ethylene 10wt%) 15.0g of-Vi, vinyl MQ resin such as molecular formula 1(viscosity is 500 centipoises, contents of ethylene 5wt%) 35g, add static inhibitor, as structural formula (7), n=10,2.0g, catalyst platinum (0)-2,4,6,8-tetramethyl--2,4,6,8-tetravinyl cyclotetrasiloxane complex solution 1.0g, platinum content 1000ppm, add successively in stirrer, mixing and stirring, obtain described component A;
The preparation of B component: take viscosity be 500 centipoises as structural formula (1), wherein R 1for-Vi, R 2for both-end vinyl polysiloxane (contents of ethylene 0.5wt%) 79.9g of-Me, vinyl MQ resin such as molecular formula 1(viscosity is 10000 centipoises, contents of ethylene=0.01wt%) 15.0g, hydrogen containing siloxane as structural formula (2), K 1for-Me and K 2for-H, viscosity is 10 centipoises, and hydrogen richness is 2.0wt%, 5.0g, 1-ethynylcyclohexanol 0.1g, adds successively in stirrer, mixing and stirring, obtains described B component;
During use, component A, B component are mixed by weight for the proportioning of 1:1, in the middle of the mixing raw material being placed in heat-conducting pad, vacuum 0.05MPa, deaeration 40 minutes, and in 125 DEG C of heating 0.5 hour.
Comparative example 2
The preparation of component A: take viscosity be 2000 centipoises as structural formula (1), wherein R 1for-Vi, R 2for both-end vinyl polysiloxane (contents of ethylene 0.2wt%) 77.9g of-Me, vinyl MDT resin such as molecular formula 2(viscosity is 500 centipoises, contents of ethylene 5wt%) 20.0g, add caking agent as structural formula (4), n=10,2.0g, catalyst platinum (0)-2,4,6,8-tetramethyl--2,4,6,8-tetravinyl cyclotetrasiloxane complex solution 0.1g, platinum content 10000ppm, adds in stirrer successively, mixing and stirring, obtains described component A;
The preparation of B component: take viscosity be 500 centipoises as structural formula (1), wherein R 1for-Vi, R 2for both-end vinyl polysiloxane (contents of ethylene 0.5wt%) 64.0g of-Me, vinyl MDT resin such as molecular formula 2(viscosity is 10000 centipoises, contents of ethylene 0.01wt%) 20.0g, hydrogen containing siloxane as structural formula (2), K 1and K 2for-H, hydrogen content is 1.0wt%, and viscosity is 100 centipoises, and 15.0g, 3-methyl isophthalic acid-butine-3-alcohol 1.0g, adds successively in stirrer, mixing and stirring, obtain described B component;
During use, component A, B component are mixed by weight for the proportioning of 1:1, in the middle of the mixing raw material being placed in heat-conducting pad, vacuum-0.1MPa, deaeration deaeration 10 minutes, and in 125 DEG C of heating 0.5 hour.
The present invention is by A obtained in each embodiment, and B component, 1:1 mixes in mass ratio, solidification value 125 DEG C, and 30 minutes time, the standard of each test event is carried out as follows, as shown in table 1.
Table 1 performance index
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (7)

1. for an antistatic silicone gel for heat-conducting pad, it is characterized in that, is that the component A of 1:1 and B component form by weight proportion,
Described component A is made up of the raw material of following weight part: base-material 95 ~ 99.84 parts, catalyzer 0.1 ~ 1 part, caking agent 0.05 ~ 2 part, 0.01 ~ 2 part, static inhibitor;
Described catalyzer is platinum vinyl siloxane complex;
Described caking agent is one or more the mixture in the organopolysiloxane of following structure, and concrete structure formula is as follows:
Wherein, n >=5,
Wherein, n >=5,
Wherein, n >=5,
Wherein, n >=5,
Described static inhibitor is one or more the mixture in the organic compound of following structure, and concrete structure formula is as follows,
Wherein, n >=10,
Wherein, n >=10;
Described B component is made up of the raw material of following weight part: base-material 84 ~ 94.9 parts, linking agent 5 ~ 15 parts, 0.1 ~ 1 part, inhibitor;
Wherein, described in A and B, base-material is the organopolysiloxane containing vinyl and the resin compound containing vinyl.
2. antistatic silicone gel according to claim 1, is characterized in that, the described organopolysiloxane containing vinyl is that vinyl bonds is combined on organopolysiloxane molecules chain end, molecular chain side chain or molecule chain end and side chain.
3. antistatic silicone gel according to claim 2, is characterized in that, the described organopolysiloxane containing vinyl is the organopolysiloxane or its mixture that at least contain two vinyl.
4. according to the arbitrary described antistatic silicone gel of claims 1 to 3, it is characterized in that, the described resin containing vinyl is vinyl MQ resin or vinyl MDT resin,
Described vinyl MQ resin is the raw material of low volatile content, and at fugitive constituent 150 DEG C, mass loss in 2 hours is less than 0.5%, and viscosity is 500 ~ 10000 centipoises, and the content of vinyl is 0.01 ~ 5wt%, and molecular formula is as follows:
(Me 3siO 0.5) a(ViMe 2siO 0.5) b(SiO 2) molecular formula 1
Wherein, a=0 ~ 1.5, b=0 ~ 1.5;
Described vinyl MDT resin is the raw material of low volatile content, and at fugitive constituent 150 DEG C, mass loss in 2 hours is less than 0.5%, and viscosity is 500 ~ 10000 centipoises, and the content of vinyl is 0.01 ~ 5wt%, and molecular formula is as follows:
(Me 3siO 0.5) a(ViMe 2siO 0.5) b(Me 2siO) (MeSiO 1.5) molecular formula 2
Wherein, a=0 ~ 1.5, b=0 ~ 1.5.
5. antistatic silicone gel according to claim 4, it is characterized in that, described linking agent is the organic hydrogen polysiloxanes being bonded to the hydrogen atom in hydrogen containing siloxane molecule on Siliciumatom containing two or more, and hydrogen content is 0.01 ~ 2wt%, and viscosity is 10 ~ 100 centipoises;
Described inhibitor is alkynes alcohols material.
6. a preparation method for the antistatic silicone gel for heat-conducting pad as described in as arbitrary in claim 1-5, is characterized in that, comprising:
The preparation of component A: under 25 DEG C of conditions, by the base-material of 95 ~ 99.84 weight parts, the catalyzer of 0.1 ~ 1 weight part, the caking agent of 0.05 ~ 2 weight part, the static inhibitor of 0.01 ~ 2 weight part joins in stirrer successively, mixes, and obtains described component A;
The preparation of B component: under 25 DEG C of conditions, by the base-material of 84 ~ 94.9 weight parts, the linking agent of 5 ~ 15 weight parts, the inhibitor of 0.1 ~ 1 weight part, joins successively in stirrer, mixes, and obtains described B component;
Under 25 DEG C of conditions, component A and B component are mixed by the weight proportion of 1:1, in the middle of the mixing raw material system sizing material of mixing being placed in heat-conducting pad, deaeration 10 ~ 40 minutes under 0.05 ~-0.1MPa vacuum, 100 ~ 150 DEG C of heating solidification in 0.4 ~ 2 hour, to obtain final product.
7. preparation method according to claim 6, described vacuum condition is 0.08MPa, deaeration 30 minutes; The described condition be heating and curing is 125 DEG C of heating 30 minutes.
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