CN103059209B - Weather-resistant resin for hot-stamping film and preparation method of resin - Google Patents
Weather-resistant resin for hot-stamping film and preparation method of resin Download PDFInfo
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- CN103059209B CN103059209B CN201310030877.0A CN201310030877A CN103059209B CN 103059209 B CN103059209 B CN 103059209B CN 201310030877 A CN201310030877 A CN 201310030877A CN 103059209 B CN103059209 B CN 103059209B
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Abstract
The invention discloses a weather-resistant resin for a hot-stamping film and a preparation method of the resin. The weather-resistant resin comprises the following compounds in parts by weight: 21-24 parts of acrylic hard monomers, 6-9 parts of acrylic soft monomers, 67-73 parts of solvents and 0.0135-0.066 parts of initiator; the preparation method comprises the following steps: (1) uniformly mixing all of the acrylic hard monomers and the acrylic soft monomers; (2) weighing 40% of the mixed monomers and 30% of the solvent in percentage by weight for uniformly mixing, heating up and reflowing the mixture in a reaction kettle; (3) weighing 40% of the solvent and 70% of the initiator in percentage by weight to mix with the residual monomers, dropping the mixture to the reaction kettle, controlling the reaction time between one hour and 1.5 hours, and keeping the reflow status to implement thermal insulation reaction for one hour to two hours after the dropping is completed; (4) weighing 30% of the solvent in percentage by weight to uniformly mix with the residual initiator, dropping the mixture to the reaction kettle, controlling the reaction time within the range of 0.5 hour and one hour, and keeping the reflow status to implement thermal insulation reaction for two hours to three hours after the dropping is completed; and (5) cooling and discharging to obtain the weather-resistant resin for the hot-stamping film.
Description
Technical field
The present invention relates to a kind of weathering resistance resin and preparation method thereof, particularly relate to a kind of blocking film weathering resistance resin and preparation method thereof.
Background technology
Blocking film is a kind of laminated film being coated with parting agent, pigment, heat-sensitive resin on a plastic film, the coating of this film can be transferred on printable fabric under applying certain temperature and pressure, therefore, thermoprint film can substitute now widely used silk screen printing, roll marks, spraying, brushing etc., and the such as application of furniture, collector surface color layers all can use thermoprint technical substitution.The advantage of thermoprint technology significantly to improve the operating environment of user, in the process of color attachment transfer, be different from traditional printing technology, do not have a large amount of VOC discharges, also do not need to carry out ink setting during thermoprint.
At present, important component part heat-sensitive resin as blocking film mainly plays binding function, generally speaking, different resin systems can be selected to obtain best interlayer attachment fastness for different printable fabrics, common at present, as cerul resin, urethane resin, polyvinyl chloride (PVC) RESINS etc. are widely used on paper and cloth-based material.As everyone knows, for general application scenario as the product such as furniture, electrical equipment, clothes of indoor requires not to be high especially to the weather-resistant property of coating.But the thermoprint material that some particular application such as license plate, traffic mark board, billboard adopt requires just high especially to the weathering resistance of heat-sensitive resin, therefore, this heat-sensitive resin, except meeting except the requirement of adhesion property, also needs satisfied outdoor complex conditions as the durability requirements of the factor such as impact, gasoline corrosion of uviolizing, dust storm.
Summary of the invention
The present invention is directed to the durability requirements that cannot meet outdoor complex conditions existed in prior art, provide a kind ofly have that UV resistant is irradiated, the blocking film weathering resistance resin of strong, the excellent performance of resistance to gasoline corrosion of anti-blown sand performance and preparation method thereof.
In order to solve the problems of the technologies described above, the present invention is achieved through the following technical solutions:
A preparation method for blocking film weathering resistance resin, is characterized in that the composition preparation comprising following weight proportion:
Hard monomer 21-24,
Soft monomer 6-9,
Solvent 67-73,
Initiator 0.0135-0.066;
Preparation process is as follows:
(1) take vinylformic acid hard monomer and the vinylformic acid soft monomer of above-mentioned weight ratio, all mix;
(2) take 40% of the total monomer weight mixed in above-mentioned steps (1), take above-mentioned weight of solvent than 30% of total amount, mix, enter reactor and be heated to backflow;
(3) take above-mentioned weight of solvent than total amount 40%, take above-mentioned initiator weight ratio total amount 70% after taking through step (2) whole monomers of remainder mix, be added drop-wise in the reactor described in step (2), time for adding is 1-1.5 hour, keeps reflux state insulation reaction 1-2 hour again after being added dropwise to complete;
(4) weight of solvent is taken than 30% of total amount, mix with by whole initiators of remainder after taking through above-mentioned steps (3), be added drop-wise in the reactor described in step (3), time for adding is 0.5-1 hour, keeps reflux state insulation reaction 2-3 hour again after being added dropwise to complete;
(5) cooling discharging, obtains a kind of blocking film weathering resistance resin.
Prepare blocking film weathering resistance resin by above-mentioned steps, owing to adopting reaction step by step, can avoid discharging amount of heat, explosion caused danger; In the control reaction times step by step, better can control molecular weight and the second-order transition temperature of resin, thus make the weathering resistance of resin and tack good.
As preferably, the preparation method of above-mentioned a kind of blocking film weathering resistance resin, described initiator weight is the 0.056%-0.182% of vinylformic acid hard monomer and vinylformic acid soft monomer total amount.Select the initiator in above-mentioned scope, monomer conversion is best, and the properties of resin is excellent, is embodied in: anti-blown sand performance is strong, the excellent performance of resistance to gasoline corrosion, UV resistant are irradiated; Initiator weighs less than 0.056% of vinylformic acid hard monomer and vinylformic acid soft monomer total amount, and reaction not exclusively; Initiator weight, higher than 0.182% of vinylformic acid hard monomer and vinylformic acid soft monomer total amount, can cause the waste of initiator, and cost increases.
As preferably, the preparation method of above-mentioned a kind of blocking film weathering resistance resin, described initiator is benzoyl peroxide.Select this initiator, the reaction of monomer can be made more complete, effectively control reaction efficiency.Initiator also can select azo-bis-isobutyl cyanide or azo two cyanogen in different heptan.
As preferably, the preparation method of above-mentioned a kind of blocking film weathering resistance resin, described solvent is that the formulated in combination of any one or two kinds of components in toluene or methyl iso-butyl ketone (MIBK) forms, and the weight ratio of the formulated in combination of described toluene and methyl iso-butyl ketone (MIBK) two kinds of components is 1: 1 to 3: 1.Select above-mentioned solvent or its combination, effectively can control the temperature of reaction of monomer, reduce reaction system viscosity, make it fully react.Solvent also can select the combination of vinyl acetic monomer or N-BUTYL ACETATE or vinyl acetic monomer and toluene, or N-BUTYL ACETATE and toluene two kinds of components formulated.
As preferably, the preparation method of above-mentioned a kind of blocking film weathering resistance resin, described vinylformic acid hard monomer comprises any one in methyl methacrylate or β-dimethyl-aminoethylmethacrylate or vinylbenzene.
As preferably, the preparation method of above-mentioned a kind of blocking film weathering resistance resin, described vinylformic acid hard monomer is that the formulated in combination of methyl methacrylate and β-dimethyl-aminoethylmethacrylate two kinds of components forms, and the weight ratio of the formulated in combination of described methyl methacrylate and β-dimethyl-aminoethylmethacrylate two kinds of components is 4: 1 to 7: 1.
As preferably, the preparation method of above-mentioned a kind of blocking film weathering resistance resin, described vinylformic acid hard monomer is that the formulated in combination of methyl methacrylate and vinylbenzene two kinds of components forms, and the weight ratio of the formulated in combination of described methyl methacrylate and vinylbenzene two kinds of components is 10:1 to 15:1.
Select aforesaid propylene acid hard monomer or its combination, the weathering resistance of resin, resistance to deformation behavior, solvent resistance can be made better.
As preferably, the preparation method of above-mentioned a kind of blocking film weathering resistance resin, described vinylformic acid soft monomer is that the formulated in combination of any one or any two components in butyl methacrylate or methyl acrylate or vinyl acetate forms, the weight ratio of the formulated in combination of described butyl methacrylate and methyl acrylate two kinds of components is 3:1 to 5:1, the weight ratio of the formulated in combination of described butyl methacrylate and vinyl acetate two kinds of components is 5:1 to 8:1, the weight ratio of the formulated in combination of described methyl acrylate and vinyl acetate two kinds of components is 4:3 to 7:3.Select the aching and limp monomer of aforesaid propylene or its combination, the snappiness of resin, ductility can be made better, improve its attachment fastness simultaneously.
A kind of blocking film weathering resistance resin, prepares gained by the preparation method of any one blocking film weathering resistance resin above-mentioned.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but they are not limitations of the present invention:
embodiment 1
A preparation method for blocking film weathering resistance resin, comprises the composition preparation of following weight proportion:
21 parts of vinylformic acid hard monomers, 6 parts of vinylformic acid soft monomers, 67 parts of solvents, 0.0135 part of initiator, preparation process is as follows:
(1) take vinylformic acid hard monomer and the vinylformic acid soft monomer of above-mentioned weight ratio, all mix;
(2) take 40% of the total monomer weight mixed in above-mentioned steps (1), take above-mentioned weight of solvent than 30% of total amount, mix, enter reactor and be heated to backflow;
(3) take above-mentioned weight of solvent than total amount 40%, take above-mentioned initiator weight ratio total amount 70% after taking through step (2) whole monomers of remainder mix, be added drop-wise in the reactor described in step (2), time for adding is 1-1.5 hour, keeps reflux state insulation reaction 1-2 hour again after being added dropwise to complete;
(4) weight of solvent is taken than 30% of total amount, mix with by whole initiators of remainder after taking through above-mentioned steps (3), be added drop-wise in the reactor described in step (3), time for adding is 0.5-1 hour, keeps reflux state insulation reaction 2-3 hour again after being added dropwise to complete;
(5) cooling discharging, obtains a kind of blocking film weathering resistance resin.
Initiator is preferably benzoyl peroxide.
Solvent preferably selects toluene or methyl iso-butyl ketone (MIBK).
Vinylformic acid hard monomer preferably selects methyl methacrylate or β-dimethyl-aminoethylmethacrylate or vinylbenzene.
Vinylformic acid soft monomer preferably selects butyl methacrylate or methyl acrylate or vinyl acetate.
embodiment 2
A preparation method for blocking film weathering resistance resin, comprises the composition preparation of following weight proportion:
21 parts of vinylformic acid hard monomers, 9 parts of vinylformic acid soft monomers, 73 parts of solvents, 0.066 part of initiator.
Solvent is the combination of toluene and methyl iso-butyl ketone (MIBK), and two kinds of component weight ratios control to prepare at 1:1 to 3:1.
The proportioning of other component and implementation step are with above-described embodiment 1.
Initiator is preferably benzoyl peroxide.
Vinylformic acid hard monomer preferably selects methyl methacrylate or β-dimethyl-aminoethylmethacrylate or vinylbenzene.
Vinylformic acid soft monomer preferably selects butyl methacrylate or methyl acrylate or vinyl acetate.
embodiment 3
A preparation method for blocking film weathering resistance resin, comprises the composition preparation of following weight proportion:
24 parts of vinylformic acid hard monomers, 9 parts of vinylformic acid soft monomers, 73 parts of solvents, 0.066 part of initiator.
Vinylformic acid hard monomer is that the formulated in combination of methyl methacrylate and β-dimethyl-aminoethylmethacrylate two kinds of components forms, and the weight ratio of the formulated in combination of described methyl methacrylate and β-dimethyl-aminoethylmethacrylate two kinds of components controls at 4:1 to 7:1.
The proportioning of other component and implementation step are with above-described embodiment 1.
Initiator is preferably benzoyl peroxide.
Solvent preferably selects toluene or methyl iso-butyl ketone (MIBK).
Vinylformic acid soft monomer preferably selects butyl methacrylate or methyl acrylate or vinyl acetate.
embodiment 4
A preparation method for blocking film weathering resistance resin, comprises the composition preparation of following weight proportion:
24 parts of vinylformic acid hard monomers, 6 parts of vinylformic acid soft monomers, 67 parts of solvents, 0.0135 part of initiator.
Vinylformic acid hard monomer is that the formulated in combination of methyl methacrylate and vinylbenzene two kinds of components forms, and the weight ratio of the formulated in combination of described methyl methacrylate and vinylbenzene two kinds of components controls at 10:1 to 15:1.
The proportioning of other component and implementation step are with above-described embodiment 1.
Initiator is preferably benzoyl peroxide.
Solvent preferably selects toluene or methyl iso-butyl ketone (MIBK).
Vinylformic acid soft monomer preferably selects butyl methacrylate or methyl acrylate or vinyl acetate.
embodiment 5
A preparation method for blocking film weathering resistance resin, comprises the composition preparation of following weight proportion:
22 parts of vinylformic acid hard monomers, 7 parts of vinylformic acid soft monomers, 70 parts of solvents, 0.0135 part of initiator.
Vinylformic acid soft monomer is that the formulated in combination of butyl methacrylate and methyl acrylate two kinds of components forms, and the weight ratio of the formulated in combination of described butyl methacrylate and methyl acrylate two kinds of components controls at 3:1 to 5:1.
The proportioning of other component and implementation step are with above-described embodiment 1.
Initiator is preferably benzoyl peroxide.
Solvent preferably selects toluene or methyl iso-butyl ketone (MIBK).
Vinylformic acid hard monomer preferably selects methyl methacrylate or β-dimethyl-aminoethylmethacrylate or vinylbenzene.
embodiment 6
A preparation method for blocking film weathering resistance resin, comprises the composition preparation of following weight proportion:
23 parts of vinylformic acid hard monomers, 8 parts of vinylformic acid soft monomers, 71 parts of solvents, 0.04 part of initiator.
Vinylformic acid soft monomer is that the formulated in combination of butyl methacrylate and vinyl acetate two kinds of components forms, and the weight ratio of the formulated in combination of described butyl methacrylate and vinyl acetate two kinds of components controls at 5:1 to 8:1.
The proportioning of other component and implementation step are with above-described embodiment 1.
Initiator is preferably benzoyl peroxide.
Solvent preferably selects toluene or methyl iso-butyl ketone (MIBK).
Vinylformic acid hard monomer preferably selects methyl methacrylate or β-dimethyl-aminoethylmethacrylate or vinylbenzene.
embodiment 7
A preparation method for blocking film weathering resistance resin, comprises the composition preparation of following weight proportion:
24 parts of vinylformic acid hard monomers, 6 parts of vinylformic acid soft monomers, 73 parts of solvents, 0.066 part of initiator.
Vinylformic acid soft monomer is that the formulated in combination of methyl acrylate and vinyl acetate two kinds of components forms, and the weight ratio of the formulated in combination of described methyl acrylate and vinyl acetate two kinds of components controls at 4:3 to 7:3.
The proportioning of other component and implementation step are with above-described embodiment 1.
Initiator is preferably benzoyl peroxide.
Solvent preferably selects toluene or methyl iso-butyl ketone (MIBK).
Vinylformic acid hard monomer preferably selects methyl methacrylate or β-dimethyl-aminoethylmethacrylate or vinylbenzene.
embodiment 8
A preparation method for blocking film weathering resistance resin, comprises the composition preparation of following weight proportion:
24 parts of vinylformic acid hard monomers, 9 parts of vinylformic acid soft monomers, 67 parts of solvents, 0.066 part of initiator.
The proportioning of other component and implementation step are with above-described embodiment 1.
Initiator is preferably benzoyl peroxide.
Solvent preferably selects toluene or methyl iso-butyl ketone (MIBK).
Vinylformic acid hard monomer preferably selects methyl methacrylate or β-dimethyl-aminoethylmethacrylate or vinylbenzene.
Vinylformic acid soft monomer preferably selects butyl methacrylate or methyl acrylate or vinyl acetate.
embodiment 9
A preparation method for blocking film weathering resistance resin, comprises the composition preparation of following weight proportion:
21 parts of vinylformic acid hard monomers, 9 parts of vinylformic acid soft monomers, 67 parts of solvents, 0.02 part of initiator.
The proportioning of other component and implementation step are with above-described embodiment 1.
Initiator is preferably benzoyl peroxide.
Solvent preferably selects toluene or methyl iso-butyl ketone (MIBK).
Vinylformic acid hard monomer preferably selects methyl methacrylate or β-dimethyl-aminoethylmethacrylate or vinylbenzene.
Vinylformic acid soft monomer preferably selects butyl methacrylate or methyl acrylate or vinyl acetate.
embodiment 10
A preparation method for blocking film weathering resistance resin, comprises the composition preparation of following weight proportion:
21 parts of vinylformic acid hard monomers, 6 parts of vinylformic acid soft monomers, 73 parts of solvents, 0.0135 part of initiator.
The proportioning of other component and implementation step are with above-described embodiment 1.
Initiator is preferably benzoyl peroxide.
Solvent preferably selects toluene or methyl iso-butyl ketone (MIBK).
Vinylformic acid hard monomer preferably selects methyl methacrylate or β-dimethyl-aminoethylmethacrylate or vinylbenzene.
Vinylformic acid soft monomer preferably selects butyl methacrylate or methyl acrylate or vinyl acetate.
embodiment 11
A preparation method for blocking film weathering resistance resin, comprises the composition preparation of following weight proportion:
24 parts of vinylformic acid hard monomers, 9 parts of vinylformic acid soft monomers, 73 parts of solvents, 0.0135 part of initiator.
The proportioning of other component and implementation step are with above-described embodiment 1.
Initiator is preferably benzoyl peroxide.
Solvent preferably selects toluene or methyl iso-butyl ketone (MIBK).
Vinylformic acid hard monomer preferably selects methyl methacrylate or β-dimethyl-aminoethylmethacrylate or vinylbenzene.
Vinylformic acid soft monomer preferably selects butyl methacrylate or methyl acrylate or vinyl acetate.
embodiment 12
A preparation method for blocking film weathering resistance resin, comprises the composition preparation of following weight proportion:
21 parts of vinylformic acid hard monomers, 6 parts of vinylformic acid soft monomers, 67 parts of solvents, 0.066 part of initiator.
The proportioning of other component and implementation step are with above-described embodiment 1.
Initiator is preferably benzoyl peroxide.
Solvent preferably selects toluene or methyl iso-butyl ketone (MIBK).
Vinylformic acid hard monomer preferably selects methyl methacrylate or β-dimethyl-aminoethylmethacrylate or vinylbenzene.
Vinylformic acid soft monomer preferably selects butyl methacrylate or methyl acrylate or vinyl acetate.
embodiment 13
A preparation method for blocking film weathering resistance resin, comprises the composition preparation of following weight proportion:
21 parts of vinylformic acid hard monomers, 6 parts of vinylformic acid soft monomers, 73 parts of solvents, 0.015 part of initiator.
The proportioning of other component and implementation step are with above-described embodiment 1.
Initiator is preferably benzoyl peroxide.
Solvent preferably selects toluene or methyl iso-butyl ketone (MIBK).
Vinylformic acid hard monomer preferably selects methyl methacrylate or β-dimethyl-aminoethylmethacrylate or vinylbenzene.
Vinylformic acid soft monomer preferably selects butyl methacrylate or methyl acrylate or vinyl acetate.
embodiment 14
A preparation method for blocking film weathering resistance resin, comprises the composition preparation of following weight proportion:
24 parts of vinylformic acid hard monomers, 6 parts of vinylformic acid soft monomers, 67 parts of solvents, 0.06 part of initiator.
Vinylformic acid hard monomer is that the formulated in combination of methyl methacrylate and vinylbenzene two kinds of components forms, and the weight ratio of the formulated in combination of described methyl methacrylate and vinylbenzene two kinds of components controls at 10:1 to 15:1.
The proportioning of other component and implementation step are with above-described embodiment 1.
Initiator is preferably benzoyl peroxide.
Solvent preferably selects toluene or methyl iso-butyl ketone (MIBK).
Vinylformic acid soft monomer preferably selects butyl methacrylate or methyl acrylate or vinyl acetate.
In a word, the foregoing is only preferred embodiment of the present invention, all equalizations done according to the scope of the present patent application patent change and modify, and all should belong to covering scope of the present invention.
Claims (4)
1. a blocking film preparation method for weathering resistance resin, is characterized in that: the composition preparation comprising following weight proportion:
Vinylformic acid hard monomer 21-24,
Vinylformic acid soft monomer 6-9,
Solvent 67-73,
Initiator 0.0135-0.066;
Described solvent is that the formulated in combination of any one or two kinds of components in toluene or methyl iso-butyl ketone (MIBK) forms, the weight ratio of the formulated in combination of described toluene and methyl iso-butyl ketone (MIBK) two kinds of components is 1:1 to 3:1, described vinylformic acid hard monomer is that the formulated in combination of methyl methacrylate and β-dimethyl-aminoethylmethacrylate two kinds of components forms, the weight ratio of the formulated in combination of described methyl methacrylate and β-dimethyl-aminoethylmethacrylate two kinds of components is 4:1 to 7:1, described vinylformic acid soft monomer is that the formulated in combination of any one or two kinds of components in butyl methacrylate or methyl acrylate forms, the weight ratio of the formulated in combination of described butyl methacrylate and methyl acrylate two kinds of components is 3:1 to 5:1,
Preparation process is as follows:
(1) take vinylformic acid hard monomer and the vinylformic acid soft monomer of above-mentioned weight ratio, all mix;
(2) take 40% of the total monomer weight mixed in above-mentioned steps (1), take above-mentioned weight of solvent than 30% of total amount, mix, enter reactor and be heated to backflow;
(3) take above-mentioned weight of solvent than total amount 40%, take 70% of above-mentioned initiator weight ratio total amount, whole monomers of remainder mix after taking through step (2), be added drop-wise in the reactor described in step (2), time for adding is 1-1.5 hour, keeps reflux state insulation reaction 1-2 hour again after being added dropwise to complete;
(4) weight of solvent is taken than 30% of total amount, mix with by whole initiators of remainder after taking through above-mentioned steps (3), be added drop-wise in the reactor described in step (3), time for adding is 0.5-1 hour, keeps reflux state insulation reaction 2-3 hour again after being added dropwise to complete;
(5) cooling discharging, obtains a kind of blocking film weathering resistance resin.
2. the preparation method of a kind of blocking film weathering resistance resin according to claim 1, is characterized in that: described initiator weight is the 0.056%-0.182% of vinylformic acid hard monomer and vinylformic acid soft monomer total amount.
3. the preparation method of a kind of blocking film weathering resistance resin according to claim 1, is characterized in that: described initiator is benzoyl peroxide.
4. a blocking film weathering resistance resin, is characterized in that: prepare obtained by the preparation method of any one blocking film weathering resistance resin in claim 1-3.
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| CN106893534A (en) * | 2017-03-02 | 2017-06-27 | 浙江龙游道明光学有限公司 | For road sign reflective membrane hot soarfing from pressure sensitive adhesive and preparation method thereof |
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| CN104004476B (en) * | 2014-05-13 | 2017-07-07 | 佛山市南海高拓包装材料有限公司 | Adhesive for electrochemical aluminium thermoprinting and preparation method thereof and anodized aluminium |
| CN107384263A (en) * | 2017-08-18 | 2017-11-24 | 佛山市永恒达新材料科技有限公司 | The adhesive of high durable, high-adhesive-strength |
| CN108102021A (en) * | 2017-12-30 | 2018-06-01 | 张义群 | Highlighted thermoprint packing box glazing transfer membrane and its manufacture craft |
| CN109651559B (en) * | 2018-12-11 | 2021-11-09 | 上海绘兰材料科技有限公司 | Acrylic resin for release-free ironing cloth electrochemical aluminum and preparation method and application thereof |
| CN110435320B (en) * | 2019-08-14 | 2021-08-03 | 河南科技大学 | Production process of heat transfer film for solvent-free infusion soft bag |
| CN115340833B (en) * | 2021-12-02 | 2023-11-10 | 广东邦固化学科技有限公司 | Environment-friendly aqueous back glue for tipping paper thermoprinting film for high-speed ironing and preparation method thereof |
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| ATE400624T1 (en) * | 2001-12-07 | 2008-07-15 | 3M Innovative Properties Co | ACRYLIC PRESSURE SENSITIVE HOT HOT ADHESIVE AND USE THEREOF |
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