CN109206616A - A kind of preparation method of the organic foam stabilizer with flame retardant property - Google Patents
A kind of preparation method of the organic foam stabilizer with flame retardant property Download PDFInfo
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- CN109206616A CN109206616A CN201810901362.6A CN201810901362A CN109206616A CN 109206616 A CN109206616 A CN 109206616A CN 201810901362 A CN201810901362 A CN 201810901362A CN 109206616 A CN109206616 A CN 109206616A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0014—Use of organic additives
- C08J9/0042—Use of organic additives containing silicon
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Abstract
The invention belongs to macromolecular stabilizer agent fields, and in particular to a kind of preparation method of the organic foam stabilizer with flame retardant property；The composition of a kind of organic foam stabilizer with flame retardant property are as follows: mass fraction is 20-30 parts of dimethyldichlorosilane, 40-60 parts of xylyl dichlorosilane, 60-100 parts of active silicic acid sodium, 2-4 parts of acid-base modifier, 1-2 parts of initiator, 120-150 parts of mixed solvent, 4-5 parts of catalyst；The stabilizer prepared through the invention, there is good flame retardant effect because of rolling into a ball containing a large amount of siloxy, additionally since the active force between lone pair electrons on intermolecular active force and oxygen makes it have good emulsifying effectiveness, simultaneously, because it has a large amount of benzene radicals, with good heat insulation.
Description
Technical field
The invention belongs to macromolecular stabilizer agent fields, and in particular to a kind of organic foam stabilizer with flame retardant property
Preparation method.
Background technique
Organic foam stabilizer is a kind of object largely applied in hard or flexible polyurethane material synthesis process
Matter, wide range of applications.
Chinese patent application CN 103910887B discloses a kind of applied to the organic of single-component cranny filler of polyurethane foam
The preparation method of silicon foam stabilizer, step are as follows: (1) allyl alcohol, ethylene oxide and propylene oxide are added in a kettle, in alkali
Property catalyst action under, be not more than 0.5MPa controlled at 90~130 DEG C, pressure, 4~6h obtains allyl capped copolyether；
(2) polyethers prepared by step 1 is reacted at 85~120 DEG C with metallic sodium, is passed through excessive halogenated alkane, 4~6h of reaction obtains first
Base blocks copolyether；(3) the high containing hydrogen silicone oil for being 1~2% by octamethylcy-clotetrasiloxane, hexamethyldisiloxane and hydrogen content
2~6h is reacted in the presence of acid ion exchangers obtains the silicon oil of low hydrogen content that hydrogen content is 0.05~1.0%；(4) by steps 1 and 2
Catalyst is added with 3 product mixes, 3~8h of reaction obtains organic foam stabilizer under the conditions of pressure is 0.5~2atm, is made
Foam stabiliser there is good dimensional stability, higher expansion ratio and mobility, but its flame retardant property in foaming
It is poor.
Chinese patent application CN 107722846A discloses a kind of hard polyaminoester or polyisocyanurate foam of producing
Method, by by isocyanates and polyalcohol urethanes and/or isocyanurate catalyst, water, it is optional its
His foaming agent, optional fire retardant and other optional additives (such as: filler, emulsifier, pure organic stabilizer and surface
Activating agent, thinner, dyestuff, antioxidant, UV stabilizer, antistatic agent) in the presence of reacted, used have general formula
(I) foam stabiliser R-Si (CH3) 2-O- [- Si (CH3) 2-O-] n- [- Si (CH3) R-O-] m-Si (CH3) 2-R, wherein R
=-(CH2) x-O- (CH2-CHR '-O) y-R ", preparation method is relatively easy, but the stablizing effect of its stabilizer is poor.
For above-mentioned there are problem, a kind of organic foam stabilizer with flame retardant property is researched and developed to meet the market demand
Seem even more important.
Summary of the invention
In order to achieve the purpose that in background technique, the organic foam stabilizer proposed by the present invention with flame retardant property
Preparation method；The stabilizer prepared through the invention has good flame retardant effect because of rolling into a ball containing a large amount of siloxy, this
Active force between the outer lone pair electrons because of on intermolecular active force and oxygen makes it have good emulsifying effectiveness, meanwhile,
Because it has a large amount of benzene radicals, with fine heat insulation.
What the present invention realized by the following technical solutions:
A kind of preparation method of the organic foam stabilizer with flame retardant property, it is characterised in that described one kind has fire-retardant
The composition of the organic foam stabilizer of performance are as follows: mass fraction is 20-30 parts of dimethyldichlorosilane, the two of 40-60 parts
Tolyl dichlorosilane, 60-100 parts of active silicic acid sodium, 2-4 parts of acid-base modifier, 1-2 parts of initiator, 120-150 parts
Mixed solvent, 4-5 parts of catalyst.
Further, a kind of organic foam stabilizer with flame retardant property the preparation method comprises the following steps: by reaction kettle
Temperature maintains 65-75 DEG C, and mechanical agitator revolving speed is 200-300rpm, and it is molten that 120-150 parts of mixing is added into reaction kettle
Agent, after constant temperature 1-2 hours, by 60-100 parts of active silicic acid sodium, 2-4 parts of acid-base modifier, 40-60 parts of xylyl two
Chlorosilane is added in reaction kettle, the speed with 1-2s/ drop of 20-30 parts of dimethyldichlorosilane is added dropwise on one side, separately
1-2 parts of initiator is added dropwise in an outer constant pressure buret with the speed of 5-10s/ drop, by 4-5 parts after being added dropwise completely
Catalyst is added dropwise with the speed of 3-5s/ drop, after being added dropwise completely, keeps reacting 1-2 hours under this condition, then by temperature liter
It is 2-5 DEG C high, it reacts 1-2 hours, is spray-dried the substance after fully reacting, drying temperature is controlled at 50-80 DEG C, is removed
It goes the substance obtained after solvent to be added in distilled water to impregnate 5-10 hours, after rinsing 2-3 times, obtained object is dried, dry
The substance obtained after dry is exactly the organic foam stabilizer with flame retardant property.
Further, the active silicic acid sodium are as follows: 100-120 parts of sodium metasilicate is added in a kettle, temperature is increased
To 40-60 DEG C, 4-5 parts of sodium citrate, 1-2 parts of lauric acid, 0.5-1 parts of stearic acid is added, it is cooling after reaction 2-3 hours
The substance obtained to room temperature, the substance are exactly active silicic acid sodium.
Further, the initiator are as follows: by 1-2 parts, object that 2-5 parts of organotin is obtained after mixing
Matter, the substance are exactly initiator.
Further, the acid-base modifier are as follows: by 1-2 parts of sodium bicarbonate, 3-5 parts of sodium carbonate, 1-2 parts of nanometer
Lotus leaf hydrophobing agent, 1-2 parts of stearic acid, 1-2 parts of silane coupling agent are added in reaction kettle, carry out under the conditions of 30-40 DEG C anti-
It answers, room temperature is cooled to after fully reacting, the substance obtained after product is crushed, the substance is exactly acid-base modifier.
Further, the mixed solvent are as follows: obtained the DMF of 10-20:4-5 and hexamethylene after mixing
Substance, the substance are exactly mixed solvent.
Further, the catalyst are as follows: 1-2 parts of butyl lithium is dissolved in 20-30 parts of hexamethylene, is configured to
Solution, the substance are exactly catalyst.
Further, the reaction condition in the claim 2 are as follows: entire reaction all carries out in anhydrous conditions.
Beneficial to benefit
1, the present invention carries out triblock copolymer using dimethyldichlorosilane, xylyl dichlorosilane, active silicic acid sodium, because
There is good flame retardant effect to roll into a ball containing a large amount of siloxy；
2, triblock copolymer prepared by the present invention, because of the active force between lone pair electrons on intermolecular active force and oxygen
Make it have good emulsifying effectiveness；
3, triblock copolymer prepared by the present invention has good heat-insulated effect because it has a large amount of benzene radicals
Fruit.
Specific embodiment
In order to keep the purpose of the present invention, technical scheme and beneficial effects clearer, below in conjunction with experimental data, to this
The preferred embodiment of invention is described in detail, to facilitate the technical staff to understand.
Embodiment 1
A kind of organic foam stabilizer with flame retardant property the preparation method comprises the following steps: temperature of reaction kettle is maintained 75 DEG C, machine
Tool agitator speed is 200rpm, 120 parts of mixed solvent is added into reaction kettle, after constant temperature 1-2 hours, by 100 parts of work
Property sodium metasilicate, 4 parts of acid-base modifier, 40 parts xylyl dichlorosilane be added reaction kettle in, on one side by 20 parts of diformazan
The speed with 2s/ drop of base dichlorosilane is added dropwise, in addition in a constant pressure buret 2 parts of initiator with the speed of 10s/ drop
Degree is added dropwise, and 4 parts of catalyst is added dropwise with the speed of 3s/ drop after being added dropwise completely, and after being added dropwise completely, keeping should
Under the conditions of react 1-2 hours, then by temperature increase 5 DEG C, react 2 hours, the substance is spray-dried after fully reacting,
Drying temperature, which controls the substance for removing at 65 DEG C and obtaining after solvent and is added in distilled water, to be impregnated 10 hours, after rinsing 3 times, will
To object dried, the substance obtained after drying is exactly the organic foam stabilizer with flame retardant property.
Further, the active silicic acid sodium are as follows: 120 parts of sodium metasilicate is added in a kettle, raises the temperature to 60
DEG C, 5 parts of sodium citrate, 2 parts of lauric acid, 1 part of stearic acid is added, the substance being cooled to room temperature after reacting 3 hours,
The substance is exactly active silicic acid sodium.
Further, the initiator are as follows: by 1 part, substance that 5 parts of organotin is obtained after mixing, should
Substance is exactly initiator.
Further, the acid-base modifier are as follows: dredge 2 parts of sodium bicarbonate, 5 parts of sodium carbonate, 2 parts of nano-lotus leaf
Aqua, 1 part of stearic acid, 2 parts of silane coupling agent are added in reaction kettle, are reacted under the conditions of 40 DEG C, after fully reacting
It is cooled to room temperature, the substance obtained after product is crushed, the substance is exactly acid-base modifier.
Further, the mixed solvent are as follows: the substance for being obtained the DMF of 20:5 and hexamethylene after mixing,
The substance is exactly mixed solvent.
Further, the catalyst are as follows: 2 parts of butyl lithium is dissolved in 30 parts of hexamethylene, the solution being configured to,
The substance is exactly catalyst.
Further, the reaction condition in the claim 2 are as follows: entire reaction all carries out in anhydrous conditions.
Embodiment 2
A kind of organic foam stabilizer with flame retardant property the preparation method comprises the following steps: temperature of reaction kettle is maintained 75 DEG C, machine
Tool agitator speed is 300rpm, 150 parts of mixed solvent is added into reaction kettle, after constant temperature 1 hour, by 100 parts of activity
Sodium metasilicate, 2 parts of acid-base modifier, 60 parts of xylyl dichlorosilane are added in reaction kettle, on one side by 20 parts of dimethyl
The speed with 2s/ drop of dichlorosilane is added dropwise, in addition in a constant pressure buret 1 part of initiator with the speed of 5s/ drop
It is added dropwise, 4 parts of catalyst is added dropwise with the speed of 3s/ drop after being added dropwise completely, after being added dropwise completely, keep this
It is reacted 2 hours under part, then temperature is increased 2 DEG C, reacted 2 hours, be spray-dried the substance after fully reacting, dried
Temperature, which controls the substance for removing at 80 DEG C and obtaining after solvent and is added in distilled water, impregnates 10 hours, after rinsing 2 times, by what is obtained
Object is dried, and the substance obtained after drying is exactly the organic foam stabilizer with flame retardant property.
Further, the active silicic acid sodium are as follows: 120 parts of sodium metasilicate is added in a kettle, raises the temperature to 60
DEG C, 4-5 parts of sodium citrate, 1-2 parts of lauric acid, 1 part of stearic acid is added, what reaction was cooled to room temperature after 2 hours
Substance, the substance are exactly active silicic acid sodium.
Further, the initiator are as follows: by 1 part, substance that 5 parts of organotin is obtained after mixing, should
Substance is exactly initiator.
Further, the acid-base modifier are as follows: dredge 2 parts of sodium bicarbonate, 5 parts of sodium carbonate, 2 parts of nano-lotus leaf
Aqua, 1 part of stearic acid, 2 parts of silane coupling agent are added in reaction kettle, are reacted under the conditions of 40 DEG C, after fully reacting
It is cooled to room temperature, the substance obtained after product is crushed, the substance is exactly acid-base modifier.
Further, the mixed solvent are as follows: the substance for being obtained the DMF of 10:5 and hexamethylene after mixing,
The substance is exactly mixed solvent.
Further, the catalyst are as follows: 2 parts of butyl lithium is dissolved in 30 parts of hexamethylene, the solution being configured to,
The substance is exactly catalyst.
Further, the reaction condition in the claim 2 are as follows: entire reaction all carries out in anhydrous conditions.
Embodiment 3
A kind of organic foam stabilizer with flame retardant property the preparation method comprises the following steps: temperature of reaction kettle is maintained 75 DEG C, machine
Tool agitator speed is 200rpm, 125 parts of mixed solvent is added into reaction kettle, after constant temperature 2 hours, by 100 parts of activity
Sodium metasilicate, 4 parts of acid-base modifier, 60 parts of xylyl dichlorosilane are added in reaction kettle, on one side by 30 parts of dimethyl
The speed with 2s/ drop of dichlorosilane is added dropwise, in addition in a constant pressure buret 2 parts of initiator with the speed of 10s/ drop
It is added dropwise, 4 parts of catalyst is added dropwise with the speed of 3s/ drop after being added dropwise completely, after being added dropwise completely, keep this
It is reacted 1-2 hours under part, then temperature is increased 5 DEG C, reacted 2 hours, be spray-dried the substance after fully reacting, done
Dry temperature control removes the substance obtained after solvent and is added in distilled water and impregnate 10 hours, after rinsing 3 times, will obtain at 60 DEG C
Object dried, the substance obtained after drying is exactly the organic foam stabilizer with flame retardant property.
Further, the active silicic acid sodium are as follows: 100 parts of sodium metasilicate is added in a kettle, raises the temperature to 40
DEG C, 4 parts of sodium citrate, 2 parts of lauric acid, 1 part of stearic acid is added, the substance being cooled to room temperature after reacting 3 hours,
The substance is exactly active silicic acid sodium.
Further, the initiator are as follows: by 2 parts, substance that 5 parts of organotin is obtained after mixing, should
Substance is exactly initiator.
Further, the acid-base modifier are as follows: dredge 2 parts of sodium bicarbonate, 5 parts of sodium carbonate, 2 parts of nano-lotus leaf
Aqua, 1 part of stearic acid, 1 part of silane coupling agent are added in reaction kettle, are reacted under the conditions of 40 DEG C, after fully reacting
It is cooled to room temperature, the substance obtained after product is crushed, the substance is exactly acid-base modifier.
Further, the mixed solvent are as follows: the substance for being obtained the DMF of 20:4 and hexamethylene after mixing,
The substance is exactly mixed solvent.
Further, the catalyst are as follows: 1 part of butyl lithium is dissolved in 30 parts of hexamethylene, the solution being configured to,
The substance is exactly catalyst.
Further, the reaction condition in the claim 2 are as follows: entire reaction all carries out in anhydrous conditions.
Embodiment 4
A kind of organic foam stabilizer with flame retardant property the preparation method comprises the following steps: temperature of reaction kettle is maintained 65 DEG C, machine
Tool agitator speed is 300rpm, 120 parts of mixed solvent is added into reaction kettle, after constant temperature 1 hour, by 100 parts of activity
Sodium metasilicate, 2 parts of acid-base modifier, 40 parts of xylyl dichlorosilane are added in reaction kettle, on one side by 30 parts of dimethyl
The speed with 2s/ drop of dichlorosilane is added dropwise, in addition in a constant pressure buret 2 parts of initiator with the speed of 5s/ drop
It is added dropwise, 4 parts of catalyst is added dropwise with the speed of 5s/ drop after being added dropwise completely, after being added dropwise completely, keep this
It is reacted 2 hours under part, then temperature is increased 5 DEG C, reacted 2 hours, be spray-dried the substance after fully reacting, dried
Temperature, which controls the substance for removing at 50-80 DEG C and obtaining after solvent and is added in distilled water, impregnates 10 hours, after rinsing 2 times, will obtain
Object dried, the substance obtained after drying is exactly the organic foam stabilizer with flame retardant property.
Further, the active silicic acid sodium are as follows: 120 parts of sodium metasilicate is added in a kettle, raises the temperature to 60
DEG C, 5 parts of sodium citrate, 1 part of lauric acid, 1 part of stearic acid is added, the substance being cooled to room temperature after reacting 3 hours,
The substance is exactly active silicic acid sodium.
Further, the initiator are as follows: by 1 part, substance that 2 parts of organotin is obtained after mixing, should
Substance is exactly initiator.
Further, the acid-base modifier are as follows: dredge 2 parts of sodium bicarbonate, 5 parts of sodium carbonate, 2 parts of nano-lotus leaf
Aqua, 1 part of stearic acid, 1 part of silane coupling agent are added in reaction kettle, are reacted under the conditions of 40 DEG C, after fully reacting
It is cooled to room temperature, the substance obtained after product is crushed, the substance is exactly acid-base modifier.
Further, the mixed solvent are as follows: the substance for being obtained the DMF of 20:5 and hexamethylene after mixing,
The substance is exactly mixed solvent.
Further, the catalyst are as follows: 2 parts of butyl lithium is dissolved in 30 parts of hexamethylene, the solution being configured to,
The substance is exactly catalyst.
Further, the reaction condition in the claim 2 are as follows: entire reaction all carries out in anhydrous conditions.
Experimental analysis:
1, the high temperature resistance detection of stabilizer
The similar stabilizer that the embodiment 1-4 organic foam stabilizer prepared and market are bought, is put into high temperature furnace, then
Control temperature is started to warm up from 100 DEG C, is opened after every 5 DEG C of the raising of temperature and is observed cloth situation, when cloth changes colour
The temperature of discoloration is recorded, this temperature is exactly the temperature that cloth is able to bear, and test observations are as shown in the table:
As seen from the above table, its heat-resisting ability of organic foam stabilizer prepared by the present invention is than similar stabilizer that market is bought
Heat-resisting ability is stronger, and intensity has been more than 40% or more, therefore it is with good high-temperature resistant result.
2, the flame retardant property detection of stabilizer
The similar stabilizer that the embodiment 1-4 organic foam stabilizer prepared and market are bought, carries out flame retardant property test,
It light 5-10 seconds with open fire, then withdraws open fire, observes its combustion case, test observations such as following table institute
Show:
As seen from the above table, organic foam stabilizer fire retardancy prepared by the present invention is more fire-retardant than the similar stabilizer that market is bought
Ability is stronger, and combustion phenomena would not occurs in it after open fire leaves.
Finally, it is stated that preferred embodiment above is only used to illustrate the technical scheme of the present invention rather than limits, although logical
It crosses above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be
Various changes are made to it in form and in details, without departing from defined by claims of the present invention.
Claims (8)
1. a kind of preparation method of the organic foam stabilizer with flame retardant property, it is characterised in that described one kind has resistance
Fire the composition of the organic foam stabilizer of performance are as follows: dimethyldichlorosilane that mass fraction is 20-30 parts, 40-60 parts
Xylyl dichlorosilane, 60-100 parts of active silicic acid sodium, 2-4 parts of acid-base modifier, 1-2 parts of initiator, 120-150
The mixed solvent, 4-5 parts of catalyst of part.
2. a kind of preparation method of organic foam stabilizer with flame retardant property according to claim 1, feature
Be, a kind of organic foam stabilizer with flame retardant property the preparation method comprises the following steps: temperature of reaction kettle is maintained
65-75 DEG C, mechanical agitator revolving speed is 200-300rpm, and 120-150 parts of mixed solvent, constant temperature 1-2 are added into reaction kettle
After hour, 60-100 parts of active silicic acid sodium, 2-4 parts of acid-base modifier, 40-60 parts of xylyl dichlorosilane are added
In reaction kettle, the speed with 1-2s/ drop of 20-30 parts of dimethyldichlorosilane is added dropwise on one side, in addition a constant pressure
1-2 parts of initiator is added dropwise in buret with the speed of 5-10s/ drop, by 4-5 parts of catalyst with 3- after being added dropwise completely
The speed of 5s/ drop is added dropwise, and after being added dropwise completely, keeps reacting 1-2 hours under this condition, then temperature is increased 2-5 DEG C, instead
It answers 1-2 hours, is spray-dried the substance after fully reacting, drying temperature is controlled at 50-80 DEG C, is obtained after removing solvent
To substance be added distilled water in impregnates 5-10 hours, flushing 2-3 times after, obtained object is dried, is obtained after drying
Substance is exactly the organic foam stabilizer with flame retardant property.
3. a kind of preparation method of organic foam stabilizer with flame retardant property according to claim 1, feature
It is, the active silicic acid sodium are as follows: 100-120 parts of sodium metasilicate is added in a kettle, raises the temperature to 40-60 DEG C,
4-5 parts of sodium citrate, 1-2 parts of lauric acid, 0.5-1 parts of stearic acid is added, reaction is cooled to room temperature to obtain after 2-3 hours
Substance, which is exactly active silicic acid sodium.
4. a kind of preparation method of organic foam stabilizer with flame retardant property according to claim 1, feature
Be, the initiator are as follows: by 1-2 parts, substance that 2-5 parts of organotin is obtained after mixing, the substance is just
It is initiator.
5. a kind of preparation method of organic foam stabilizer with flame retardant property according to claim 1, feature
It is, the acid-base modifier are as follows: 1-2 parts of sodium bicarbonate, 3-5 parts of sodium carbonate, 1-2 parts of nano-lotus leaf is hydrophobic
Agent, 1-2 parts of stearic acid, 1-2 parts of silane coupling agent are added in reaction kettle, are reacted, have been reacted under the conditions of 30-40 DEG C
It is cooled to room temperature after complete, the substance obtained after product is crushed, the substance is exactly acid-base modifier.
6. a kind of preparation method of organic foam stabilizer with flame retardant property according to claim 1, feature
It is, the mixed solvent are as follows: the substance for being obtained the DMF of 10-20:4-5 and hexamethylene after mixing, the substance
It is exactly mixed solvent.
7. a kind of preparation method of organic foam stabilizer with flame retardant property according to claim 1, feature
It is, the catalyst are as follows: be dissolved in 1-2 parts of butyl lithium in 20-30 parts of hexamethylene, the solution being configured to, the object
Matter is exactly catalyst.
8. a kind of preparation method of organic foam stabilizer with flame retardant property according to claim 1, feature
It is, the reaction condition in the claim 2 are as follows: entire reaction all carries out in anhydrous conditions.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112191272A (en) * | 2020-09-29 | 2021-01-08 | 苏州思德新材料科技有限公司 | Organosilicon foam catalyst and preparation method thereof |
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