CN106832113B - A kind of temperature-resistant anti-salt flooding polymers containing nano particle - Google Patents
A kind of temperature-resistant anti-salt flooding polymers containing nano particle Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
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Abstract
The invention discloses a kind of temperature-resistant anti-salt flooding polymers containing nano particle.It is prepared using the method included the following steps: (1) accessing amino in nano-silica surface, obtain modified manometer silicon dioxide;(2) modified manometer silicon dioxide, water-soluble monomer and water are mixed, the pH to 4~8 for adjusting mixed system is completely dispersed modified manometer silicon dioxide in water;Disodium ethylene diamine tetraacetate, ferrous sulfate and tetramethylethylenediamine is added into the mixed system after adjusting pH value, azo-bis-isobutyrate hydrochloride, ammonium persulfate and hydrogen peroxide is then added, carries out reaction I in a nitrogen atmosphere, carries out reaction II after heating;The pH for the reaction product for reacting II is adjusted to 8~9 and carries out constant temperature aging, is crushed after drying.The present invention utilizes the dispersion performance and high temperature stability performance of modified manometer silicon dioxide itself, by the interaction between polymer, improves the rigidity of polymer molecule, forms network structure between polymer molecule, generates the performances such as excellent temperature-resistant anti-salt is anti-aging.
Description
Technical field
The present invention relates to a kind of temperature-resistant anti-salt flooding polymers containing nano particle belong to water soluble polymer synthesis skill
Art field.
Background technique
Chemical flooding technology is one of the technical measures that oil recovery factor is improved in China, and wherein water-soluble polymer is real
One of the key chemical agent for applying chemical flooding is expanded the swept volume of displacing fluid by the tackifying of polymer, may be implemented substantially
Degree improves the purpose of oil recovery factor.Currently, polymer displacement of reservoir oil, binary combination flooding (polymer-surfactant), tri compound
The tertiary oil recovery technologies such as the displacement of reservoir oil (alkali-polymer-surfactant) obtain in the east main force such as triumph, grand celebration, Liaohe River oil field
It is widely applied, and achieves significant oil increasing precipitation effect and good economic and social benefits.But with chemical displacement of reservoir oil technology
It is constantly promoted and applied in oil field, implements the reservoir condition of chemical flooding worse and worse, the reservoir reserve of low temperature low mineralization is more next
Fewer, high temperature and high salt oil deposit will become the battle position of chemical displacement of reservoir oil research of technique and popularization and application, but drive used at present from now on
The shortcomings that oily chemical agent generally existing not heatproof not salt resistance, chemical displacement of reservoir oil technology has been seriously affected in high temperature and high salt oil deposit
Application effect has become and restricts the technical bottleneck that chemical flooding technology is promoted and applied in high temperature and high salt oil deposit.Therefore, it researchs and develops
Temperature-resistant anti-salt, efficient, stable Polymer Used For Oil Displacement product are extremely urgent.
From the point of view of the structure and performance of polymer, to maintain acrylamide copolymer under salting liquid and high temperature
Viscosity, the method that can be taken mainly have: (1) introducing the polymer chain with big steric hindrance on main polymer chain, mention
High polymer chain rigidity;(2) interaction between polymer molecular chain is improved, to maintain it under salting liquid and high temperature
Hydrodynamic volume prevents being greatly lowered for viscosity.However, crossing the introducing of multifunctional monomer, product on the one hand will increase
Cost, on the other hand, compared with acrylamide, often polymerization activity is poor for function monomer, thus will lead to the molecule of copolymer
Measure relatively low, thickening property is bad, this will improve the use concentration of product.
Chinese patent document CN 102181010A discloses a kind of preparation method of Heat Resistant and Salt Tolerant Polymer, preparation method
It is as follows: by anionic monomer, acrylic sodium sulfonate, cationic monomer, acrylate, alpha-olefin and acrylamide be dissolved in from
In sub- water, surfactant is added, adjusts under the conditions of pH value of solution is 9~10,30~60 DEG C and leads to nitrogen 30 minutes, over cure is added
Hydrochlorate initiator reacts 12h under the conditions of 30~60 DEG C of temperature, and with acetone precipitation, washing, vacuum drying obtains white powder
Polymer, resulting polymers can be used on enhancing oil recovery in polymer flooding.
Chinese patent document CN 103320111A discloses a kind of synthetic method of quadripolymer oil displacement agent, the displacement of reservoir oil
The function that agent is prepared by acrylamide (AM), acrylic acid (AA), n-vinyl pyrrolidone (NVP), ethylenediamine and maleic anhydride
The quadripolymer that monomer (YEML) is constituted.Its synthetic method is that YEML monomer obtained is first added in flask, add AM,
NVP, AA and NaOH lead to nitrogen 30min, initiator are then added, and continue logical 10~20min of nitrogen, at 30~60 DEG C of temperature
React 4~12h.It finally washed, crushed with dehydrated alcohol, drying obtained AM/AA/NVP/YEML quadripolymer, preparation gathers
Closing object can be used to improve oil recovery factor.
Above-mentioned patent realizes the promotion of polymer temperature-resistant anti-salt performance by introducing function monomer, in the process,
It often has the disadvantage that function monomer preparation process is cumbersome, there are the subsequent operations such as purification, increase product cost;With third
Acrylamide monomer is compared, and function monomer polymerization activity is poor, and polymer molecular weight is not high, in use process, the polymer that needs
Concentration is high;The introducing of hydrophobic type function monomer, interior salt form function monomer, reduces the solubility property of polymer, in use process,
The dissolution time of polymer increases, and insoluble matter ratio increases, and influences using and promoting for product.
Summary of the invention
The object of the present invention is to provide a kind of temperature-resistant anti-salt flooding polymers containing nano particle, the present invention is conventional third
On the basis of acrylamide polymer, introducing has the modified manometer silicon dioxide compared with strong interaction with polymer molecule, from
And it plays and improves the rigidity of polymer molecule, improve between the high-temperature stability of side group in polymer molecule, building polymer molecule
The effects of network.
A kind of temperature-resistant anti-salt flooding polymers containing nano particle provided by the invention, using the side included the following steps
Method is prepared:
(1) amino is accessed in nano-silica surface, obtains modified manometer silicon dioxide;
(2) modified manometer silicon dioxide, water-soluble monomer and water are mixed, adjusts the pH value of mixed system to 4~8
It is completely dispersed the modified manometer silicon dioxide in water;Ethylenediamine tetra-acetic acid is added into the mixed system after adjusting pH value
Then azo-bis-isobutyrate hydrochloride, ammonium persulfate and hydrogen peroxide is added in disodium, ferrous sulfate and tetramethylethylenediamine,
Reaction I is carried out under nitrogen atmosphere, carries out reaction II after heating;The pH value of the reaction product of the reaction II is adjusted to 8~9 simultaneously
Constant temperature aging is carried out, crushes after drying, the temperature-resistant anti-salt flooding polymers containing nano particle can be obtained.
Above-mentioned flooding polymers, in step (1), the nano silica is as a kind of general nano material, tool
Have size tunable, low manufacture cost, it is nontoxic, specific surface area is high many advantages, such as.The nano-silica surface is with a large amount of
Silicone hydroxyl, can by reaction its surface introduce amino, to prepare the modified manometer silicon dioxide of surface amination.With not
Modified nano silica is compared, and the modified manometer silicon dioxide surface can be cationized, and therefore, is had very excellent
Dispersion performance, under high temperature and alkaline environment, particle itself has better stability.
What the method used by nano-silica surface access amino can be known to the skilled person appoints
The method of what amination nano silica, includes but is not limited to the method included the following steps: by nano silica and band
There is the silane coupling agent of amino to be scattered in the mixed liquor of water and ethyl alcohol, carries out flowing back after system pH is adjusted to 7~9 anti-
It answers, the modified manometer silicon dioxide will can be obtained after reaction product filtering, drying.
Concentration of the nano silica in the mixed liquor can be 10~100gL-1, concretely 30~
60g·L-1, 40~50gL-1、40g·L-1Or 50gL-1。
The partial size of the nano silica can be 10~300nm, concretely 10~150nm, 80~100nm, 30~
50nm。
Concentration of the silane coupling agent with amino in the mixed liquor can be 5~50gL-1, concretely 18
~25gL-1、18g·L-1Or 25gL-1。
The silane coupling agent with amino can be aminopropyl triethoxysilane, 3- (2- aminoethyl amino) propyl three
Methoxy silane, 3- (2- aminoethyl amino) propyl-triethoxysilicane, [3- (2- aminoethyl amino) propyl] dimethoxy silicon
Alkane, (3- methylaminopropyl) trimethoxy silane, 3- aminopropyl dimethyl methoxy silane, 3- [2- (2- aminoethyl amino) second
Base amino] propyl trimethoxy silicane, any one of (3- aminopropyl) dimethylethoxysilane.
In the mixed liquor, the volume ratio of second alcohol and water is (8~11): 1, concretely 9:1.
The temperature of the back flow reaction can be 78~82 DEG C, and concretely 80 DEG C, the time can be 4~6 hours, concretely
4 hours.
Above-mentioned flooding polymers, in step (2), the water-soluble monomer, the modified manometer silicon dioxide and water
Weight ratio can be 1:(0.001~0.08): (0.5~15), concretely 1:(0.02~0.04): (2~3), 1:0.02:3,1:
0.04:3 or 1:0.02:2.
The water-soluble monomer can be at least one mixture of acrylamide and following monomer: ethenyl pyrrolidone
Ketone, sodium acrylate, 2- acrylamide-2-methylpro panesulfonic acid sodium, sodium vinyl sulfonate, sodium styrene sulfonate;The water solubility
Any one of monomer concretely following 1) -3):
1) mixture of acrylamide and 2- acrylamide-2-methylpro panesulfonic acid sodium;
2) mixture of acrylamide, 2- acrylamide-2-methylpro panesulfonic acid sodium and vinyl pyrrolidone;
3) mixture of acrylamide, sodium acrylate and vinyl pyrrolidone.
In the mixture, the mass percentage of the acrylamide can be 40%~95%, concretely 60%~
80%, 60% or 80%.
In step (2), the modified manometer silicon dioxide, water-soluble monomer is specifically adjusted in above-mentioned flooding polymers
The pH value for the mixed system being mixed to get with water is to 5.5~7.5,5.6~6.3,5.6 or 6.3.The dispersion is under agitation
It carries out.
Above-mentioned flooding polymers, in step (2), the quality of the disodium ethylene diamine tetraacetate can be the water-soluble mono
The 0.0002%~0.005% of the quality of body, concretely 0.002%~0.004%, 0.002% or 0.004%;
The quality of the ferrous sulfate can be the 0.00002%~0.0005% of water-soluble mono weight, concretely
0.0002%~0.0003%, 0.0002% or 0.0003%;
The quality of the tetramethylethylenediamine can be the 0.00005%~0.001% of water-soluble mono weight, concretely
0.0002%;
The quality of the azo-bis-isobutyrate hydrochloride can be the 0.002~0.02% of the water-soluble mono weight, tool
Body can be 0.006%;
The quality of the ammonium persulfate can be the 0.0001~0.001% of the water-soluble mono weight, concretely
0.0004%;
The quality of the hydrogen peroxide can be the 0.00001%~0.0005% of water-soluble mono weight, concretely
0.0003%~0.0004%, 0.0003% or 0.0004%.
Above-mentioned flooding polymers, in step (2), the disodium ethylene diamine tetraacetate, the ferrous sulfate and described four
The order of addition of methyl ethylenediamine is unrestricted, the azo-bis-isobutyrate hydrochloride, the ammonium persulfate and the peroxidating
The order of addition of hydrogen is unrestricted.
Above-mentioned flooding polymers, in step (2), the temperature of the reaction I can be within 10 DEG C, concretely 8~10
DEG C, 8 DEG C or 10 DEG C, the time can be 1~10 hour, concretely 1~5 hour, 2~4 hours, 2 hours or 4 hours.
Above-mentioned flooding polymers, in step (2), the temperature of the reaction II can be 50~80 DEG C, the time can for 0.5~
5 hours, concretely 1~3 hour, 1.5~3 hours, 1.5 hours or 3 hours.
The pH of the reaction product of the reaction II in step (2), can be specifically adjusted to 8.6 by above-mentioned flooding polymers
And carry out constant temperature aging.The temperature of the constant temperature aging is identical as the temperature of the reaction II, and the time is 1~3 hour, specifically may be used
It is 2 hours.
The present invention can be with using the modified manometer silicon dioxide itself with good dispersion performance and high temperature stability performance
Very strong hydrogen bond action is formed with the side group in polymer molecule, so as to form " organic and inorganic " composite construction, is improved poly-
The rigidity and high-temperature stability of adduct molecule;In addition, the cation on modified manometer silicon dioxide surface can and polymer molecule
Anion on chain forms very strong electrostatic interaction, so as to construct the network structure between polymer molecule, enhancing polymerization
The performances such as the temperature-resistant anti-salt of object is anti-aging.
The invention has the following beneficial effects:
(1) raw material used in the method for the present invention is easy to get, cheap, and preparation process is simple, easily operated.
(2) monomer reactivity selected by the method for the present invention is higher, and easily prepared high molecular weight products, thickening property is excellent,
Product dosage is small when use.
(3) the method for the present invention has good dispersion performance and high-temperature stability using modified manometer silicon dioxide itself
Can, stronger interaction between polymer by it can be improved the rigidity of polymer molecule, form good polymer
Intermolecular net structure, to generate the performances such as excellent temperature-resistant anti-salt is anti-aging.
(4) nano particle of the present invention itself has certain washing oil effect.
(5) product that the method for the present invention is prepared and other chemicals for EOR compatibilities are good.
(6) product that the method for the present invention is prepared uses safe, smaller to environmental hazard.
Above-mentioned various features show that the method for the present invention is suitble to industrial production, and are with a wide range of applications.
Detailed description of the invention
Fig. 1 is oil displacement experiment moisture content/recovery ratio and solution injected slurry volume relation curve of polymer in embodiment 1.
Specific embodiment
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
The present invention will be further described combined with specific embodiments below, but the scope of the present invention is not limited only to this.
Embodiment 1, temperature-resistant anti-salt flooding polymers of the preparation containing nano particle
The temperature-resistant anti-salt flooding polymers containing nano particle are prepared in accordance with the following steps:
(1) preparation of modified manometer silicon dioxide
Disperse water for nano silica and the silane coupling agent with amino: ethyl alcohol be 1:9 (v/v) system in,
Regulation system pH to 8, back flow reaction 4 hours, product filtering, drying obtained modified manometer silicon dioxide.Nanometer titanium dioxide used
The partial size of silicon is 80~100nm, concentration 50gL-1, the silane coupling agent with amino is aminopropyl triethoxysilane, dense
Degree is 18gL-1。
(2) preparation of the temperature-resistant anti-salt flooding polymers containing nano particle
By the above-mentioned modified manometer silicon dioxide being prepared of 1g, 30g acrylamide, 20g 2- acrylamido -2- first
Base propanesulfonate and 150g deionized water are added in the wolf bottle equipped with blender, logical nitrogen pipe and thermometer, temperature 8
DEG C, pH 6.3 is stirred and is passed through nitrogen to modified manometer silicon dioxide and is completely dispersed, and then sequentially adds 1mg ethylenediamine tetrem
Acid disodium, 0.1mg ferrous sulfate, 0.1mg tetramethylethylenediamine, 3mg azo-bis-isobutyrate hydrochloride, 0.2mg ammonium persulfate and
0.15mg hydrogen peroxide reacts 2 hours, then raises the temperature to 60 DEG C, reacts 1.5 hours, and NaOH solution is added by system pH
8.6 are adjusted to, constant temperature aging 2 hours (60 DEG C), it is poly- to obtain the temperature-resistant anti-salt displacement of reservoir oil containing nano particle for product is dry, crushing
Close object.
Embodiment 2, temperature-resistant anti-salt flooding polymers of the preparation containing nano particle
As described in Example 1, except that the partial size of the nano silica in step (1) is 30~50nm, concentration
For 45gL-1。
Embodiment 3, temperature-resistant anti-salt flooding polymers of the preparation containing nano particle
As described in Example 1, except that the silane coupling agent in step (1) with amino is N- aminoethyl-γ-ammonia
Propyl trimethoxy silicane, concentration 25gL-1。
Embodiment 4, temperature-resistant anti-salt flooding polymers of the preparation containing nano particle
As described in Example 1, except that the dosage of the modified manometer silicon dioxide in step (2) is 2g.
Embodiment 5, temperature-resistant anti-salt flooding polymers of the preparation containing nano particle
As described in Example 1, except that acrylamide is 40g, 2- acrylamido -2- methyl-prop in step (2)
Sodium sulfonate is 10g, deionized water 100g.
Embodiment 6, temperature-resistant anti-salt flooding polymers of the preparation containing nano particle
As described in Example 1, except that monomer is 30g acrylamide, 10g 2- acrylamido-in step (2)
2- methyl propane sulfonic acid sodium, 10g vinyl pyrrolidone.
Embodiment 7, temperature-resistant anti-salt flooding polymers of the preparation containing nano particle
As described in Example 1, except that monomer is 30g acrylamide, 10g sodium acrylate, 10g second in step (2)
Vinyl pyrrolidone.
Embodiment 8, temperature-resistant anti-salt flooding polymers of the preparation containing nano particle
As described in Example 1, except that disodium ethylene diamine tetraacetate is 2mg in step (2), ferrous sulfate is
0.15mg, hydrogen peroxide 0.2mg.
Embodiment 9, temperature-resistant anti-salt flooding polymers of the preparation containing nano particle
As described in Example 1, except that it is 4 hours, 60 DEG C that reaction pH, which is 5.6,10 DEG C of reaction time, in step (2)
Reaction is 3 hours.
Comparative example 1 prepares flooding polymers
As described in Example 1, except that modified manometer silicon dioxide is not added.
Comparative example 2, certain flooding polymers
Comparative example 2 is certain Oil Field flooding polymers (Tianjin Bo Hong petrochemical industry Co., Ltd, BHKY-3).
Embodiment and the evaluation of comparative example properties of product:
The polymer solution for being 0.2% with mineralized water prepared polymer concentration, with the gear of WARRING blender 1 stirring 20 seconds,
Under conditions of 90 DEG C, aging 90 days, shearing front and back, aging front and back polymer are tested with Brookfield DV3T type viscosimeter
The viscosity of solution, test temperature are 90 DEG C, and test revolving speed is 6r/min.The composition of mineralized water is as shown in table 1, and anti-shear performance is commented
The results are shown in Table 2 for valence, and high-temperature aging resisting Evaluation results are as shown in table 3.
Table 1, mineralized water composition
Table 2, anti-shear performance evaluation result
Table 3, high-temperature aging resisting Evaluation results
It carries out improving recovery ratio laboratory experiment using polymer prepared by embodiment 1, by polymer mineralized water obtained
It is configured to 0.2% polymer solution, which is injected into (fill out sand tube sectional area 4.91cm in one-dimensional sandpack column2, length
30cm) initial oil saturation is 75%, water drive to moisture content 98%, (crude oil used at 90 DEG C, shear rate 7.34s-1Condition
Lower viscosity is 61.5mPas) injection rate is 1mL/min, after injecting the aqueous solutions of polymers of 0.35PV, continues with water drive extremely
Moisture content reaches 98%, measures recovery ratio and improves 20.3%.Oil displacement experiment moisture content/the recovery ratio and solution of polymer are injected
The relation curve of volume is as shown in Figure 1.
Claims (7)
1. a kind of temperature-resistant anti-salt flooding polymers containing nano particle, it is characterised in that: it is using the side included the following steps
Method is prepared:
(1) amino is accessed in nano-silica surface, obtains modified manometer silicon dioxide;
(2) modified manometer silicon dioxide, water-soluble monomer and water are mixed, adjusting the pH value of mixed system to 4~8 makes institute
Modified manometer silicon dioxide is stated to be completely dispersed in water;Ethylenediamine tetra-acetic acid two is added into the mixed system after adjusting pH value
Then azo-bis-isobutyrate hydrochloride, ammonium persulfate and hydrogen peroxide is added, in nitrogen in sodium, ferrous sulfate and tetramethylethylenediamine
Reaction I is carried out under gas atmosphere, carries out reaction II after heating;The pH value of the reaction product of the reaction II is adjusted to 8~9 to go forward side by side
Row constant temperature aging, crushes after drying, and the temperature-resistant anti-salt flooding polymers containing nano particle can be obtained;
In step (2), the weight ratio of the water-soluble monomer, modified manometer silicon dioxide and water is 1:(0.001~0.08):
(0.5~15);
The water-soluble monomer is at least one mixture of acrylamide and following monomer: vinyl pyrrolidone, propylene
Sour sodium, 2- acrylamide-2-methylpro panesulfonic acid sodium, sodium vinyl sulfonate, sodium styrene sulfonate;It is described in the mixture
The mass percentage of acrylamide is 40%~95%.
2. flooding polymers according to claim 1, it is characterised in that: described in nano silica table in step (1)
Method used by face access amino, which comprises the following steps that, disperses nano silica and silane coupling agent with amino in
In the mixed liquor of water and ethyl alcohol, back flow reaction is carried out after system pH is adjusted to 7~9, will be after reaction product filtering, drying
The modified manometer silicon dioxide can be obtained.
3. flooding polymers according to claim 2, it is characterised in that: in step (1), the nano silica is in institute
Stating the concentration in mixed liquor is 10~100gL-1;The partial size of the nano silica is 10~300nm;
Concentration of the silane coupling agent with amino in the mixed liquor is 5~50gL-1;
The silane coupling agent with amino is aminopropyl triethoxysilane, 3- (2- aminoethyl amino) propyl trimethoxy
Silane, 3- (2- aminoethyl amino) propyl-triethoxysilicane, [3- (2- aminoethyl amino) propyl] dimethoxysilane, (3-
Methylaminopropyl) trimethoxy silane, 3- aminopropyl dimethyl methoxy silane, 3- [2- (2- aminoethyl amino) ethylamino]
Any one of propyl trimethoxy silicane, (3- aminopropyl) dimethylethoxysilane;
In the mixed liquor, the volume ratio of second alcohol and water is (8~11): 1;
The temperature of the back flow reaction is 78~82 DEG C, and the time is 4~6 hours.
4. flooding polymers according to any one of claim 1-3, it is characterised in that: in step (2), the ethylenediamine
The quality of tetraacethyl disodium is the 0.0002%~0.005% of the quality of the water-soluble monomer;
The quality of the ferrous sulfate is the 0.00002%~0.0005% of water-soluble mono weight;
The quality of the tetramethylethylenediamine is the 0.00005%~0.001% of water-soluble mono weight;
The quality of the azo-bis-isobutyrate hydrochloride is the 0.002~0.02% of the water-soluble mono weight;
The quality of the ammonium persulfate is the 0.0001~0.001% of the water-soluble mono weight;
The quality of the hydrogen peroxide is the 0.00001%~0.0005% of water-soluble mono weight.
5. flooding polymers according to any one of claim 1-3, it is characterised in that: in step (2), the reaction I
Temperature be 10 DEG C within, the time be 1~10 hour.
6. flooding polymers according to any one of claim 1-3, it is characterised in that: in step (2), the reaction II
Temperature be 50~80 DEG C, the time be 0.5~5 hour.
7. flooding polymers according to any one of claim 1-3, it is characterised in that: the temperature of the constant temperature aging with
The temperature of the reaction II is identical, and the time is 1~3 hour.
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CN117402299A (en) * | 2022-07-08 | 2024-01-16 | 中国石油天然气股份有限公司 | Micro-nano spherical modified silica acid liquid gelatinizer and preparation method and application thereof |
CN117645867B (en) * | 2024-01-30 | 2024-04-09 | 盘锦辽河油田华联实业集团有限公司 | Surfactant composition for improving recovery ratio and preparation method thereof |
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