CN104292796A - Application of zinc isoocatanoate in reduction on agglomeration of white carbon black, white carbon black dispersing agent containing zinc isoocatanoate and preparation method thereof - Google Patents
Application of zinc isoocatanoate in reduction on agglomeration of white carbon black, white carbon black dispersing agent containing zinc isoocatanoate and preparation method thereof Download PDFInfo
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Abstract
The invention provides application of zinc isoocatanoate in reduction on agglomeration of white carbon black. According to research, the inventor discovers that the polarity of a silanol group on the surface of white carbon black can be reduced by zinc isoocatanoate so as to play a role in dispersing white carbon black. Under the support of the function, zinc isoocatanoate can be used in the application field of multiple white carbon blacks. The invention also provides a white carbon black dispersing agent containing zinc isoocatanoate and a preparation method thereof. The method is simple, free of pollution, energy-saving and environment-friendly; the obtained dispersing agent has functions of physical dispersion and chemical dispersion, and is suitable for dispersing sizing materials with high filling amount of white carbon black, so that the dispersibility of the white carbon black can be improved, the processing performance of the sizing material also can be improved, the mixing time is shortened, the smoothness and dispersion uniformity of the sizing material is increased, the flowability of the sizing material in the processing and mixing stage is increased, and the Mooney viscosity is reduced; moreover, the white carbon black dispersing agent has a strengthening effect, and the mechanical property of vulcanized rubber is improved.
Description
Technical field
The present invention relates to a kind of rubber White carbon black dispersant and preparation method thereof, belong to technical field of fine.
Background technology
In order to improve the physical strength of tire, wear resistance and anti-slippery, need in rubber, add a large amount of packing strengthening agent white carbon blacks.Because white carbon black surface exists a large amount of silicone hydroxyl, these groups easily assemble conglomeration, are difficult to dispersed in tyre production process, and the mooney viscosity of rubber unvulcanizate easily rebounds, thus affect mechanical mechanics property.So, the technology type of White carbon black dispersant or promoting agent is added when compounding rubber, to the chemical property improving white carbon black surface silanol groups, improve white carbon black surfactivity, realize good distribution in rubber, and then improve or improve compound physical and chemical property has obtained effect very significantly.
At present, the processing aid that white carbon black disperses in rubber generally has three types: alcohol and alcamines promoting agent, zinc soap class dispersion agent and silane coupling agent.Alcohol and alcamines promoting agent when compounding rubber usually adsorb by the polarity silanol base on white carbon black surface, the process of absorption, be exactly white carbon black silanol based polar oneself shielding process, make the curability of sizing material interference-free.The mechanism of action of zinc soap class dispersion agent utilizes hydrionic activity on white carbon black surface silanol groups exactly, and there is cation replacement effect with it, and then reduce the polarity on white carbon black surface, control white carbon black ion and unite, reduce sizing material mooney viscosity, realize processing characteristics and improve.But this kind of dispersion agent is little to the physical and chemical performance effect improving cross-linked rubber.Silane coupling agent not only improves silica compound processing characteristics, makes the cross-linked rubber physical and chemical performance of white carbon black filler gum also obtain larger raising and improvement simultaneously.But coupling agent does not thoroughly solve all problems of application, and can produce a large amount of high salt organic waste waters in silane coupling agent production process, and environmental pollution is serious, and price is relatively expensive.
Summary of the invention
The object of this invention is to provide a kind of isocaprylic acid zinc and reduce the application in white carbon black reunion.
Another object of the present invention is to provide a kind of White carbon black dispersant, and this dispersion agent can make the white carbon black of high-content dispersing property in sizing material excellent.
Another object of the present invention is to provide the preparation method of this White carbon black dispersant, and the method technique is simple, pollution-free, products obtained therefrom excellent property.
The concrete technical scheme that the present invention adopts is as follows:
Contriver is found by research, and isocaprylic acid zinc can reduce the polarity of white carbon black surface silanol groups, isocaprylic acid zinc is added the reunion that can well prevent white carbon black in white carbon black, plays the effect of dispersion white carbon black.Under the support of this effect, isocaprylic acid zinc can be used in the Application Areas of multiple white carbon black, for disperseing white carbon black, prevents it from reuniting, and such as, in the rubber item field containing white carbon black, plays the effect of White carbon black dispersant.In addition, isocaprylic acid zinc also can be re-dubbed the White carbon black dispersant with multiple efficacies with other compositions, has both played the effect of dispersion white carbon black, can improve again some performances of sizing material.
Be below the dispersion effect experiment of the sizing material adding isocaprylic acid zinc dispersion white carbon black and do not add isocaprylic acid, method is as follows:
1, test sizing compound formula is (weight part): SCR#100 part, ZnO 5 parts, white carbon black 175GR 60 parts, Si-69 4 parts, promotor 3.6 parts, Sulfur 1.6 parts, 0 part, isocaprylic acid zinc or 3 parts.
2, during test, not add the sizing material of isocaprylic acid zinc as blank, checking adds the dispersiveness of the sizing material of 3 parts of isocaprylic acid zinc.Because isocaprylic acid zinc is thickness state, for the ease of adding, add again in sizing material after first isocaprylic acid zinc and part white carbon black being blended together powder in advance, method is as follows: isocaprylic acid zinc is heated to 100 DEG C, then according to the mass ratio of 1:1, the isocaprylic acid zinc of white carbon black 175GR and heating is uniformly mixed in miniature kneader, pours out for subsequent use after mixing.
3, by two parts of sizing material sections of preparation, with sem observation slice surface white carbon black dispersion effect, the scanning electron microscopic picture not adding the sizing material of isocaprylic acid zinc as shown in Figure 1, adds the scanning electron microscopic picture of the sizing material of isocaprylic acid zinc as shown in Figure 2.As can be seen from the picture, isocaprylic acid zinc has the good action of dispersion white carbon black, can use it for dispersion white carbon black or reduce white carbon black and reunite.
The invention provides a kind of White carbon black dispersant, its composition comprises isocaprylic acid zinc.
In above-mentioned White carbon black dispersant, the content of isocaprylic acid zinc is 1-100wt%, preferred 20-99wt%, further preferred 40-70wt%, most preferably 55.3-66.7wt%.
In above-mentioned White carbon black dispersant, also comprise polyoxyethylene glycol, organic filler and inorganic filler components, with some performances making White carbon black dispersant except disperseing the effect of white carbon black can also improve sizing material.Each ingredients weight parts content is as follows:
Isocaprylic acid zinc 80-100 part
Polyoxyethylene glycol 30-50 part
Organic filler 1-10 part
Mineral filler 10-20 part.
In above-mentioned White carbon black dispersant, each component preferred content following (weight part):
90 parts, isocaprylic acid zinc
Polyoxyethylene glycol 40 parts
Organic filler 5 parts
Mineral filler 15 parts.
In above-mentioned White carbon black dispersant, the molecular weight of described polyoxyethylene glycol is 200-20000, such as, in PEG200, PEG400, PEG2000, PEG4000, PEG6000, PEG10000 and PEG20000 etc. one or more, are preferably at least one in PEG2000 and PEG4000.
In above-mentioned White carbon black dispersant, described organic filler is Wax-for preventing rubber and/or fatty acid ester, preferred fat acid esters.Wherein, described Wax-for preventing rubber is the Wax-for preventing rubber that market is sold.Described fatty acid ester can select pentaerythritol stearate, PETO, glyceryl monostearate, glycerin fatty acid ester, fatty acid methyl ester etc.
In above-mentioned White carbon black dispersant, described mineral filler is at least one in potter's clay, talcum powder, mica powder, polynite and calcium carbonate, is preferably calcium carbonate.
The preparation method of above-mentioned White carbon black dispersant, comprise the following steps: by isocaprylic acid zinc, polyoxyethylene glycol and organic filler melt blending at 80 ~ 100 DEG C, then add mineral filler to stir, obtain homogeneous thick liquid mixture, mixture is cooled film-making or melt pelletization, obtain White carbon black dispersant.
In above-mentioned preparation method, the time of melt blending is 2-3h.
The present invention is on the basis of isocaprylic acid zinc, after further research and preferably, obtain above-mentioned White carbon black dispersant composition, at least containing isocaprylic acid zinc, polyoxyethylene glycol, organic filler and mineral filler four kinds of compositions in said composition, isocaprylic acid zinc and polyoxyethylene glycol have the effect of physical dispersion and chemical dispersion simultaneously, be applicable to the dispersion of high white carbon black loading level sizing material, not only can improve the dispersiveness of white carbon black, processing characteristics and the mechanical property of sizing material can also be improved.Organic filler and mineral filler have the effect improving properties of rubber, and the processing characteristics of silica compound, safety performance and physical and mechanical properties are further enhanced.Through a large amount of experiment screenings, above-mentioned four kinds of compositions are carried out composite according to specific consumption, each composition is made to work in coordination with onset, when gained dispersion agent makes white carbon black content is higher in rubber, dispersing property is also excellent, also makes the processing characteristics of silica compound, safety performance and physical and mechanical properties all be improved adding of dispersion agent in addition.
White carbon black dispersant composition of the present invention is containing the organic long-chain compound being rich in hydroxyl group absorption body, the hydroxyl of dialogue carbon blacksurface carries out adsorbing or reacting, not only with the silanol base on white carbon black surface, there is very strong chemical reaction ability, but also it is based polar to reduce white carbon black silanol by physisorption, reacts with rubber matrix simultaneously and form a kind of novel cross-linked network and promote that rubber is formed firmly in conjunction with glue with white carbon black.
White carbon black dispersant of the present invention can be suitable for all kinds of rubber item, such as the rubber item etc. of styrene-butadiene rubber(SBR) goods, natural rubber products and multiple rubber mix.It can make white carbon black loading level account for the favorable dispersity of rubber 70wt% or following sizing material.
The present invention has the following advantages:
1, the composition such as isocaprylic acid zinc, polyoxyethylene glycol in dispersion agent, economic environmental protection, pollution-free, there is the effect of physical dispersion and chemical dispersion simultaneously, be applicable to the dispersion of high white carbon black loading level sizing material, not only can improve the dispersiveness of white carbon black, the processing characteristics of sizing material can also be improved, shorten mixing time, strengthen the slipperiness of sizing material, dispersion homogeneity, improve the mobility of sizing material in processing mix stage, reduce mooney viscosity, and there is reinforcing effect, improve the mechanical property of cross-linked rubber.
2, the organic filler in dispersion agent has physics plasticising, anti-aging function to sizing material, improves processing characteristics and the safety performance of sizing material.
3, the interpolation of White carbon black dispersant of the present invention can make sizing material in process safety performance, physical and mechanical properties and vulcanization rate etc., be obtained for raising and improve.Mixing process for the various rubber such as natural rubber and synthetic rubber can improve the dispersiveness of white carbon black in sizing material, and significantly can reduce the viscosity of sizing material, improve mobility and the rate of extrusion of sizing material, thus reduce the energy expenditure of tire or goods processing, improve melting efficiency, also contribute to the demoulding of vulcanizate, keep mould clean.
4, simple and direct, pollution-free, the energy-conserving and environment-protective of dispersant preparation method of the present invention, meet the policy requirements of national green chemical industry, cleanly production.
Accompanying drawing explanation
fig. 1 isdo not add the scanning electron microscopic picture of the sizing material of isocaprylic acid zinc.
Fig. 2 is the scanning electron microscopic picture of the sizing material adding isocaprylic acid zinc.
Fig. 3 is the watt consumption figure of different sample.
Fig. 4 is the extruded velocity figure of different sample.
Fig. 5 is the Mooney viscosity value figure of different sample.
embodiment
According to specific embodiment, the present invention will be further elaborated below, and if no special instructions, each Ingredient Amount is weight part.
The present invention's polyoxyethylene glycol used, Wax-for preventing rubber, fatty acid ester are prior art, market can be buied, such as polyoxyethylene glycol can purchased from Jinan Lu Ying Chemical Co., Ltd., Wax-for preventing rubber can purchased from Dalian Petrochemical Branch, China Petroleum and Natural Gas Co., Ltd., and fatty acid ester can purchased from Liaocheng Rui Jie Chemical Co., Ltd..
Following embodiment isocaprylic acid zinc used can be bought from market; also can prepare by the following method; step is: with in condenser, water trap, whipping appts and heatable reaction vessel, add zinc oxide, solvent, logical nitrogen protection; steam heating; be warming up to 80 DEG C of unlatching stirrings and at the uniform velocity drip isocaprylic acid in reactor, adding rear maintenance reactor temperature is 80 DEG C ~ 120 DEG C, and the water that reaction generates is separated by water trap; promote that reaction is carried out, reaction about needs 1 ~ 2h.Lower the temperature when not having water to generate, underpressure distillation, remaining liq is isocaprylic acid zinc.The mol ratio of zinc oxide and isocaprylic acid is 1:2.05-2.15.
exemplify the embodiment of several preferred dispersants formula of the present invention below, to be further described the present invention.
embodiment 1
The formula of White carbon black dispersant of the present invention is: 90 parts, isocaprylic acid zinc, Macrogol 2000 40 parts, fatty acid ester 5 parts, 15 parts, calcium carbonate.
Preparation method is: by isocaprylic acid zinc, Macrogol 2000 and Wax-for preventing rubber 80 DEG C stir melt blendings, at the temperature of 90 DEG C, then add calcium carbonate be uniformly mixed, pour out cooling film-making or fusing and pelleting obtain White carbon black dispersant of the present invention.
embodiment 2
White carbon black dispersant formula of the present invention is: 90 parts, isocaprylic acid zinc, Macrogol 4000 40 parts, fatty acid ester 5 parts, 15 parts, calcium carbonate.Preparation method is with embodiment 1.
embodiment 3
White carbon black dispersant formula of the present invention is: 90 parts, isocaprylic acid zinc, polyethylene glycol 6000 40 parts, fatty acid ester 5 parts, 15 parts, calcium carbonate.Preparation method is with embodiment 1.
embodiment 4
White carbon black dispersant formula of the present invention is: 90 parts, isocaprylic acid zinc, Macrogol 2000 40 parts, Wax-for preventing rubber 5 parts, 15 parts, calcium carbonate.Preparation method is with embodiment 1.
embodiment 5
White carbon black dispersant formula of the present invention is: 90 parts, isocaprylic acid zinc, Macrogol 2000 20 parts, Macrogol 200 20 parts, Wax-for preventing rubber 3 parts, fatty acid ester 2 parts, 15 parts, potter's clay.Preparation method is with embodiment 1.
embodiment 6
White carbon black dispersant formula of the present invention is: 90 parts, isocaprylic acid zinc, Macrogol 2000 40 parts, Wax-for preventing rubber 5 parts, talcum powder 15 parts.Preparation method is with embodiment 1.
embodiment 7
White carbon black dispersant formula of the present invention is: 80 parts, isocaprylic acid zinc, Macrogol 2000 50 parts, Wax-for preventing rubber 2 parts, fatty acid ester 3 parts, 5 parts, potter's clay, 10 parts, calcium carbonate.Preparation method is with embodiment 1.
embodiment 8
White carbon black dispersant formula of the present invention is: 100 parts, isocaprylic acid zinc, Macrogol 2000 30 parts, fatty acid ester 5 parts, mica powder 5 parts, polynite 5 parts, 5 parts, calcium carbonate.Preparation method is with embodiment 1.
embodiment 9
White carbon black dispersant formula of the present invention is: 90 parts, isocaprylic acid zinc, poly(oxyethylene glycol) 400 15 parts, PEG 20000 35 parts, fatty acid ester 1 part, mica powder 20 parts.Preparation method is with embodiment 1.
embodiment 10
White carbon black dispersant formula of the present invention is: 90 parts, isocaprylic acid zinc, Macrogol 200 20 parts, PEG20000 10 parts, fatty acid ester 10 parts, polynite 1 part, talcum powder 9 parts.Preparation method is with embodiment 1.
above-mentioned obtained dispersion agent is respectively used in SBR sizing material, to prove beneficial effect of the present invention.
one, sizing material processing characteristics, safety performance and physical and mechanical properties experiment
1, SBR sizing compound formula (weight part): SBR1502 70 parts, BR9000 30 parts, ZnO 5 parts, white carbon black 175GR 70 parts, carbon black 6 parts, promotor 3.6 parts, Sulfur 1.6 parts, White carbon black dispersant 3 parts.
2, calendering process:
One section of mixing employing 1L Banbury mixer, initial temperature 100 DEG C, revolution 60r/min.
Two-stage mixing, initial temperature 100 DEG C, revolution 60r/min, adds one section of rubber master batch to glue temperature 130 DEG C of binder removals.
Mill sulphurization, promotor bottom sheet are parked to be measured.
3, performance test
White carbon black dispersant embodiment 1 to embodiment 10 made makes 10 parts of SBR sizing materials according to above-mentioned formula respectively, and preparation is simultaneously a does not add the sizing material of White carbon black dispersant in contrast, and each performance of gained sizing material is as shown in following table 1 and table 2:
As can be seen from the above table, compared with the sizing material not adding White carbon black dispersant, adding of each dispersion agent of the present invention makes the processing characteristics of sizing material, safety performance and physical and mechanical properties all be improved and improve, and wherein the dispersing agent performance of embodiment 1-3 is best.
two, the safe White carbon black dispersant HST Comparison study test of White carbon black dispersant of the present invention and Yanggu China
1, according to the formula of above-mentioned sizing material, prepare 3 parts of SBR sizing materials, a copy of it dispersion agent used is the White carbon black dispersant of embodiment 1, and second part of dispersion agent used is the safe White carbon black dispersant HST of Yanggu China, and the 3rd part of sizing material does not add dispersion agent, as blank.
2, the performance test of gained sizing material is as follows, to prove the effect of White carbon black dispersant prepared by the present invention.
2.1, processing characteristics test experiments
Measuring column plug capillary rheometer method according to HG/T14300-2012(rubber rheological property), test above-mentioned 3 sample sizing material processing characteristicies, each sample watt consumption, extruded velocity, mooney viscosity test result are shown in Fig. 3-5.
As can be seen from the figure, the present invention and HST White carbon black dispersant can play the effect reducing sizing material mooney viscosity, power consumption of polymer processing and improve rate of extrusion, but White carbon black dispersant effect of the present invention is more remarkable.
2.2, vulcanization characteristics test experiments
Embodiment 1 White carbon black dispersant and the impact of safe White carbon black dispersant HST on SBR rubber vulcanization characteristic of Yanggu China as shown in table 3:
Can be found out by table 3, White carbon black dispersant of the present invention has good effect in the processing safety improving sizing material and vulcanization rate, and comparatively the safe HST of Yanggu China is better for effect.
2.3, quantitative measurement experiment
Mensuration according to GB GB/T329-2008(vulcanized rubber or thermoplastic elastomer tear strength), the mensuration of GB GB/T328-2009(vulcanized rubber or thermoplastic elastomer tensile stress-strain performance) and GB GB/T3512-2001(rubber test method), physical and mechanical properties test is carried out to above-mentioned 3 samples, the results are shown in Table 4.
As can be seen from Table 4, the White carbon black dispersant that embodiment 1 is made is added in SBR sizing material, tensile strength, stress at definite elongation and tear strength there is lifting in various degree, illustrate that this patent product facilitates white carbon black dispersion of particles, the reinforcement cross-linked network of cross-linked rubber, reduces permanent compression set, and can improve its basic physical and mechanical properties, compared with the safe HST of Yanggu China, effect slightly well.
2.4, dynamic properties test experiments
Mensuration according to GB/T1687-93(vulcanized rubber temperature rise and wear-resisting fatigue property in angular test), carry out the test of cross-linked rubber dynamic properties to above-mentioned 3 samples, test result sees the following form 5.
As can be seen from Table 5, two kinds of White carbon black dispersant can improve the wet-sliding resistant performance of tire, reduce the rolling resistance of tire, but effect of the present invention comparatively the safe HST of Yanggu China is better.
Claims (10)
1. isocaprylic acid zinc is reducing the application in white carbon black reunion.
2. a White carbon black dispersant, is characterized in that: comprise isocaprylic acid zinc.
3. White carbon black dispersant according to claim 2, is characterized in that: the content of isocaprylic acid zinc is 1-100wt%, preferred 20-99wt%, further preferred 40-70wt%, most preferably 55.3-66.7wt%.
4. White carbon black dispersant according to claim 2, is characterized in that: also comprise polyoxyethylene glycol, organic filler and mineral filler, and each ingredients weight parts content is as follows:
Isocaprylic acid zinc 80-100 part
Polyoxyethylene glycol 30-50 part
Organic filler 1-10 part
Mineral filler 10-20 part.
5. White carbon black dispersant according to claim 4, is characterized in that, each ingredients weight parts content is as follows:
90 parts, isocaprylic acid zinc
Polyoxyethylene glycol 40 parts
Organic filler 5 parts
Mineral filler 15 parts.
6. White carbon black dispersant according to claim 4, is characterized in that: the molecular weight of described polyoxyethylene glycol is 200-20000; Described organic filler is Wax-for preventing rubber and/or fatty acid ester; Described mineral filler is at least one in potter's clay, talcum powder, mica powder, polynite and calcium carbonate.
7. White carbon black dispersant according to claim 6, is characterized in that: the molecular weight of described polyoxyethylene glycol is at least one in 2000 and 4000; Described organic filler is fatty acid ester; Described mineral filler is calcium carbonate.
8. the White carbon black dispersant according to claim 6 or 7, is characterized in that: described fatty acid ester is pentaerythritol stearate, PETO, glyceryl monostearate, glycerin fatty acid ester or fatty acid methyl ester.
9. the preparation method of a White carbon black dispersant, it is characterized in that comprising the following steps: by isocaprylic acid zinc, polyoxyethylene glycol and organic filler melt blending at 80 ~ 100 DEG C, then add mineral filler to stir, obtain homogeneous thick liquid mixture, mixture is cooled film-making or melt pelletization, obtain White carbon black dispersant.
10. preparation method according to claim 9, is characterized in that: the time of melt blending is 2-3h.
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| CN201410519422.XA CN104292796A (en) | 2014-09-30 | 2014-09-30 | Application of zinc isoocatanoate in reduction on agglomeration of white carbon black, white carbon black dispersing agent containing zinc isoocatanoate and preparation method thereof |
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| CN104829871A (en) * | 2015-04-16 | 2015-08-12 | 宜兴市聚金信化工有限公司 | White carbon black dispersing agent and preparation method thereof |
| CN109694499A (en) * | 2018-12-04 | 2019-04-30 | 彤程化学（中国）有限公司 | Reinforced filling functional additive and its application in white carbon black filling SSBR sizing material |
| CN111454561A (en) * | 2020-04-29 | 2020-07-28 | 无锡市东材科技有限公司 | High-performance white carbon black dispersing agent and preparation method thereof |
| CN114714533A (en) * | 2022-03-07 | 2022-07-08 | 中策橡胶集团股份有限公司 | Characterization method of mixing process difference of low rolling resistance rubber composition and mixing method |
| CN115260614A (en) * | 2022-07-15 | 2022-11-01 | 山东玲珑轮胎股份有限公司 | High-tear-resistance and high-wear-resistance all-steel tire tread rubber and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104829871A (en) * | 2015-04-16 | 2015-08-12 | 宜兴市聚金信化工有限公司 | White carbon black dispersing agent and preparation method thereof |
| CN104829871B (en) * | 2015-04-16 | 2017-11-03 | 宜兴市聚金信化工有限公司 | A kind of White carbon black dispersant and preparation method thereof |
| CN109694499A (en) * | 2018-12-04 | 2019-04-30 | 彤程化学（中国）有限公司 | Reinforced filling functional additive and its application in white carbon black filling SSBR sizing material |
| CN111454561A (en) * | 2020-04-29 | 2020-07-28 | 无锡市东材科技有限公司 | High-performance white carbon black dispersing agent and preparation method thereof |
| CN114714533A (en) * | 2022-03-07 | 2022-07-08 | 中策橡胶集团股份有限公司 | Characterization method of mixing process difference of low rolling resistance rubber composition and mixing method |
| CN114714533B (en) * | 2022-03-07 | 2024-06-25 | 中策橡胶集团股份有限公司 | Characterization method and mixing method of mixing process difference of low-rolling-resistance rubber composition |
| CN115260614A (en) * | 2022-07-15 | 2022-11-01 | 山东玲珑轮胎股份有限公司 | High-tear-resistance and high-wear-resistance all-steel tire tread rubber and preparation method and application thereof |
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