CN110066433A - A kind of silane coupled agent addition agent mixed method being kneaded applied to wet process - Google Patents

A kind of silane coupled agent addition agent mixed method being kneaded applied to wet process Download PDF

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Publication number
CN110066433A
CN110066433A CN201910136834.8A CN201910136834A CN110066433A CN 110066433 A CN110066433 A CN 110066433A CN 201910136834 A CN201910136834 A CN 201910136834A CN 110066433 A CN110066433 A CN 110066433A
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CN
China
Prior art keywords
mixed
component
kneaded
agent
wet process
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Pending
Application number
CN201910136834.8A
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Chinese (zh)
Inventor
王正
刘坤
刘国
王曙光
巴孟晨
高可可
杨延松
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Kai Kai New Materials Co Ltd
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Kai Kai New Materials Co Ltd
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Priority to CN201910136834.8A priority Critical patent/CN110066433A/en
Publication of CN110066433A publication Critical patent/CN110066433A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
    • C08K3/36Silica
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/54Silicon-containing compounds
    • C08K5/541Silicon-containing compounds containing oxygen
    • C08K5/5425Silicon-containing compounds containing oxygen containing at least one C=C bond
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/003Additives being defined by their diameter
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/014Additives containing two or more different additives of the same subgroup in C08K

Abstract

The invention discloses a kind of silane coupled agent addition agent mixed methods being kneaded applied to wet process, including selecting solution polymerized butadiene styrene rubber solution, silane coupling agent, white carbon black mixing, stirring shear is added to be mixed by the way of mechanical stirring blending, make mixed liquor under high pressure to spray in first mixed pond in mixture, is condensed after mixed liquor is further dispersed by way of grinding.It will be transferred in heating belt type drying machine after the dehydration of the micelle of cohesion and desolventizing, heat drying obtains rubber master batch under vacuum.Invention significantly improves the uniformity coefficients of dispersion, shorten jitter time, are suitable for large-scale industrial production.

Description

A kind of silane coupled agent addition agent mixed method being kneaded applied to wet process
Technical field
The present invention relates to rubber materials, in particular to a kind of silane coupled agent addition agent mixing side being kneaded applied to wet process Method.
Background technique
Wet process mixing technology is proposed at first by the Cabot Co., Ltd in the U.S., refers to rubber also in Heveatex or rubber polymer When newborn, the fillers such as carbon black, white carbon black, montmorillonite are added thereto, dispersion is uniformly mixed by mechanical stirring, then by coprecipitated The method that rubber compound is made.By the performance study discovery to rubber product, wet process is kneaded, and there is filler to be uniformly dispersed, technique section Can, the advantages that product properties is good.
During the processing of rubber, mixing is one of most basic and most important machining process.It is being kneaded It requires various compounding agents to be dispersed in raw rubber in the process, to obtain preferable mechanical property, while guaranteeing the composition of sizing material With performance uniformity.Requirement to calendering process is that speed is fast, high production efficiency, low energy consumption.Calendering process is to glue stuff compounding There is decisive influence with the quality of finished product.
Solution polymerized butadiene styrene rubber is widely used in the fields such as tire, adhesive tape, sebific duct.It is filled out what solution polymerized butadiene styrene rubber wet process was kneaded In material, phyllosilicate composite material, form factor is than high, intensity is high, heat-resist, air-tightness compared with traditional gum filler It is good.During the preparation process, the selection of filler has the function of key, while the partial size of filler to the intrinsic performance of the rubber of formation It is also important influence factor with hybrid mode, the excessive filler of partial size is difficult to play reinforcing and modifying function well, instead It will affect the performance of rubber.The too small filler of partial size then easily causes reunion, poor dispersion.Due to presently used filler Bioblast diameter it is often smaller, large specific surface area is easily reunited, be difficult to so as to cause it is evenly dispersed, to limit it Reinforcing effect.It is mainly prepared by way of filler addition-stirring-dispersion-cohesion at present, wherein filler is in rubber Influence of the degree of scatter to final performance in solution is very big, and currently used mode has and will stir resulting mixture and pass through One nozzle sprays in the case where high pressure high shear, and above-mentioned ejecta is made to make mixed liquor in Guan Zhongyu by swan neck more than one Tube wall hits the dispersibility for increasing filler and additive, but the above method obtains and is suitable for small-scale experimental study, is producing greatly It is difficult to realize in amount production.There is presently no mature effective, suitable for large-scale industrial production preparation methods.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of silane coupled agent addition agent being kneaded applied to wet process is mixed Conjunction method.
The complete technical solution of the present invention includes:
A kind of silane coupled agent addition agent mixed method being kneaded applied to wet process, which comprises the steps of:
(1) solution polymerized butadiene styrene rubber solution, silane coupling agent are selected, white carbon black mixing the ratio of each component is solution polymerized butylbenzene Rubber solutions: silane coupling agent: white carbon black=1000:(6~8): (45~52);
(2) said mixture addition stirring shear is mixed by the way of mechanical stirring blending, stirring speed Degree is 1200rpm, and control whipping temp is at 45 DEG C, mixing time 3h;
(3) just mixed pond is added in the mixture of acquisition, which includes pond body, and two sides will mix by way of pumping Object extraction is closed to send to the nozzle in respective front, nozzle is located at pond body top, is oppositely arranged, and make mixed liquor under high pressure to spray, into The dispersion of one step, the nozzle are circumferential weld shape, spray mixed liquor with gap-like, and the angle between two nozzles is 120~160 °, Mixture after dispersion falls into just mixed pond, can carry out circulation dispersion.
(4) it is condensed after further being dispersed mixed liquor by way of grinding.By cohesion and the glue of desolventizing It is transferred to after grain dehydration in heating belt type drying machine, heat drying obtains rubber master batch under vacuum.
Silane coupling agent described in step (1) includes component A and B component, and wherein component A is vinyl triethoxyl silicon Alkane or vinyltrimethoxysilane, B component are vinyl three (beta-methoxy ethyoxyl) silane, the mass ratio of component A and B component For (1~2): 5.
White carbon black partial size described in step (1) is 30~80 μm.
The improvement of the present invention compared with the existing technology are as follows: selected reasonable rubber compounded mix, phyllosilicate nano Composite material, form factor is than high, intensity is high, heat-resist, air-tightness is good compared with traditional gum filler;White carbon black improves Anti-slippery, wearability and the rolling resistance of butadiene-styrene rubber.Reasonable partial size and additional amount have been selected, dispersibility and property are improved Can, selected silane coupling agent component is reasonable, significantly improves the glue-joint strength of various rubber, and removing reaches by force 7.95.Using To the mode of spray dispersion, the uniformity coefficient of dispersion is significantly improved, jitter time is shortened, it is raw to be suitable for large-scale industry It produces.The stirring shear of use can be achieved at the same time and stir at low speed and high speed shear, while realize lysate preparation and emulsification Process significantly improves production efficiency.
Detailed description of the invention
Pool structure schematic diagram is just mixed shown in Fig. 1 present invention.
In figure: 1- pond body, 2- conveyance conduit, 3- mixed liquor, 4- nozzle.
Specific embodiment
The present invention will be further described With reference to embodiment.
Embodiment 1:
Select 1000 parts of solution polymerized butadiene styrene rubber solution, 1 part of vinyltriethoxysilane, 5 parts of (beta-methoxy second of vinyl three Oxygroup) silane, 48 parts of granularities are that 60 μm of white carbon black is mixed, and it is total using mechanical stirring that stirring shear is added in mixture Mixed mode is mixed, mixing speed 1200rpm, and control whipping temp is at 45 DEG C, mixing time 3h;By the mixed of acquisition It closes object and just mixed pond is added, which includes pond body 1, and two sides are taken out by way of pumping, by mixture 3 by conveyance conduit 2 It fetches and delivers to the nozzle 4 in respective front, nozzle is located above pond body, is oppositely arranged, divides mixed liquor to spray, further under high pressure It dissipates, the nozzle is circumferential weld shape, sprays mixed liquor with gap-like, and injection pressure is 40MPa, and the angle between two nozzles is 160 °, the mixture after dispersing falls into just mixed pond, disperses 3h.After mixed liquor is further dispersed by way of grinding It is condensed.It will be transferred in heating belt type drying machine after the dehydration of the micelle of cohesion and desolventizing, under vacuum heat drying Obtain rubber master batch.The rear mixing such as stearic acid, anti-aging agent, promotor is added in above-mentioned resulting rubber master batch to vulcanize in mixer, Obtain vulcanizate.
Embodiment 2:
The solution polymerized butadiene styrene rubber solution of 1000 parts of selection, 2 parts of vinyltriethoxysilane, 4 parts of three (beta-methoxys of vinyl Ethyoxyl) silane, 50 parts of granularities are that 45 μm of white carbon black is mixed, and mixture is added stirring shear and uses mechanical stirring The mode of blending is mixed, mixing speed 1200rpm, and control whipping temp is at 45 DEG C, mixing time 3h;By acquisition Just mixed pond is added in mixture, which includes pond body, and two sides are sent mixture extraction to respective front by way of pumping Nozzle, nozzle is located above pond body, is oppositely arranged, and disperses mixed liquor to spray, further under high pressure, the nozzle is Circumferential weld shape, sprays mixed liquor with gap-like, and injection pressure is 60MPa, and the angle between two nozzles is 160 °, after dispersing Mixture falls into just mixed pond, disperses 3h.It is condensed after mixed liquor is further dispersed by way of grinding.It will cohesion And be transferred in heating belt type drying machine after the micelle dehydration of desolventizing, heat drying obtains rubber master batch under vacuum.It will be above-mentioned The rear mixing such as stearic acid, anti-aging agent, promotor is added in mixer and is vulcanized for resulting rubber master batch, obtains vulcanizate.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way, it is all according to the present invention Technical spirit any simple modification to the above embodiments, change and equivalent structural changes, still fall within skill of the present invention In the protection scope of art scheme.

Claims (3)

1. a kind of silane coupled agent addition agent mixed method being kneaded applied to wet process, which comprises the steps of:
(1) solution polymerized butadiene styrene rubber solution, silane coupling agent are selected, white carbon black mixing the ratio of each component is solution polymerized butadiene styrene rubber Solution: silane coupling agent: white carbon black=1000:(6~8): (45~52);
(2) said mixture addition stirring shear is mixed by the way of mechanical stirring blending, mixing speed is 1200rpm, control whipping temp is at 45 DEG C, mixing time 3h;
(3) just mixed pond is added in the mixture of acquisition, which includes pond body, and two sides are by way of pumping, by mixture Extraction is sent to the nozzle in respective front, and nozzle is located above pond body, is oppositely arranged, is made mixed liquor under high pressure to spray, further Dispersion, the nozzle are circumferential weld shape, spray mixed liquor with gap-like, and the angle between two nozzles is 120~160 °, dispersion Mixture later falls into just mixed pond, can carry out circulation dispersion.
(4) it is condensed after further being dispersed mixed liquor by way of grinding.The micelle of cohesion and desolventizing is taken off It is transferred to after water in heating belt type drying machine, heat drying obtains rubber master batch under vacuum.
2. a kind of silane coupled agent addition agent mixed method being kneaded applied to wet process as described in claim 1, feature exist In, silane coupling agent described in step (1) include component A and B component, wherein component A be vinyltriethoxysilane or Vinyltrimethoxysilane, B component are vinyl three (beta-methoxy ethyoxyl) silane, and the mass ratio of component A and B component is (1 ~2): 5.
3. such as a kind of silane coupled agent addition agent mixed method being kneaded applied to wet process claimed in claims 1-2, feature It is, white carbon black partial size described in step (1) is 30~80 μm.
CN201910136834.8A 2019-02-25 2019-02-25 A kind of silane coupled agent addition agent mixed method being kneaded applied to wet process Pending CN110066433A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114591551A (en) * 2022-04-14 2022-06-07 安徽永正密封件有限公司 Seepage-proofing rubber ring and floor drain with same

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999016600A1 (en) * 1997-09-30 1999-04-08 Cabot Corporation Elastomer composite blends and methods for producing them
CN101735466A (en) * 2009-11-06 2010-06-16 华东理工大学 Method for preparing rubber composite by high-pressure mixing equipment and application thereof
CN103203810A (en) * 2013-01-10 2013-07-17 怡维怡材料研究院有限公司 Continuous manufacturing method for rubber masterbatch, rubber masterbatch prepared by using continuous manufacturing method and rubber product

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999016600A1 (en) * 1997-09-30 1999-04-08 Cabot Corporation Elastomer composite blends and methods for producing them
CN101735466A (en) * 2009-11-06 2010-06-16 华东理工大学 Method for preparing rubber composite by high-pressure mixing equipment and application thereof
CN103203810A (en) * 2013-01-10 2013-07-17 怡维怡材料研究院有限公司 Continuous manufacturing method for rubber masterbatch, rubber masterbatch prepared by using continuous manufacturing method and rubber product

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
骆培成等: "液-液快速混合设备研究进展", 《化工进展》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114591551A (en) * 2022-04-14 2022-06-07 安徽永正密封件有限公司 Seepage-proofing rubber ring and floor drain with same

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Application publication date: 20190730