CN110193890A - A kind of wet process mixing continuous production technology of isoprene rubber - Google Patents
A kind of wet process mixing continuous production technology of isoprene rubber Download PDFInfo
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- CN110193890A CN110193890A CN201910492292.8A CN201910492292A CN110193890A CN 110193890 A CN110193890 A CN 110193890A CN 201910492292 A CN201910492292 A CN 201910492292A CN 110193890 A CN110193890 A CN 110193890A
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- isoprene rubber
- rare earth
- filler
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- isoprene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/002—Methods
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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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/205—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase
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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
- C08J2309/00—Characterised by the use of homopolymers or copolymers of conjugated diene hydrocarbons
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- Engineering & Computer Science (AREA)
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses a kind of wet processes of isoprene rubber to be kneaded continuous production technology, includes the following steps: the preparation of (1) isoprene rubber solution；(2) white carbon black, carbon black, nano rare earth filler and isoprene rubber solution are stirred smart dispersion；(3) the isoprene rubber solution after essence dispersion is subjected to two-stage mixing and obtains finished rubber.The present invention realizes the mass production technique of isoprene rubber, reduces costs, and improves production efficiency, and the separately made dispersion liquid of the lesser filler of granularity is added, and reduces the usage amount of organic solvent, and two-part calendering process is suitble to the demand of production.
Description
Technical field
The present invention relates to rubber materials, in particular to the wet process of a kind of isoprene rubber is kneaded continuous production technology.
Background technique
The high-cis that isoprene rubber (polyisoprene) is synthesized by isoprene (cis- Isosorbide-5-Nitrae content is 92%~97%)
Synthetic rubber, closest to natural rubber, water resistance, electrical insulating property is more than natural rubber.It is that a kind of comprehensive performance is led to well
With synthetic rubber, it is mainly used for tire production, in addition to aviation and band tyre, can replaces natural rubber.But its raw rubber is strong
Degree, adherence, tearing toughness, the fatigue durability of processing performance and vulcanizate etc. are slightly less than natural rubber.China at present
The certain components of all-steel load-bearing radial tire needed for isoprene rubber from Russia introduce, import volume is more than 10,000 tons, valence
Lattice are also stepping up.
The domestic wet process to isoprene rubber is kneaded continuous production technical research and is concentrated mainly on Sinopec's stock at present
The units such as part Co., Ltd, Beijing Chemical Research Institute, Qingdao University of Science and Technology, but its research is concentrated on laboratory stage progress
The polymerization of isoprene rubber, rare earth addition etc., there are no the mature production technology for forming large-scale industrial production and being applicable in,
Simultaneously to the adding technology of the common reinforcing filler of the rubber productions such as isoprene rubber and carbon black, white carbon black, and specific effect
It there is no report.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of wet processes of isoprene rubber to be kneaded continuous production technology.And
According to the industrialized production parameter of exploitation, proposes applicable filler processing and Multistage dispersion mode, significantly improve the property of rubber
Energy.
The complete technical solution of the present invention includes:
A kind of wet process mixing continuous production technology of isoprene rubber, which comprises the steps of:
(1) preparation of isoprene rubber solution；
(2) white carbon black, carbon black, nano rare earth filler and isoprene rubber solution are stirred smart dispersion；
(3) the isoprene rubber solution after essence dispersion is subjected to two-stage mixing and obtains finished rubber.
Wherein, step 1 is that organic solvent is added using isoprene monomer, and after being activated using activating component,
Finally using the method for two sections of polymerizations, the preparation of isoprene rubber solution is realized.
Step 2 is the isoprene rubber performance requirement first according to actual production, joined specific filler component, and to it
Dosage has carried out reasonable restriction.The isoprene rubber of filler essence dispersion is formd by the way of shear-mixed using being separately added into and stirring
Solution.
Step 3 is to be groped in actual production, has finally chosen two-part mixing, and first segment first is mixed using high speed
Refining, is sufficiently mixed filler and part addO-on therapy, then stands cooling a period of time, and it is mixed then to carry out second segment at this slow speed
Refining, and by the way of water cooling, it is maintained at roller temperature in one zone of reasonableness, prevents its temperature excessively high, improve rubber
State of cure (vulcanization).
The improvement of the present invention compared with the existing technology are as follows: isoprene rubber lab scale synthetic method in the prior art is referred to,
On the basis of reasonable improvement, simplifies and falls process portion, and realize the mass production technique of isoprene rubber, reduce costs,
Production efficiency is improved, the reasonable filler of simultaneous selection enhances component, while being directed to different filler component, and granularity is lesser
The separately made dispersion liquid of filler prevents from reuniting in the early stage.Remaining filler is then directly added into, and reduces the usage amount of organic solvent,
Two-part calendering process is found out, preparation takes into account efficiency and performance, is suitble to the demand of production, and synthetic rubber wet process is kneaded and is connected
Continuous technical transform is 10,000 tons production line, realizes the technological industrialization.
Specific embodiment
The present invention will be further described With reference to embodiment.
(1) preparation of isoprene rubber solution:
By 100 parts of isoprene monomers, 0.4~0.6 part of diisobutylaluminium hydride and triisobutyl aluminium mixture anti-
It answers in kettle and is mixed, and realize uniform activation at 40 DEG C to stir 6h under the revolving speed of 200~400rpm.Hydrogenate two isobutyls
The mass ratio of base aluminium and triisobutyl aluminium is 2:1, and 450 parts of hexane solvents are added in the isoprene monomer after activation, are then added
Enter 0.08 part of active rare earth catalyst prepolymerization 1h at 45~55 DEG C, after standing 3h, 0.15 part of active rare earth catalyst be added,
It polymerize 4h at 55~65 DEG C, obtains isoprene rubber solution.
(2) selection isoprene rubber solution: 100-120 parts；White carbon black: 12~15 parts, carbon black: 6~8 parts, nano rare earth is filled out
Material: 0.1~0.3 part.Solvent is added in nano rare earth filler, is dispersed with stirring to obtain nano rare earth filler dispersion liquid.By Nano Rare
Isoprene rubber solution is added in native filler mixed liquor and other fillers, and smart dispersion is carried out by the way of rotational shear, obtains filler
Isoprene rubber solution after essence dispersion.The granularity of nano rare earth filler is nanoscale herein, and the granularity of carbon black and white carbon black is
Micron order, therefore the separately made dispersion liquid of rare earth filler that granularity is minimum, is easiest to reunion is made using organic solvent first, it prevents
Reunite in the early stage.And remaining filler is then then added in rubber solutions together with other large-sized fillers, reduces organic molten
The usage amount of agent carries out smart dispersion by the way of integrally stirring and partial cut, obtains isoprene rubber essence dispersion liquid.
(3) by isoprene rubber essence dispersion liquid obtained above into two-stage mixing, the isoamyl rubber of organic solvent will be recycled first
Glue essence dispersion liquid, addition, which accounts for, the stearic acid of its total amount 2% and accounts for the zinc oxide of its total amount 3.5%, in quick mixer with
50r/min revolving speed carries out first segment mixing, mixes filler and addO-on therapy, it is small that the rubber compound bottom sheet arrived after mixing stands 12
When, vulcanizing agent and ultras is then added and is kneaded to obtain finished rubber with the speed progress second segment of 15r/min, second segment is mixed
Guarantee that roller temperature is no more than 40 DEG C when refining, with can full cure.
Especially, the wherein production method of white carbon black are as follows: white carbon black production is carried out using atomization, specially configures 100
The water glass solution that part mass percent concentration is 20%, is added 0.02 part of CTMAB (molecular formula are as follows: C19H42BrN) at 85 DEG C
Under 10min stirred with the speed of 400rpm, be subsequently sent in atomisation tower, atomisation tower center is equipped with high speed centrifugation turntable, and centrifugation turns
Multiple outlets are equipped on the outside of disk, water glass solution is entered high speed centrifugation turntable by pipeline and is rotated with 1200 turns of speed,
And thrown away under the action of the centrifugal force by multiple outlets, it is atomized the air nozzle that multiple alignment outlets are surrounded on inner wall of tower, and
The carbon dioxide gas of high speed, the water for making carbon dioxide gas and throwing away are sprayed by the water glass solution that air nozzle alignment is thrown away
Glass solution is contacted and is atomized, and is increased the contact area of water glass solution and carbon dioxide gas using the above method, is made
Reaction can be completed in 2-3s and generate white carbon black.
Above-mentioned preparation method of the invention is atomized with reference in the prior art using atomizing disk to a certain extent
Method, but atomizing disk atomization in the prior art is directly to spray water glass solution to high-speed rotating atomizing disk disk
On, and droplet is formed under the action of the centrifugal force, with the carbon dioxide gas precursor reactant in atomisation tower.Carbon dioxide in the above process
Gas pressure is smaller, and is static contact with waterglass drop, and reaction is not enough, mode of the invention, using centrifugal water
The mode of glass solution and the direct high speed contact of carbon dioxide gas stream realizes atomization, improves nebulization efficiency.The hard charcoal that will be obtained
The collection of black wash liquid is separated by solid-liquid separation, dry, subsequent processing, white carbon black filler needed for obtaining rubber production.
Using method of the invention, builds up and produce 10,000 tons synthetic rubber continuous wet process mixing production line one per year, realize life
Production process than 20% or more traditional handicraft energy conservation, meanwhile, so that preparation high-performance compounded rubber for tire production roll resistance
Power and wet-sliding resistant performance reach Labeling Act of European Union rule B grade standard, and rolling resistance reduces by 20% or more, and wear-resisting property improves 20%
More than.
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 (4)
1. a kind of wet process of isoprene rubber is kneaded continuous production technology, which comprises the steps of:
(1) preparation of isoprene rubber solution；
(2) white carbon black, carbon black, nano rare earth filler and isoprene rubber solution are stirred smart dispersion；
(3) the isoprene rubber solution after essence dispersion is subjected to two-stage mixing and obtains finished rubber.
2. a kind of wet process of isoprene rubber according to claim 1 is kneaded continuous production technology, which is characterized in that step
It (1) is specially by 100 parts of isoprene monomers, 0.4~0.6 part of diisobutylaluminium hydride and triisobutyl aluminium mixture anti-
It answers in kettle and is mixed, and realize uniform activation at 40 DEG C to stir 6h under the revolving speed of 200~400rpm.Hydrogenate two isobutyls
The mass ratio of base aluminium and triisobutyl aluminium is 2:1, and 450 parts of hexane solvents are added in the isoprene monomer after activation, are then added
Enter 0.08 part of active rare earth catalyst prepolymerization 1h at 45~55 DEG C, after standing 3h, 0.15 part of active rare earth catalyst be added,
It polymerize 4h at 55~65 DEG C, obtains isoprene rubber solution.
3. a kind of wet process of isoprene rubber according to claim 1 is kneaded continuous production technology, which is characterized in that step
It (2) is specially selection isoprene rubber solution: 100-120 parts；White carbon black: 12~15 parts, carbon black: 6~8 parts, nano rare earth filler:
0.1~0.3 part.Solvent is added in nano rare earth filler, is dispersed with stirring to obtain nano rare earth filler dispersion liquid.Nano rare earth is filled out
Expect that isoprene rubber solution is added in mixed liquor and other fillers, smart dispersion is carried out by the way of rotational shear, obtains filler essence point
Isoprene rubber solution after dissipating.
4. a kind of wet process of isoprene rubber according to claim 1 is kneaded continuous production technology, which is characterized in that step
(3) it is specially the isoprene rubber essence dispersion liquid that will recycle organic solvent first, the stearic acid and Zhan Qizong for accounting for its total amount 2% is added
The zinc oxide of amount 3.5% carries out first segment mixing in quick mixer with 50r/min revolving speed, keeps filler and addO-on therapy mixed
It closes, the rubber compound bottom sheet arrived after mixing stands 12 hours, and vulcanizing agent and ultras is then added and is carried out with the speed of 15r/min
Second segment is kneaded to obtain finished rubber, guarantees that roller temperature is no more than 40 DEG C when second segment is kneaded, with can full cure.
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| CN201910492292.8A CN110193890B (en) | 2019-06-06 | 2019-06-06 | Wet mixing continuous production method of isoprene rubber |
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| CN110193890B CN110193890B (en) | 2020-05-19 |
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85102250A (en) * | 1985-04-01 | 1987-01-17 | 中国科学院长春应用化学研究所 | The mass polymerization of isoprene under the rare earth catalyst effect |
| CN101781411A (en) * | 2009-12-21 | 2010-07-21 | 中国科学院长春应用化学研究所 | Preparation method of rare earth isoprene rubber |
| CN101880345A (en) * | 2009-05-06 | 2010-11-10 | 淄博鲁华泓锦化工股份有限公司 | Pre-mixing process in rare-earth isoprene rubber production process |
| CN102532613A (en) * | 2010-12-29 | 2012-07-04 | 中国石油化工股份有限公司 | Rubber composition |
| CN103224659A (en) * | 2013-03-25 | 2013-07-31 | 怡维怡材料研究院有限公司 | Filler, synthetic rubber and wet rubber compound integrated production method |
| CN103936015A (en) * | 2014-04-28 | 2014-07-23 | 北京化工大学 | Method for preparing white carbon black slurry by using spraying method |
| CN103936014A (en) * | 2014-04-28 | 2014-07-23 | 北京化工大学 | Preparation method of novel white carbon black |
| CN104591195A (en) * | 2015-01-09 | 2015-05-06 | 北京化工大学 | Method of preparing white carbon black by virtue of carbonization method |
| CN105732867A (en) * | 2014-12-11 | 2016-07-06 | 中国石油天然气股份有限公司 | Solution polymerization method for rare earth isoprene rubber |
-
2019
- 2019-06-06 CN CN201910492292.8A patent/CN110193890B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85102250A (en) * | 1985-04-01 | 1987-01-17 | 中国科学院长春应用化学研究所 | The mass polymerization of isoprene under the rare earth catalyst effect |
| CN101880345A (en) * | 2009-05-06 | 2010-11-10 | 淄博鲁华泓锦化工股份有限公司 | Pre-mixing process in rare-earth isoprene rubber production process |
| CN101781411A (en) * | 2009-12-21 | 2010-07-21 | 中国科学院长春应用化学研究所 | Preparation method of rare earth isoprene rubber |
| CN102532613A (en) * | 2010-12-29 | 2012-07-04 | 中国石油化工股份有限公司 | Rubber composition |
| CN103224659A (en) * | 2013-03-25 | 2013-07-31 | 怡维怡材料研究院有限公司 | Filler, synthetic rubber and wet rubber compound integrated production method |
| CN103936015A (en) * | 2014-04-28 | 2014-07-23 | 北京化工大学 | Method for preparing white carbon black slurry by using spraying method |
| CN103936014A (en) * | 2014-04-28 | 2014-07-23 | 北京化工大学 | Preparation method of novel white carbon black |
| CN105732867A (en) * | 2014-12-11 | 2016-07-06 | 中国石油天然气股份有限公司 | Solution polymerization method for rare earth isoprene rubber |
| CN104591195A (en) * | 2015-01-09 | 2015-05-06 | 北京化工大学 | Method of preparing white carbon black by virtue of carbonization method |
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