CN104629082A - Method for recovering and refining solvent and monomer in industrial production of rare earth isoprene rubber - Google Patents
Method for recovering and refining solvent and monomer in industrial production of rare earth isoprene rubber Download PDFInfo
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- CN104629082A CN104629082A CN201310552695.XA CN201310552695A CN104629082A CN 104629082 A CN104629082 A CN 104629082A CN 201310552695 A CN201310552695 A CN 201310552695A CN 104629082 A CN104629082 A CN 104629082A
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- 239000002904 solvent Substances 0.000 title claims abstract description 59
- 239000000178 monomer Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000007670 refining Methods 0.000 title claims abstract description 17
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 16
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 16
- 229920003049 isoprene rubber Polymers 0.000 title claims abstract description 14
- 238000009776 industrial production Methods 0.000 title abstract 2
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 claims abstract description 186
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 59
- 238000011084 recovery Methods 0.000 claims abstract description 39
- 238000010992 reflux Methods 0.000 claims abstract description 18
- 238000000605 extraction Methods 0.000 claims abstract description 10
- 238000001179 sorption measurement Methods 0.000 claims abstract description 7
- 238000003860 storage Methods 0.000 claims abstract description 4
- 229920001195 polyisoprene Polymers 0.000 claims description 13
- 229920001971 elastomer Polymers 0.000 claims description 11
- 239000005060 rubber Substances 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 9
- 239000003112 inhibitor Substances 0.000 claims description 9
- 238000000746 purification Methods 0.000 claims description 8
- 239000002044 hexane fraction Substances 0.000 claims description 7
- 238000006116 polymerization reaction Methods 0.000 claims description 7
- 238000007600 charging Methods 0.000 claims description 4
- -1 isoprenyl moiety Chemical group 0.000 claims description 4
- 150000001412 amines Chemical class 0.000 claims description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 3
- 150000004053 quinones Chemical class 0.000 claims description 3
- 239000002594 sorbent Substances 0.000 claims description 3
- KJQMOGOKAYDMOR-UHFFFAOYSA-N CC(=C)C=C.CC(=C)C=C Chemical compound CC(=C)C=C.CC(=C)C=C KJQMOGOKAYDMOR-UHFFFAOYSA-N 0.000 claims description 2
- 150000001345 alkine derivatives Chemical class 0.000 claims description 2
- 238000011049 filling Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 150000001299 aldehydes Chemical class 0.000 claims 1
- 239000006260 foam Substances 0.000 claims 1
- 150000002576 ketones Chemical class 0.000 claims 1
- 238000004064 recycling Methods 0.000 abstract description 4
- 229920000642 polymer Polymers 0.000 abstract description 2
- 238000005086 pumping Methods 0.000 abstract 2
- 238000005265 energy consumption Methods 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 22
- 239000007789 gas Substances 0.000 description 15
- 239000000463 material Substances 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 244000043261 Hevea brasiliensis Species 0.000 description 8
- 229920003052 natural elastomer Polymers 0.000 description 8
- 229920001194 natural rubber Polymers 0.000 description 8
- 230000008569 process Effects 0.000 description 7
- 239000000470 constituent Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000010092 rubber production Methods 0.000 description 4
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000012452 mother liquor Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 2
- 230000008676 import Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000005062 Polybutadiene Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- VLLYOYVKQDKAHN-UHFFFAOYSA-N buta-1,3-diene;2-methylbuta-1,3-diene Chemical compound C=CC=C.CC(=C)C=C VLLYOYVKQDKAHN-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 230000005226 mechanical processes and functions Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
The invention relates to a method for recovering a solvent and a monomer in industrial production of rare earth isoprene rubber; the side-draw position of the solvent recovery tower is close to 60-70 theoretical plates on the top of the tower; pumping part of refined hexane solvent into a storage tank from a side draw metering tank to be used as solvent for producing isoprene rubber, and refluxing part of isoprene to the top of the separator; the side-draw position of the isoprene refining tower is close to 70-90 theoretical plates on the top of the tower; gas-phase isoprene is extracted from the side line of the isoprene refining tower; pumping part of isoprene into an adsorption tower by a side draw metering tank to obtain a polymer grade isoprene monomer, and refluxing part of isoprene to the top of the separator; the method finishes solvent recovery and refining, recycling of unreacted monomers and refining of fresh monomers by only two rectifying towers with side line extraction, reduces equipment investment and energy consumption, and realizes complete continuous recycling of the hexane solvent and partial recycling of isoprene.
Description
Technical field:
The present invention relates to a kind of purification and recover method of solvent and monomer in rare-earth isoprene rubber suitability for industrialized production.
Background technology
Natural rubber is the most important raw material of Tire production, is and national economy and the closely-related valuable cargo of national security, with oil, iron ore with being classified as national strategy resource.Chinese rubber Year's consumption, more than 3,100,000 tons, occupies first place in the world.And China's natural rubber output only about 600,000 tons, only account for 5.4% of Gross World Product, the degree of self-sufficiency of natural rubber is less than 1/3, and lower than the most basic national security security system, criticality has exceeded the strategic materials such as oil, iron ore.In order to meet domestic development, the annual import natural rubber of China more than 2,000,000 tons, will account for more than 20% of Natural Rubber in The World total resources.The major hidden danger that import is national security depended on unduly by natural rubber.Polyisoprene rubber molecular structure and performance and natural rubber very close, alternative natural rubber, this is that the development of synthesis polyisoprene rubber provides a wide developing direction.Polyisoprene rubber has realized industrialization in states such as Russia, the U.S., Japan, and China has also started starting in this field, is progressively going deep into and development, C
5separation and deep processing are classified as key industry field in 12 planning, and application market is very wide.
Rare earth method polyisoprene rubber take isoprene as monomer, hexane is solvent, under rare earth catalyst effect, carry out solution polymerization form glue, containing a large amount of hexanes and unreacted isoprene monomer (isoprene transformation efficiency general control 75 ~ 85%) in glue, glue obtains polyisoprene rubber and mother liquor through elutriation cohesion and extruding drying.Containing whole solvents, unreacted monomer, water and trace impurity that polymerization is used in mother liquor, set up a set of for reclaiming unreacted monomer isoprene and hexane solvent in mother liquor, the method of refining isoprene materials simultaneously, polyisoprene rubber production cost can be reduced, reduce the wasting of resources, for polymerized unit provides qualified monomer and solvent, it is one of industrialized gordian technique of polyisoprene rubber.
At present, the patent be separated with the recovery of unreacted monomer about solvent in polyisoprene rubber production process is less, the recoverying and utilizing method of solvent and unreacted monomer in patent CN200710014320.2(solution polymerization process production polymer process) in refer to the dehydration, de-light and de-heavy that a kind of use rectifying tower completes solvent and unreacted monomer, but monomer is not separated with solvent by the method completely, also cannot overcome the autohemagglutination of monomer in rectifying tower in treating process simultaneously.Patent CN1908040A(technique of refining solvent in process of producing synthetic rubber) in mention and substitute single tower distillation technique with multiple rectifying tower, by improving the working pressure of an effect rectifying tower, utilize pressure difference and the temperature head of every, add the thermal source that last effect rectifying tower top gaseous phase solvent condenses hotwork is a rear effect rectifying tower reboiler, although the method can save a certain amount of steam consumption and cooling-water consumption, but in actual mechanical process, the operation stability of a rear effect rectifying tower is easily subject to the impact of last effect rectifying tower rising evaporating capacity.Patent CN102234356.A(rare-earth isoprene butadiene rubber production method) relate to the refining operational path of solvent recuperation and monomer, adopt multitower circulation preparation technology flow process, solve the monomer that causes because various of monomer and impurity boiling point thereof intersect and the lower problem of solvent purity, in order to allow vaporization and the condensation repeatedly between each rectifying tower of a large amount of solvent and monomer, more steam and water coolant need be consumed.
Summary of the invention
The object of this invention is to provide a kind of purification and recover method of solvent and monomer in rare-earth isoprene rubber suitability for industrialized production.By double tower continuous processing cohesion reclaimed unreacted isoprene, hexane solvent and micro-moisture in oil phase from, from solvent recovery tower side take-off gas phase hexane solvent, by separator with after the cooling of side take-off condenser condenses, obtain the refined hexane solvent being used for rare-earth isoprene rubber and producing; Unreacted isoprene enters isoprene treating tower together with fresh isoprene, from this tower side take-off gas phase isoprene, by separator with after the cooling of side take-off condenser condenses, then by absorption tower adsorbs removal of impurities, obtain the refining isoprene being used for rare-earth isoprene rubber and producing; Specifically comprise the steps:
(1) solvent recovery tower theoretical plate number is about 50 ~ 80 pieces, tower top temperature 35 ~ 38 DEG C, tower top pressure 0.1 ~ 5kPa, bottom temperature 69 ~ 76 DEG C, tower reactor pressure 3 ~ 10kPa, reflux temperature 15 ~ 20 DEG C, reflux ratio 10 ~ 50; Cohesion reclaims oil phase at solvent recovery tower near tower top 10 ~ 20 pieces of theoretical tray place chargings; Solvent recovery tower side take-off position is at close tower top 60 ~ 70 pieces of theoretical tray places;
(2) part refined hexane solvent is pumped into storage tank by side take-off test tank, and as the solvent producing polyisoprene rubber, part hexane solvent is back to separator top, reflux ratio 0.01 ~ 0.5, reflux temperature is 40 ~ 60 DEG C;
(3) from solvent recovery tower side take-off gas phase hexane fraction, its water-content≤10ppm is controlled, isoprene content≤0.1%; Level of inhibitor≤1ppm;
(4) isoprene treating tower theoretical plate number is 70 ~ 100 pieces, tower top temperature 33 ~ 35 DEG C, tower top pressure 0.1 ~ 5kPa, bottom temperature 35 ~ 42 DEG C, tower reactor pressure 3 ~ 10kPa, reflux temperature 15 ~ 20 DEG C, reflux ratio 100 ~ 200; After the recovery isoprene of solvent recuperation column overhead mixes with fresh isoprene, near 15 ~ 25 pieces of theoretical tray place chargings of isoprene treating tower tower top; Isoprene treating tower side take-off position is at close tower top 70 ~ 90 pieces of theoretical tray places;
(5) from isoprene treating tower side take-off gas phase isoprene, wherein water-content≤25ppm is controlled, level of inhibitor≤1ppm;
(6) part isoprene is pumped into adsorption tower by side take-off test tank, and obtain polymerization grade isoprene monomer, part isoprene is back to separator top, reflux ratio 0.01 ~ 0.5, reflux temperature is 15 ~ 30 DEG C;
(7) stopper used can be quinones, amine and phenolic inhibitor, and add from recovery tower and isoprene treating tower overhead condenser gas phase ingress after dissolving with isoprene, add-on is 0.05 ~ 0.1 ‰ of upflowing vapor amount.
Beneficial effect of the present invention:
(1) condense refiltered oil and complete solvent and being separated of unreacted monomer and refining of solvent by one with side take-off rectifying tower, the rate of recovery of unreacted isoprene and hexane solvent reaches 99.6% and 99.5% respectively, can be directly used in polymerization produce from side take-off refined hexane solvent.Refined by isoprene treating tower after the recovery isoprene of recovery tower overhead extraction mixes with fresh isoprene, remove light constituent impurity, stopper and minor amount of water, from side take-off gas phase isoprene, produce for rare-earth isoprene rubber polymerization after absorption tower adsorbs removal of impurities after condensation, without significant difference compared with the product that its property indices of the polyisoprene rubber produced is produced after refining with use fresh feed, if reclaim isoprene because of recycled number of times too much, when making foreign matter content severe overweight in the refining isoprene of isoprene treating tower side take-off, then recovery isoprenyl moiety can be sent out-of-bounds.Achieve the complete continuous circulation of hexane solvent to apply mechanically and isoprenyl moiety recycle, to reduction polyisoprene rubber production cost, reduce the wasting of resources and environmental pollution significant.
(2) isoprene contains 1,4 unsaturated double-bonds, belong to heat-sensitive material, by high temperature autohemagglutination phenomenon is obvious, easily in Ta Nei and overhead condenser, generate autopolymer occluding device, and cause the cis-content of polymerization polyisoprene rubber product and molecular weight distribution to have a negative impact.Therefore by controlling solvent recovery tower and isoprene treating tower tower top pressure and tower top temperature and adding a certain amount of stopper continuously in the gas phase ingress of overhead condenser, the phenomenon of isoprene autohemagglutination is alleviated.
(3) by installing the inner separator having special construction at solvent recovery tower and isoprene treating tower side line gas phase extraction mouth, significantly improve heavy constituent impurity and stopper in the gas phase hexane fraction gentle phase isoprene of side take-off and carry serious phenomenon secretly, especially when condensing oil phase and raw material isoprene heavy constituent foreign matter content is higher, this separator obviously can reduce foreign matter content in refined hexane solvent and refining isoprene, enables the purity of hexane fraction content and refining isoprene in refined hexane solvent reach more than 99.7%.
(4) according to polarity and the molecular diameter of detrimental impurity, use the adsorption tower of one or more filling sorbent material, trace impurity rectifying being difficult to remove is removed further, as monoolefine, and alkynes, the water of aldehyde ketone and denier.
Embodiment
Embodiment 1
(1) refiltered oil phase composite is in table 1, control certain flow enters into solvent recovery tower and is separated, at tower top hexane, the light constituent such as isoprene and minor amount of water through recovery tower condenser condenses cooling after in recovery tower return tank of top of the tower, then a part of extraction enter together with fresh isoprene isoprene treating tower carry out isoprene refining (when reclaim isoprene because of recycled number of times too much, when its foreign matter content exceedes prescribed value, send out-of-bounds by all or part of for recovery isoprene, do not enter isoprene treating tower to refine together with fresh isoprene, another part returns stream by the Liquid level certain flow of recovery tower return tank, the free-water be enriched at the bottom of tank is regularly released, control heavy component content≤1% such as recovery tower tower top hexane,
(2) from side take-off gas phase hexane fraction, wherein water-content≤10ppm is controlled, isoprene content≤0.1%, level of inhibitor≤1ppm.Qualified gas phase hexane fraction enters in side take-off test tank after separator and the condensation of recovery tower side line condenser device, cooling.A material part in side take-off test tank controls certain flow and is back to separator top, and another part is according to refined hexane extraction test tank Liquid level flow extraction extremely corresponding refined hexane storage tank.In recovery tower tower reactor, heavy component is according to the extraction of material composition control flow, focuses on.
Add stopper in recovery tower overhead condenser gas phase ingress, stopper addition is 0.03 ‰ of rectifying tower upflowing vapor amount.
(3) be separated being driven in isoprene treating tower after the recovery isoprene of solvent recovery tower overhead extraction and fresh isoprene on-line mixing; Tower top light constituent and with the minor amount of water of isoprene azeotropic after isoprene treating tower condenser condenses cools, enter into isoprene treating tower return tank, the free-water be enriched at the bottom of tank is regularly released, oil phase controls certain flow and returns stream, when the material light constituent too high levels in return tank of top of the tower affects quality product, release partial material in return tank, recycling; From isoprene treating tower side take-off gas phase isoprene cut, control wherein water-content≤25ppm, level of inhibitor≤1ppm.Qualified gas phase isoprene send in side take-off test tank after separator and isoprene treating tower side line condenser condenses, cooling.In material a part control certain flow be back to side take-off test tank top, material is pumped into adsorption tower according to side take-off test tank Liquid level flow by another part.In isoprene treating tower tower reactor, heavy component is according to the extraction of material composition control flow, focuses on.
Add stopper in isoprene treating tower overhead condenser gas phase ingress, stopper addition is 0.03 ‰ of rectifying tower upflowing vapor amount.
(4), after isoprene adsorption-edulcoration tower runs for some time continuously, when purification capacity declines obvious, artificial regeneration's process need be carried out to sorbent material.
Table 1: cohesion refiltered oil phase composite
| Sequence number | Title | wt% |
| 1 | Low-boiling-point substance | 0.0285 |
| 2 | Isoprene | 2.3061 |
| 3 | Hexane fraction | 97.4601 |
| 4 | Dipolymer | 0.0214 |
| 5 | Water | 0.1825 |
| 6 | High boiling material | 0.0132 |
| 7 | TBC | 0.0041 |
Table 2: solvent recuperation column overhead, side take-off material form
Table 2: isoprene treating tower tower top, side take-off material form
Table 3: isoprene drying tower turnover material composition
Claims (5)
1. the recovery method of solvent and monomer in rare-earth isoprene rubber suitability for industrialized production, is characterized in that:
(1) solvent recovery tower theoretical plate number is 50 ~ 80 pieces, tower top temperature 35 ~ 38 DEG C, tower top pressure 0.1 ~ 5kPa, bottom temperature 69 ~ 76 DEG C, tower reactor pressure 3 ~ 10kPa, reflux temperature 15 ~ 20 DEG C, reflux ratio 30 ~ 50; Cohesion reclaims oil phase at solvent recovery tower near tower top 10 ~ 20 pieces of theoretical tray place chargings; Solvent recovery tower side take-off position is at close tower top 60 ~ 70 pieces of theoretical tray places;
(2) from side take-off test tank, part refined hexane solvent is pumped into storage tank, as the solvent producing polyisoprene rubber, part isoprene is back to separator top, reflux ratio 0.01 ~ 0.5, reflux temperature is 40 ~ 60 DEG C;
(3) from solvent recovery tower side take-off gas phase hexane fraction, its water-content≤10ppm is controlled, isoprene content≤0.1%; Level of inhibitor≤1ppm;
(4) isoprene treating tower theoretical plate number is 70 ~ 100 pieces, tower top temperature 33 ~ 35 DEG C, tower top pressure 0.1 ~ 5kPa, bottom temperature 35 ~ 42 DEG C, tower reactor pressure 3 ~ 10kPa, reflux temperature 15 ~ 20 DEG C, reflux ratio 100 ~ 200; After the recovery isoprene of solvent recuperation column overhead mixes with fresh isoprene, near 15 ~ 25 pieces of theoretical tray place chargings of isoprene treating tower tower top; Isoprene treating tower side take-off position is at close tower top 70 ~ 90 pieces of theoretical tray places;
(5) from isoprene treating tower side take-off gas phase isoprene, wherein water-content≤25ppm is controlled, level of inhibitor≤1ppm;
(6) part isoprene is pumped into adsorption tower by side take-off test tank, and obtain polymerization grade isoprene monomer, part isoprene is back to separator top, reflux ratio 0.01 ~ 0.5, reflux temperature is 15 ~ 30 DEG C;
(7) stopper used can be quinones, amine and phenolic inhibitor, and add from recovery tower and isoprene treating tower overhead condenser gas phase ingress after dissolving with isoprene, add-on is 0.05 ~ 0.1 ‰ of upflowing vapor amount.
2. solvent and MONOMER RECOVERY process for purification in a kind of rare-earth isoprene rubber suitability for industrialized production according to claim 1, is characterized in that: separator is the equipment possessing separation and foam removal function.
3. the purification and recover method of solvent and monomer in a kind of rare-earth isoprene rubber suitability for industrialized production according to claim 1, it is characterized in that: after separator, enter side line condenser from the gas phase isoprene of side take-off, the adsorption tower adsorption selection that condensed refining isoprene enters the different sorbent material of filling of multiple series connection is in order refined in isoprene isoprene polymerization influential trace impurity monoolefine, alkynes and aldehyde, ketone.
4. the purification and recover method of solvent and monomer in a kind of rare-earth isoprene rubber suitability for industrialized production according to claim 1, it is characterized in that: refined by isoprene treating tower after the recovery isoprene of recovery tower overhead extraction mixes with fresh isoprene, when recovery isoprene because recycled number of times is too much, when making foreign matter content severe overweight in the refining isoprene of isoprene treating tower side take-off, then recovery isoprenyl moiety can be sent out-of-bounds.
5. the purification and recover method of solvent and monomer in a kind of rare-earth isoprene rubber suitability for industrialized production according to claim 1, is characterized in that: the described stopper that adds is: quinones, amine and phenolic inhibitor.
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| CN109438165A (en) * | 2018-12-29 | 2019-03-08 | 山东京博石油化工有限公司 | A kind of separation and recovery method of isobutene recycling tower bottom liquid |
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| CN111793153A (en) * | 2020-06-30 | 2020-10-20 | 北京诺维新材科技有限公司 | Preparation method and preparation device of rubber |
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| CN109438165B (en) * | 2018-12-29 | 2022-03-15 | 山东京博石油化工有限公司 | Separation and recovery method of isobutene recovery tower bottom liquid |
| CN112745439A (en) * | 2019-10-31 | 2021-05-04 | 中国石油化工股份有限公司 | Polymer solution preparation method and butyl rubber production method |
| CN112745439B (en) * | 2019-10-31 | 2022-07-12 | 中国石油化工股份有限公司 | Polymer solution preparation method and butyl rubber production method |
| CN111793153A (en) * | 2020-06-30 | 2020-10-20 | 北京诺维新材科技有限公司 | Preparation method and preparation device of rubber |
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