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CN202124586U - Stirrer - Google Patents

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Publication number
CN202124586U
CN202124586U CN2011200743612U CN201120074361U CN202124586U CN 202124586 U CN202124586 U CN 202124586U CN 2011200743612 U CN2011200743612 U CN 2011200743612U CN 201120074361 U CN201120074361 U CN 201120074361U CN 202124586 U CN202124586 U CN 202124586U
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China
Prior art keywords
whisking appliance
diameter
type stirring
turbine type
leaf disc
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Expired - Lifetime
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CN2011200743612U
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Inventor
张国娟
张�杰
李传清
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Sinopec Beijing Research Institute of Chemical Industry
China Petroleum and Chemical Corp
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Sinopec Beijing Research Institute of Chemical Industry
China Petroleum and Chemical Corp
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Abstract

The utility model relates to a stirrer which can be used for a polymerization reaction kettle for preparing rare earth isoprene rubber. The stirrer comprises a stirring shaft, a double helical ribbon type agitator blade and a four inclined blade disk turbo type agitator blade, wherein the double helical ribbon type agitator blade and the four inclined blade disk turbo type agitator blade are installed on the stirring shaft. In the stirrer disclosed by the utility model, the mass transfer and heat transfer process in the polymerization reaction kettle is enhanced, so that high-viscosity material in the polymerization reaction kettle achieves good mixing effect, the cis-form-1,4-configuration content and the number-average molar mass as well as the molecular weight distribution coefficient of the rare earth isoprene rubber product are improved, the efficiency of catalyst in reaction can be effectively improved, and production cost is lowered.

Description

Whisking appliance
Technical field
The utility model relates to a kind of whisking appliance, relates more specifically to a kind of whisking appliance that is used to prepare rare-earth isoprene rubber.
Background technology
What rare-earth isoprene rubber was that isoprene monomer solution polymerization under the rare earth catalyst effect generates is main polymkeric substance with suitable-1,4 structural unit.Because its physicals is all similar with tree elastomer (NR) with mechanical property, rare-earth isoprene rubber also is called as " natural synthetic rubber ".Particularly; Rare-earth isoprene rubber has excellent elasticity, stopping property, creep resistant, wear resistance, thermotolerance and tear strength; And tensile strength and elongation are also near tree elastomer; Therefore the surrogate that can be used as tree elastomer in some cases also can use with tree elastomer (NR) or the combination of other viton.Therefore, rare-earth isoprene rubber is widely used in Rubber processing fields such as tire, adhesive tape, sebific duct.
In the rare-earth isoprene rubber production process, raw material is behind premix, and its main polyreaction is carried out in a plurality of placed in-line continuous stir reactor reactor drums (CSTR) usually, and wherein near complete mixing flow, and there is not back-mixing in reaction mass between each reaction kettle in each reaction kettle.Said reaction kettle is made up of kettle and whisking appliance, though still internal reaction material near complete mixing flow, exists but still have short circuit, dead band phenomenon.In addition; In the solution polymerization process of preparation rare-earth isoprene rubber; The admixture of polyreaction material (comprising isoprene monomer, solvent and catalyzer) in still will directly influence speed, the catalyst levels of polyreaction, and cis-configuration content, molecular weight and the MWD of gained rubber product.Therefore, selecting suitable whisking appliance is very important to whole polymerization process.
In the prior art, the synthesizing rare-earth polyisoprene rubber adopts the polymerization stirrer identical with the synthesizing rare-earth cis-1,4-polybutadiene rubber mostly.For example; In the rare earth polybutadiene rubber production technique, use the double ribbon agitator typically be suitable for high sticking system, Muscovite Kauchuk company has adopted double ribbon agitator equally in carrying out rare-earth isoprene rubber synthetic polymeric kettle, and adopts isopyknic three stills series connection continuous polymerization technique; The cis of the rare-earth isoprene rubber that obtains-1; 4-configuration content can reach 96wt%, and molecular weight can reach 420,000, and the MWD coefficient can reach 3.24.
In the rare-earth isoprene rubber building-up process that adopts many stills tandem process; Go out on advancing under mostly the trend of material in polymeric kettle is; The monomer isoprene forms the bigger polymers soln of viscosity after polymerization; And along with increasing progressively of polymeric kettle order; The viscosity of resulting polymers solution increases gradually, and the material viscosity that therefore gets in the polymeric kettle at the bottom of the polymeric kettle is all low than the material viscosity in the polymeric kettle, thereby the LV material that must occur just having got into from the still bottom and the high-viscosity material in the polymeric kettle are difficult to the blended problem.
The two ribbon impellers of the typical case who is adopted in the prior art, its oar footpath is bigger, is generally about 95% of polymeric kettle internal diameter.This constructional feature has been strengthened the mixing between the still wall place material, but along the mixture strength that stirs axial still region intermediate material then relatively a little less than.And the material inlet at the bottom of the still often is in above-mentioned mixture strength more weak zone relatively; Therefore be unfavorable for just getting into mixing between viscosity is lower in the polymeric kettle material and the higher reaction mass of the interior viscosity of still, and then influence monomeric transformation efficiency and final quality product.
Especially; This kind situation can appear at following occasion: at the bottom of still, directly add quantitative, as to be used for specific purposes material by processing requirement; Because this strand material is generally the liquid of the very low similar water of viscosity, cause mixing difficulty between the interior high viscosity copolymer solution of itself and still.
Therefore; Solution polymerization process for the preparation rare-earth isoprene rubber; Need further to improve the pattern of whisking appliance in the polymeric kettle; Make it help just getting into mixing between the lower material of viscosity in the polymeric kettle and the higher reaction mass of the interior viscosity of still, and then improve the quality of monomeric transformation efficiency and the finished product.
The utility model content
To above-mentioned problem; The utility model provides a kind of whisking appliance that is used to produce rare-earth isoprene rubber; It can strengthen mixing between LV material that polymeric kettle still bottom just got into and the interior high-viscosity material of still effectively; More help the carrying out of polyreaction, and then improve the quality of monomeric transformation efficiency and the finished product.
According to the utility model, a kind of whisking appliance that is used in the polymerization reaction kettle for preparing rare-earth isoprene rubber is provided, comprise stir shaft and be installed in the two ribbon impellers on this stir shaft.Wherein, four oblique leaf disc turbine type stirring rakes also have been installed on stir shaft.
According to an embodiment of the utility model, the diameter of said four oblique leaf disc turbine type stirring rakes and the diameter ratio of polymeric kettle are 1/5-1/2, are preferably 1/4-2/5, more preferably 1/3.The diameter ratio of the width of blade of said four oblique leaf disc turbine type stirring rakes and four oblique leaf disc turbine type stirring rakes is 1/5-1/4, is preferably 1/4.The diameter ratio of the depth of blade of said four oblique leaf disc turbine type stirring rakes and said four oblique leaf disc turbine type stirring rakes is 3/20-1/4, is preferably 1/5.
According to an embodiment of the utility model, the blade of said four oblique leaf disc turbine type stirring rakes is installed on the disk of being located on the stir shaft with 45.Said blade embeds in the said disk at the middle part of its height, and the width of embedding is the 1/3-2/3 of its whole blade width, is preferably 1/2.And said four oblique leaf disc turbine type stirring rakes are the 1/5-1/3 of its pitch with its center apart from the distance from bottom of two ribbon impellers, and 1/4 the mode of being preferably is installed on the stir shaft.In one embodiment, the diameter ratio of the diameter of disk and four oblique leaf disc turbine type stirring rakes is 3/5-4/5, is preferably 3/4.
According to an embodiment of the utility model, the diameter of said pair of ribbon impeller and the diameter ratio of polymeric kettle are 90%-98%, are preferably 95%.The ribbon width is the 5%-15% of ribbon diameter, is preferably 10%.The ratio of pitch and ribbon diameter is 0.5-1.5, is preferably 1.0.
Compared with prior art; The beneficial effect of the utility model is: said pair of ribbon impeller makes polymer material in polymeric kettle, form whole systemic circulation; Said four oblique leaf disc turbine type stirring rakes then are used to make the LV material in the firm entering polymeric kettle to disperse simultaneously; Thereby reach the purpose of material in the thorough mixing still, be beneficial to the carrying out of subsequent solution polyreaction.
Description of drawings
To come the utility model is described in more detail based on various embodiment and with reference to accompanying drawing hereinafter.Wherein:
Fig. 1 is the synoptic diagram according to the whisking appliance of the utility model;
Fig. 2 has been to use the synoptic diagram according to the isoprene monomer solution polymerization flow process of the polymeric kettle of the whisking appliance of Fig. 1.
In each width of cloth figure, identical member is indicated by similar Reference numeral.Accompanying drawing is not according to the scale of reality.
Embodiment
Below through embodiment the utility model is described in further detail, but these embodiment should not think the restriction to the utility model scope.Need to prove that in addition all scope parts that relates to numerical value in the utility model have all comprised two endpoint values of this scope.
Fig. 1 has shown the whisking appliance 10 according to the utility model.This whisking appliance 10 comprises the stir shaft 11 that is driven by motor M.Duplex belt stirring rake 12 and four oblique leaf disc turbine type stirring rakes 13 have been installed on stir shaft 11, and wherein four oblique leaf disc turbine type stirring rakes 13 link to each other with stir shaft 11 through disk 14.
Fig. 2 has been to use the synoptic diagram according to the isoprene monomer solution polymerization flow process of the polymerization reaction kettle of the utility model whisking appliance 10.Wherein, having the isoprene pipeline 21 of interchanger 24, the solvent line 23 that has interchanger 25 and catalyst line 22 all leads in the premixed device 26.Three polymerization reaction kettles 27,28,29 after premixed device 26, have been arranged.These three polymerization reaction kettle 27-29 have all used the whisking appliance 10 according to the utility model.
In technological process, solvent at first mixes in premixed device 26 after catalyzer and cooled isoprene, the cooling, feeds in the polymeric kettle then and reacts.Preferably; The shared opening for feed that is positioned on the premixed device 26 of catalyzer and solvent, and isoprene uses an opening for feed separately, simultaneously as shown in Figure 2; Can add cooled solvent in the bottom of second polymeric kettle 28 to it through other passage, final product can be discharged by outlet 20.
Embodiment 1:
The volume of employed polymerization reaction kettle is 120L, and diameter is 450mm, and height is 750mm.In this embodiment, the diameter of two ribbon impellers 12 is 95% of a polymerization reaction kettle diameter, and the ribbon width is 10% of its stirring rake diameter, and the ratio of pitch and ribbon diameter is 1, and the height of whole ribbon equates with the interior liquid material height of polymeric kettle.
In this embodiment, the diameter of four oblique leaf disc turbine type stirring rakes 13 is 1/3 of a polymerization reaction kettle diameter.Its width of blade is 1/4 of said four oblique leaf disc turbine type stirring rake diameters, and depth of blade is 1/5 of said four oblique leaf disc turbine type stirring rake diameters.In addition, blade pass is crossed disk 14 and is installed on the stir shaft 11, and its width that embeds disk 14 is 1/2 of a whole blade width, and its setting angle is 45 °.The diameter of disk 14 is that the center of 3/4, four oblique leaf disc turbine type stirring rake 13 of four oblique leaf disc turbine type stirring rake diameters is 1/4 of its pitch apart from the distance from bottom of two ribbon impellers 12.
In actual process; At first will be in the isoprene monomer (14.6kg/h that being used under the normal temperature and pressure prepares the polyreaction material of rare-earth isoprene rubber; Polymerization-grade), solvent (73.75kg/h; Solvent as used herein is a hexanaphthene) in interchanger 24,25, carry out precooling, precooling is to-22 ℃.At this, employed heat-eliminating medium is a liquefied ammonia.Polyreaction material after the precooling is incorporated into respectively carries out premix in the premixed device 26.(2.9kg/h, concentration is 6 * 10 with the neodymium series catalysts -6MolNd/ml; Solvent is a hexanaphthene; The concrete composition of neodymium series catalysts as used herein is an isoprene by the molar ratio computing of each component: neodecanoic acid neodymium: triisobutyl aluminium: aluminium diethyl monochloride=50: 1: 10: 3) be incorporated in the premixed device 26, carry out premix operation fully with above-mentioned isoprene monomer, solvent.Wherein, the shared opening for feed of solvent and catalyzer is incorporated into premixed device 26, and isoprene monomer then is incorporated in the premixed device 26 through an opening for feed separately.Simultaneously add cooled quantitative solvent (21.05kg/h, solvent as used herein are hexanaphthene) through independent opening for feed in the bottom of second polymerization reaction kettle 28.
Next, carry out the operation of polymerization stage according to said flow process.The polyreaction material that forms behind precooling, the premix is got in each polymerization reaction kettle successively react, and the mean residence time in each polymerization reaction kettle is respectively: first polymerization reaction kettle is 55min, and second, third polymerization reaction kettle is 45min.Wherein the inner temperature of reaction of each polymerization reaction kettle is followed successively by 35 ℃, 42 ℃ and 50 ℃.In technological process, the rotating speed of whisking appliance is 50rpm.
According to present embodiment, the transformation efficiency of isoprene monomer in the exit of first polymerization reaction kettle is 68wt%, and is 98.5wt% at the final transformation efficiency in the exit of trimerization reaction kettle.Analyze the cis-1 of confirming resulting rare-earth isoprene rubber product in the present embodiment, 4-configuration content, number-average molecular weight and MWD coefficient, its result lists in the table 1.
Embodiment 2:
The diameter of the oblique leaf disc turbine type stirring rake 13 of four in the said whisking appliance is 1/4 of a polymerization reaction kettle diameter, and other parts are identical with embodiment 1.
According to present embodiment, the transformation efficiency of isoprene monomer in the first reaction kettle exit is 67wt%, and the final transformation efficiency in last still exit is 96wt%.The mass analysis of the rare-earth isoprene rubber product that is obtained after reaction is accomplished is as a result in the row following table 1.
Embodiment 3:
The diameter of the oblique leaf disc turbine type stirring rake 13 of four in the said whisking appliance is 2/5 of a polymerization reaction kettle diameter, and other parts are identical with embodiment 1.
According to this embodiment, the transformation efficiency of isoprene monomer in the first reaction kettle exit is 68wt%, and the final transformation efficiency in last still exit is 98wt%.The mass analysis result of the rare-earth isoprene rubber product that reaction is obtained after accomplishing lists in the table 1.
Embodiment 4:
The center of the oblique leaf disc turbine type stirring rake 13 of four in the said whisking appliance is 1/5 of its pitch apart from the distance from bottom of two ribbon impellers 12, and other parts are identical with embodiment 1.
According to should embodiment, the transformation efficiency of isoprene monomer in the first reaction kettle exit be 66wt%, and the final transformation efficiency in last still exit is 96wt%.The mass analysis result of the rare-earth isoprene rubber product that reaction is obtained after accomplishing lists in the table 1.
Embodiment 5:
The center of the oblique leaf disc turbine type stirring rake 13 of four in the said whisking appliance is 1/3 of its pitch apart from the distance from bottom of two ribbon impellers 12, and other parts are identical with embodiment 1.
According to present embodiment, the transformation efficiency of isoprene monomer in the first reaction kettle exit is 65wt%, and the final transformation efficiency in last still exit is 95wt%.The mass analysis result of the rare-earth isoprene rubber product that reaction is obtained after accomplishing lists in down in 1.
Comparative Examples 1:
Whisking appliance in the polymerization reaction kettle only keeps two ribbon impellers 12 wherein, removes four oblique leaf disc turbine type stirring rakes 13 of bottom, and other parts are identical with embodiment 1.
According to this Comparative Examples, the transformation efficiency of isoprene monomer in the first reaction kettle exit is 63wt%, and the final transformation efficiency in last still exit is 90wt%.The mass analysis result of the rare-earth isoprene rubber product that reaction is obtained after accomplishing lists in down in 1.
Comparative Examples 2:
Employed catalyst consumption is risen to original 2 times, and other parts are identical with Comparative Examples 1.
According to this Comparative Examples, the transformation efficiency of isoprene monomer in the first reaction kettle exit is 67wt%, and the final transformation efficiency in last still exit is 95wt%.The mass analysis result of the rare-earth isoprene rubber product that reaction is obtained after accomplishing lists in down in 1.
Table 1
Figure BSA00000455009400071
From the foregoing description and Comparative Examples, can find out; Use is carried out the isoprene monomer polyreaction according to the whisking appliance of the utility model; Can make the cis-1 of resulting polyisoprene rubber product, 4-configuration content is obviously higher, and number-average molecular weight is bigger and the MWD coefficient is littler; That is, resulting polyisoprene rubber quality product is better.In addition, also can reduce catalyst consumption when using whisking appliance according to the utility model to carry out the isoprene monomer polymerization, reduce production costs.
Though the utility model is described, under the situation of the scope that does not break away from the utility model, can carries out various improvement and can replace parts wherein to it with equivalent with reference to preferred embodiment.The utility model is not limited to disclosed specific embodiment in the literary composition, but comprises all technical schemes in the scope that falls into claim.

Claims (20)

1. a whisking appliance that is used in the polymerization reaction kettle for preparing rare-earth isoprene rubber comprises stir shaft and is installed in the two ribbon impellers on the said stir shaft, wherein, four oblique leaf disc turbine type stirring rakes has been installed also on said stir shaft.
2. whisking appliance according to claim 1 is characterized in that, the diameter of said four oblique leaf disc turbine type stirring rakes and the diameter ratio of polymerization reaction kettle are 1/5-1/2.
3. whisking appliance according to claim 2 is characterized in that, the diameter of said four oblique leaf disc turbine type stirring rakes and the diameter ratio of polymerization reaction kettle are 1/4-2/5.
4. whisking appliance according to claim 3 is characterized in that, the diameter of said four oblique leaf disc turbine type stirring rakes and the diameter ratio of polymerization reaction kettle are 1/3.
5. according to each described whisking appliance in the claim 1 to 4, it is characterized in that the diameter ratio of the width of blade of said four oblique leaf disc turbine type stirring rakes and said four oblique leaf disc turbine type stirring rakes is 1/5-1/4.
6. according to each described whisking appliance in the claim 1 to 4, it is characterized in that the diameter ratio of the depth of blade of said four oblique leaf disc turbine type stirring rakes and said four oblique leaf disc turbine type stirring rakes is 3/20-1/4.
7. whisking appliance according to claim 6 is characterized in that, the diameter ratio of the depth of blade of said four oblique leaf disc turbine type stirring rakes and said four oblique leaf disc turbine type stirring rakes is 1/5.
8. according to each described whisking appliance in the claim 1 to 4, it is characterized in that the blade of said four oblique leaf disc turbine type stirring rakes is seated in the disk place on the said stir shaft with 45.
9. whisking appliance according to claim 8 is characterized in that, said blade is embedded in the said disk in the middle of its height, and the width of embedding is the 1/3-2/3 of its whole blade width.
10. whisking appliance according to claim 9 is characterized in that, the width of said embedding is 1/2 of its whole blade width.
11. whisking appliance according to claim 8 is characterized in that, the diameter ratio of the diameter of said disk and said four oblique leaf disc turbine type stirring rakes is 3/5-4/5.
12. whisking appliance according to claim 11 is characterized in that, the diameter ratio of the diameter of said disk and said four oblique leaf disc turbine type stirring rakes is 3/4.
13., it is characterized in that the diameter of said pair of ribbon impeller and the diameter ratio of polymeric kettle are 90%-98% according to each described whisking appliance in the claim 1 to 4.
14. whisking appliance according to claim 13 is characterized in that, the diameter of said pair of ribbon impeller and the diameter ratio of polymeric kettle are 95%.
15. whisking appliance according to claim 13 is characterized in that, the ribbon width of said pair of ribbon impeller is the 5%-15% of ribbon diameter.
16. whisking appliance according to claim 15 is characterized in that, the ribbon width of said pair of ribbon impeller is 10% of a ribbon diameter.
17. whisking appliance according to claim 15 is characterized in that, the ratio of the pitch of said pair of ribbon impeller and ribbon diameter is 0.5-1.5.
18. whisking appliance according to claim 17 is characterized in that, the ratio of the pitch of said pair of ribbon impeller and ribbon diameter is 1.0.
19., it is characterized in that said four oblique leaf disc turbine type stirring rakes are that the mode of the 1/5-1/3 of pitch is installed on the stir shaft with its center apart from the distance from bottom of two ribbon impellers according to each described whisking appliance in the claim 1 to 4.
20. whisking appliance according to claim 19 is characterized in that, said four oblique leaf disc turbine type stirring rakes are that 1/4 mode of pitch is installed on the stir shaft with its center apart from the distance from bottom of two ribbon impellers.
CN2011200743612U 2011-03-21 2011-03-21 Stirrer Expired - Lifetime CN202124586U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104368289A (en) * 2013-08-13 2015-02-25 苏州华日金菱机械有限公司 Spiral stirrer
CN104629110A (en) * 2013-11-12 2015-05-20 中国石油化工股份有限公司 Masterbatch and preparation method thereof, vulcanized rubber and application thereof
CN107473255A (en) * 2017-08-22 2017-12-15 江苏师范大学 A kind of method for preparing yittrium oxide nanocrystalline powder with four oblique leaf agitator co-precipitation

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104368289A (en) * 2013-08-13 2015-02-25 苏州华日金菱机械有限公司 Spiral stirrer
CN104629110A (en) * 2013-11-12 2015-05-20 中国石油化工股份有限公司 Masterbatch and preparation method thereof, vulcanized rubber and application thereof
CN107473255A (en) * 2017-08-22 2017-12-15 江苏师范大学 A kind of method for preparing yittrium oxide nanocrystalline powder with four oblique leaf agitator co-precipitation

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Granted publication date: 20120125