专利摘要:
A reactor for carrying out polymerizations in systems with high concentration of polymer is constituted by a cylindrical body (1) having vertical axis with upper and lower heads; in correspondence of a generatrix of the cylinder an opening (2) with vertical-axis is provided, which puts the interior of the cylinder in communication with the body (3) of an extruder, it too with vertical axis, and solid with the reactor.
公开号:SU1715197A3
申请号:SU4027740
申请日:1986-06-03
公开日:1992-02-23
发明作者:Гордини Сильвано
申请人:Эникем Эластомери, С.П.А. (Фирма);
IPC主号:
专利说明:

The invention relates to reaction vessels used for carrying out polymerization in systems with a high concentration of polymer.
The aim of the invention is to improve the heat removal and homogenization of the reaction mixture during the polymerization of butadiene.
FIG. 1 shows the reaction apparatus, a general view. Cross section; in FIG. 2, the same prodyl section: in FIG. 3 paddle stirrers.
The catalytic polymerization reaction apparatus contains a cylindrical vertical housing 1 with a lid 2 and a bottom 3, an extruder 4 with an extrusion chamber in communication with the bottom 3 of the apparatus, and means for introducing the monomer (or monomer and solvent) and catalyst into the housing 1 and removing polymer from the housing 1. The means for introducing the monomer is made in the form of a nozzle 5, and the means for unloading polymerizate from the housing 1 is made in the form of an exhaust nozzle 6 and ensures the release of the polymer in the form of a concentrated solution in the monomer (pax monomer) silt in the possible mixture thereof with a solvent.
The reaction apparatus has an outlet nozzle 7 for Evaporating reaction components in order to remove the heat of reaction or vapors of the same monomer in the case of block polymerization for temperature control. R | the stock unit is also equipped with a vertical agitator with an njpiH shaft placed in the housing 1, to which one or more levers 8 and
oblique blades 9 on it, having a taper from top to bottom in order to exert axial pressure on the lower part of the reaction apparatus, depending on the direction of rotation of the agitator.
The housing 1 is made with vertical blades 10 from the bottom 3 to the cover 2 located between the blades 9 of the agitator. The agitator shaft 8 has an outer jacket 11 formed from a monolithic tube with a lower head to eliminate the Weisenbert effect, which can occur if the shaft 8 rotates in contact with the reaction medium.
The catalyst inlet means is made in the form of a nozzle 12 located adjacent to the jacket 11 of the shaft 8. The extruder 4 is integral with the housing 1 and communicated with it through the hole 13 with a vertical axis, and the means for introducing the catalyst are placed in the bottom 3 of the housing 1 near the shaft 8 agitators.
Extruder A can be single-screw or double-screw, and the characteristics of the screws are such as to ensure the transport zone in accordance with the release of the polymer from the apparatus, therefore this zone is at least equal to the length of the hole 13. The measuring apparatus also provides for measuring temperature , the maximum level of the reaction system, etc. The reaction apparatus can be used to carry out any polymerization in systems with a high polymer concentration of up to 60 wt.% And higher.
The reaction apparatus operates as follows.
Monomer or monomer with a solvent is loaded into the body 1 of the apparatus through the nozzle 5, and through the nozzle 12 the catalyst used in the polymerization reaction is fed. The reaction mass is stirred under certain conditions for some time. The polymer layer with the swollen monomer under the equilibrium conditions (solid phase) is maintained in the lowermost part of the reaction apparatus, since the blades 9 of the stirrer create the effect of axial downward pressure.
The apparatus also contains a monomer layer in which a negligible amount of polymer is dissolved, and in the upper part of the housing 1 there is a gas layer that is discharged through the exhaust nozzle 7, while the polymer is released through the exhaust nozzle 6 by transporting the polymer through the hole 13 and the extruder 4 .
Example. The test was carried out in accordance with the continuous method by using a reaction apparatus having an internal diameter of 250 mm and
blades 300 mm in height, equipped with two sets of three rotating blades and three sets of two stationary blades. During the test, butadiene polymerized in the presence of
0 solvent as a result of using a neodymium-based catalyst that meets the following definitions: at least one neodymium compound is selected from oxide, alkoxides, phenates or
5 neodymium carboxylates or mixtures of this with other components of rare-earth elements: at least one organic compound containing (alcohol or feiol) hydroxyl groups or
0 carboxyl groups selected from alcohols, phenolic and carboxylic acids with POSSIBLE.M addition of water; at least one organometallic compound of aluminum or its corresponding hydrate derivatives, at least one halogenated compound selected from secondary or tertiary alkyl halides. aryl or alkylaryl halides, halides of organic acids, metal or organometallic halides, hydrogen halides, and halogens.
In particular, it is used in a composition prepared as follows.
In a vessel with a capacity of 5 liters. equipped with a stirrer and heat exchange system, in a nitrogen atmosphere was loaded: 220 g (0.62 mol) of neodymium oxide (NdaOa) at 95%; 945 g (3.8
0 mol) of naphthenic acid with an acidity number of 230: 180 g (1.9 mol) of tert.butyl chloride at 98%, 2.8 kg of vaseline oil: 10 ml of an aqueous solution of HCl at 37% by weight. The mixture was stirred inside the vessel.
5 in a nitrogen atmosphere at 60 ° C for 3 hours. At the end of this period, an oil-like mixture was obtained.
The mixture thus obtained was loaded into a 120 l vessel equipped with
0 stirrer. 50 l of a solution containing 0.8 mol / l of aluminum diisobutyl monohydride in vaseline oil was also loaded into the same vessel.
The reaction mass was mixed in
5 atmosphere of nitrogen at room temperature (about 20 ° C) for 2 hours.
At the end of this time period, a catalytic solution was obtained which contained the following concentrations relative to neodymium, aluminum, and chlorine: neoIM - 0; 023 g-atom / l; aluminum - 0.74 gatom / l; chlorine — 0.034 g-atom / l, which (solution) was used in the polymerization.
Various production capacities were tested in the range of 4–20 kg / h of polymer by varying the millimeter speed of 20–80 rpm, while the temperature (60 ° C) and the extruder unloading rate (80 g / min) were kept constant.
A typical course of operation corresponds to the following conditions. Supplied butadiene is 55 kg / h, butadiene evaporates and returns to the cycle after condensation 35 kg / h, the catalyst feed corresponds to 8 mm / h of neodymium, the resulting product 11 kg / h of polymer, polymer viscosity according to Muney, 41 ± 2, the polymer concentration at release from the extruder is about 62%.
Polybutadiene is insoluble in monomer. Under constant conditions, starting from the bottom, the following situation is established inside the reactor.
The polymer layer with the swollen monomer under the equilibrium conditions (solid phase) is maintained in the lowest part of the reaction apparatus, because the agitator blades create the effect of axial downward pressure. The monomer layer in which the neglected amount of polymer is dissolved is the gas upper layer.
The catalyst, supplied adjacent to the shaft jacket, results in a solid phase uniformly distributed inside, surrounding the same shirt, due to the effect produced by the rotating blade.
权利要求:
Claims (1)
[1]
A reaction apparatus for catalytic polymerization in systems with a high polymer concentration, comprising a vertical body with a lid and a bottom, an extruder with an extrusion chamber communicated with the bottom of the body, and means for introducing monomer and catalyst and discharging the polymerizate, characterized in that in order to improve the heat exchange and homogenize the reaction mixture during the polymerization process of butadiene, it is equipped with a vertical stirrer disposed in the housing with a drive shaft and bevel blades on it, with this m case is made with vertical blades from the bottom to the lid, located between the stirrer blades, the extruder is formed integrally with the housing, and means for introducing a catalyst arranged in the housing near the bottom of the agitator shaft.
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figure 1
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法律状态:
2006-12-27| REG| Reference to a code of a succession state|Ref country code: RU Ref legal event code: MM4A Effective date: 20050604 |
优先权:
申请号 | 申请日 | 专利标题
IT21040/85A|IT1186731B|1985-06-05|1985-06-05|POLYMERIZATION REACTOR IN CONCENTRATED SYSTEMS|
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