Method and system for polymerizing acrylates

Abstract

The invention relates to a method for polymerizing acrylates using a reactor (50). Reaction heat produced in the reactor (50) is discharged via a boiling cooler (40) in that gaseous vapors produced in the reactor (50) are supplied to the boiling cooler (40), and condensed vapors are returned to the reactor (50) from the boiling cooler (40). At least one component containing acrylate is at least partly added via the boiling cooler (40) and reaches the reactor (50) via the boiling cooler (40). The invention additionally relates to a system for polymerizing an acrylate, comprising a reactor (50) and a boiling cooler (40) for discharging reaction heat produced in the reactor (50). The boiling cooler (40) has at least one filling opening (46) for supplying at least one component containing acrylate.

Claims

1. A process for polymerizing acrylates by a reactor, where heat of reaction arising in the reactor is removed by an evaporative cooler by feeding gaseous vapor formed in the reactor to the evaporative cooler and recirculating condensed vapor from the evaporative cooler to the reactor, wherein at least one component containing acrylate is introduced at least partly via the evaporative cooler and goes via the evaporative cooler into the reactor, wherein a reduced pressure is generated in the reactor, wherein a reduced pressure compared to atmospheric pressure prevails in the reactor during the polymerization of the acrylate.

2. The process of claim 1, wherein the at least one component contains butyl acrylate.

3. The process of claim 1, wherein a further component containing a monomer having two double bonds is at least partly introduced into the evaporative cooler.

4. The process of claim 1, wherein the at least one component is at least partly introduced from above through a cap of the evaporative cooler.

5. The process of claim 1, wherein the at least one component is at least partly introduced from above into a plurality of vertical tubes of the evaporative cooler.

6. The process of claim 1, wherein the reactor is evacuated through the evaporative cooler by a vacuum pump via a subatmospheric pressure conduit.

7. The process of claim 1, wherein the polymerization of the acrylate is carried out as discontinuous process in the reactor.

8. The process of claim 1, wherein water is introduced into the evaporative cooler.

9. The process as claimed in claim 8, wherein the water is introduced at the same time as the at least one component.

10. The process of claim 8, wherein the water is introduced at a time after the at least one component.

11. The process of claim 1, wherein the at least one component is partly introduced directly into the reactor.

12. The process of claim 1, wherein a reduced pressure in the range from 150 mbar to 350 mbar is generated in the reactor.

13. A system for polymerizing acrylates, comprising a reactor, and an evaporative cooler for removing heat of reaction arising in the reactor, wherein the evaporative cooler has at least one feed opening for introducing at least one component containing acrylate, wherein the reactor can be evacuated through the evaporative cooler by a vacuum pump in order to generate a required subatmospheric pressure in the range from 150 mbar to 350 mbar in the reactor, where a subatmospheric pressure conduit is connected to the vacuum pump and is joined to a three-way valve and the three-way valve is connected by a suction conduit to a cap of the evaporative cooler and by a bypass conduit to a lower region of the evaporative cooler, which region is arranged opposite the cap and adjacent to the reactor.

14. The system of claim 13, wherein the at least one feed opening is arranged in a cap of the evaporative cooler.

15. The system of claim 14, wherein nozzles are arranged in the cap in such a way that the component introduced through the at least one feed opening is distributed from above over vertical tubes of the evaporative cooler.

16. The system of claim 13, wherein the reactor and the evaporative cooler are arranged in such a way that vapor formed in the reactor ascends against the force of gravity into the evaporative cooler and that vapor condensed in the evaporative cooler flows together with the at least one component under the force of gravity into the reactor.

Description

BRIEF DESCRIPTION OF THE DRAWING

(1) The figure shows a schematic sectional view of a system for polymerizing an acrylate.

(2) A schematic sectional view of a system 10 for polymerizing an acrylate composed of at least one component is depicted in the figure. The system 10 serves, in particular but not exclusively, for producing acrylate rubber, in particular butyl acrylate rubber. The system 10 comprises a reactor 50. A polymerization of monomers fed in takes place in the reactor 50. A stirrer 52 is arranged within the reactor 50. The stirrer 52 can be driven rotationally by means of an electric motor which is not shown here. Other types of reactors 50 in which a polymerization of monomers fed in can take place can also be used.

(3) A feed conduit 31 is connected to the reactor 50. The feed conduit 31 serves for introducing materials directly into the reactor 50. Materials which can be introduced directly into the reactor 50 via the feed conduit 31 include, in particular, water, an emulsifier and an initiator. However, components (monomers) for producing the acrylate rubber, which contain, in particular, the above-described monomers, can also partly be introduced directly into the reactor 50 via the feed conduit 31.

(4) Furthermore, an offtake conduit 38 is connected to the reactor 50. Acrylate rubber produced in the reactor 50 can be taken off from the reactor 50 and the system 10 by means of the offtake conduit 38.

(5) The system 10 further comprises an evaporative cooler 40. The evaporative cooler 40 serves for removing heat of reaction arising in the polymerization in the reactor 50. The evaporative cooler 40 is in the present case configured as shell-and-tube heat exchanger and comprises a plurality of vertical tubes 44. The evaporative cooler 40 is closed at the top, i.e. at an end facing away from the ground, by a cap 42. Furthermore, the evaporative cooler 40 comprises a coolant inlet which is not shown here and a coolant outlet which is likewise not shown here.

(6) The reactor 50 is connected to the evaporative cooler 40 in such a way that the heat of reaction arising in the polymerization in the reactor 50 can be removed by means of the evaporative cooler 40. Here, gaseous vapor formed in the reactor 50 is fed to the evaporative cooler 40 and condensed vapor from the evaporative cooler 40 flows back into the reactor 50.

(7) Within the evaporative cooler 40, the gaseous vapor formed in the reactor 50 ascends in the vertical tubes 44. A coolant flows around the tubes 44. The coolant is fed to the evaporative cooler 40 through the coolant inlet, flows around the vertical tubes 44 and exits again from the evaporative cooler 40 through the coolant outlet. Here, the coolant cools the tubes 44 and also vapor from the reactor 50 which is present therein. As a result, the vapor condenses and the condensed vapor flows back into the reactor 50.

(8) One or more feed openings 46 are arranged in the cap 42 of the evaporative cooler 40. The feed openings 46 in the cap 42 of the evaporative cooler 40 serve for the introduction of materials, in particular components for producing the acrylate rubber, which contain, in particular, monomers, into the evaporative cooler 40. Furthermore, a plurality of nozzles 48 are provided in the cap 42 of the evaporative cooler 40. The nozzles 48 are connected to the feed openings 46. Materials which are introduced through the feed openings 46 into the cap 42 of the evaporative cooler 40 thus go to the nozzle 48 in the cap 42 of the evaporative cooler 40.

(9) The nozzles 48 are arranged in the cap 42 of the evaporative cooler 40 in such a way that materials which are introduced through the feed openings 46 into the evaporative cooler 40 are distributed from above over the vertical tubes 44 of the evaporative cooler 40. The materials introduced through the feed openings 46 into the evaporative cooler 40 thus flow under the force of gravity into the vertical tubes 44 of the evaporative cooler 40, in which the vapor from the reactor 50 condenses.

(10) A feed conduit 32 is connected to the cap 42 of the evaporative cooler 40. The feed conduit 32 serves for introducing materials into the evaporative cooler 40. The materials introduced into the evaporative cooler 40 via the feed conduit 32 include, in particular, components for producing the acrylate rubber, which contain, in particular, monomers. However, water can also be fed via the feed conduit 32 into the evaporative cooler 40.

(11) The feed conduit 32 of the evaporative cooler 40 is connected to the feed openings 46 arranged in the cap 42 of the evaporative cooler 40. Materials which are introduced via the feed conduit 32 thus go through the feed openings 46 to the nozzles 48 in the cap 42 of the evaporative cooler 40 and from there into the vertical tubes 44.

(12) The reactor 50 can be evacuated through the evaporative cooler 40 by means of a vacuum pump which is not shown here in order to generate a required subatmospheric pressure in the range from 150 mbar to 350 mbar in the reactor 50. A subatmospheric pressure conduit 35 is connected to the vacuum pump and is joined to a three-way valve 33.

(13) The three-way valve 33 is on the one hand connected by means of a suction conduit 36 to the cap 42 of the evaporative cooler 40. The three-way valve 33 is also connected by means of a bypass conduit 34 to a lower region of the evaporative cooler 40, which region is arranged opposite the cap 42 and adjacent to the reactor 50.

(14) Depending on the setting of the three-way valve 33, the reactor 50 can thus be evacuated by the vacuum pump via the suction conduit 36 and the subatmospheric pressure conduit 35 or via the bypass conduit 34 and the subatmospheric pressure conduit 35.

(15) The feed conduit 32, the feed openings 46 and the nozzles 48 of the evaporative cooler 40 are arranged in the cap 42 in such a way that materials fed in are not sucked in and carried into the suction conduit 36 by the subatmospheric pressure generated by the vacuum pump.

(16) At the beginning of the polymerization, in particular for producing acrylate rubber, water, an emulsifier and an initiator are firstly fed into the reactor 50 via the feed conduit 31. A component for producing acrylate rubber, which contains, in particular, butyl acrylate as monomer, can also be fed directly into the reactor 50 via the feed conduit 31. Likewise, a further monomer component as described above, for example the (poly)functional crosslinking monomer, can be fed directly into the reactor 50 via the feed conduit 31.

(17) In the reactor 50, a polymerization of the monomers fed in, in particular an emulsion polymerization, takes place while stirring by means of the stirrer 52. Heat of reaction arises in the polymerization. The heat of reaction results in gaseous vapor ascending from the reactor 50 into the evaporative cooler 40. The gaseous vapor formed in the reactor 50 ascends in the vertical tubes 44 of the evaporative cooler 40 and is cooled there. As a result, the vapor condenses and the condensed vapor flows back into the reactor 50.

(18) At least one component introduced via the feed conduit 32 into the evaporative cooler 40 contains butyl acrylate and is present in liquid form. A further component for producing acrylate rubber, which preferably contains a monomer having two double bonds, can additionally be introduced via the feed conduit 32 into the evaporative cooler 40.

(19) Said materials are introduced via the feed openings 46 in the cap 42 of the evaporative cooler 40 into the evaporative cooler 40. The materials are distributed by means of the nozzles 48 in the cap 42 of the evaporative cooler 40 over the vertical tubes 44 of the evaporative cooler 40. Here, the materials flow from the top under the force of gravity into the vertical tubes 44 of the evaporative cooler 40.

(20) Due to the heat of reaction which arises as a result of the polymerization in the reactor 50, gaseous vapor also ascends against the force of gravity from the reactor 50 into the vertical tubes 44 of the evaporative cooler 40. There, the vapor is cooled and condenses. Mixing of the condensed vapor with the materials which are introduced from above under the force of gravity into the vertical tubes 44 of the evaporative cooler 40 takes place. The condensed vapor subsequently flows together with the materials introduced into the evaporative cooler 40 under the force of gravity back into the reactor 50.

(21) During the polymerization of the acrylates as described here, a reduced pressure compared to atmospheric pressure prevails in the reactor 50. The pressure within the reactor 50 is in the range from 150 mbar to 350 mbar, preferably from 200 mbar to 300 mbar, in particular about 250 mbar.

(22) The process described here for polymerizing an acrylate is based on a discontinuous procedure. Water, emulsifier and initiator are firstly introduced via the feed conduit 31 into the reactor 50. After the required subatmospheric reaction pressure and the necessary reaction temperature have been attained, the introduction of the components containing monomers is commenced. The introduction of the components is effected, at least in the final phase of the polymerization, at least partly via the feed conduit 32 and the evaporative cooler 40. The polymerization commences in the reactor 50 shortly after commencement of the introduction of the required components. After the end of the introduction, the polymerization is continued until a conversion of the monomers of, at least approximately, 100% has been attained.

(23) The acrylate rubber produced is, optionally after grafting, taken off in its entirety, and thus discontinuously, from the reactor 50, and thus also from the system 10 through the offtake conduit 38 after the polymerization in the reactor 50 is complete. After subsequent cleaning of the reactor 50, a further polymerization of an acrylate to produce acrylate rubber takes place as discontinuous process. Such a discontinuous process is also referred to as batch process or charge process.

(24) The invention is explained further by means of the examples and claims.

(25) In a process known from the prior art for producing acrylate rubber (based on butyl acrylate), the components are exclusively introduced directly into the reactor 50. The water is also introduced exclusively directly into the reactor 50. The acrylate rubber produced is taken off batchwise. After a number of months (e.g. 6-9 months) up to one year, so much polymer has been formed in the evaporative cooler 40 that removal of heat via the evaporative cooler 40 is hindered. There is frequently an operating time in the range from six months to one year.

(26) In an experiment on the production of acrylate rubber (based on butyl acrylate) by means of the process of the invention in a system 10 according to the invention, the components are introduced directly into the reactor 50 only in the start-up phase and are subsequently introduced partly via the evaporative cooler 40. The water is exclusively introduced directly into the reactor 50. The acrylate rubber produced is taken off batchwise.

(27) In the present case, it took over eighteen months until so much polymer had formed in the evaporative cooler 40 that the removal of heat by the evaporative cooler 40 had been significantly hindered. An operating time of over eighteen months was thus obtained.

(28) In a further experiment on the production of acrylate rubber (based on butyl acrylate), the components are exclusively introduced directly into the reactor 50. However, the water is partly introduced via the evaporative cooler 40. The acrylate rubber produced is taken off batchwise.

(29) In the present case, it took over fourteen months until so much polymer had been formed in the evaporative cooler 40 that the removal of heat by the evaporative cooler 40 had been significantly hindered. An operating time of over fourteen months was thus obtained. The operating time has thus been increased by at least two months.

(30) The hindering of the removal of heat is made apparent, in particular, by a deterioration in the pressure control and a deterioration in the temperature control. The causes are usually a blockage in the tubes 44 of the evaporative cooler. As prophylaxis, appropriate monitoring can be carried out at regular intervals, for example every six months. For the purposes of such monitoring, the cap 42 of the evaporative cooler 40 is, for example, taken off and the tubes 44 of the evaporative cooler 40 are examined.

(31) When the process known from the prior art is used for producing acrylate rubber, it is frequently the case that about 20% of the tubes 44 of the evaporative cooler 40 have blockages after a time of only from six to twelve months.

(32) When the process of the invention is used for producing acrylate rubber, the tubes 44 have only a slight coating after a time of twelve months and only after a time of eighteen months do about 10% to 20% of the tubes 44 of the evaporative cooler 40 have blockages.

LIST OF REFERENCE NUMERALS

(33) 10 System 31 Feed conduit 32 Feed conduit 33 Three-way valve 34 Bypass conduit 35 Subatmospheric pressure conduit 36 Suction conduit 38 Offtake conduit 40 Evaporative cooler 42 Cap 44 Tube 46 Feed opening 48 Nozzle 50 Reactor 52 Stirrer