DE102013103864A1 - Method for conducting high viscous and/or high-filled material e.g. epoxy resin, through segment of feeding line of polymeric product manufacture plant, involves introducing warm gas into segment, and discharging material from segment - Google Patents

Abstract

The method involves introducing warm gas at temperature of 35 Degree Celcius into a segment (14) of a pipeline. A high viscous and/or high-filled material (A) is discharged from the segment of the pipeline. The high viscous and/or high-filled material is transferred from a tank (11) into a mixture station (20). The very viscous material is converted into a polymeric product by the mixture station. The warm gas is introduced before heating by the warm gas by a gas heater (17) preferably an air heater. The air heater is coupled and decoupled by a quick coupling.

Description

The present invention relates to a method for passing a highly viscous and / or highly filled material through a segment of a conduit or for cleaning deposits of a highly viscous and / or highly filled material in a segment of a conduit according to the preamble of claim 1.

When using highly viscous and / or highly filled materials, especially as starting materials in a plant for the production of polymers, the problem arises of impurities adhering to the walls of conduits. These are the result of segregation processes due to the low flow velocities of high-viscosity and / or filler-rich materials. These deposits are included in the next batch of material at a certain level and change the material composition of this material batch, for example the filler content. This altered and incalculable material composition causes problems, for example, in the correct dosage of other substances, such as e.g. Hardeners and catalysts, which can lead to a total uselessness of the end products. The same applies to highly viscous materials in which deposits can completely change the composition of an altered material batch.

The DE 2 332 748 discloses a process in which a reaction is carried out in a tubular reactor. Among other things, an inert gas is introduced. This gas is used to reduce the specific gravity of a viscous mass. The actual discharge takes place through a liquid film on which the viscous mass slides.

The US 3,040,760 A1 describes a double-walled pipe construction. The inner wall forms a pipeline for passing a medium. The inner wall consists of porous material. The outer wall is spaced from the inner wall so as to form an annular cavity extending along the tube axis. In this cavity, so not directly into the conduit which is provided for the medium, a gas is introduced, which penetrates through the porous inner wall and forms an air cushion, on which slides the mass along.

It is therefore an object of the present invention to provide an alternative method which avoids deposits in lines. Additionally or alternatively, the present method can also be used for cleaning lines in which deposits are already present.

The invention solves this problem by a method having the features of claim 1.

• A) Einleiten eines warmen Gases mit einer Temperatur von mindestens 35°C in das Segment der Leitung und
• B) Ableiten des hochviskosen und/oder hochgefüllten Materials aus dem Segment der Leitung.

An inventive method for passing a highly viscous and / or highly filled material through at least one segment of a line or for cleaning deposits of a highly viscous and / or highly filled material in at least one segment of a line comprises the following steps:

• A) introducing a warm gas with a temperature of at least 35 ° C into the segment of the pipe and
• B) discharging the highly viscous and / or highly filled material from the segment of the conduit.

By introducing the warm gas, in particular at a terminal portion of the line segment, the viscosity of the material as a whole is lowered, so that undissolved constituents, such as fillers, are entrained by the increased flow rate of the material in the axial direction and can not settle, thereby the formation of deposits avoided or at least reduced. In addition to mere heating of the material, the introduction of the warm gas also has the effect that the deposits are removed from the inner wall of the conduit and blown out by the increased pressure. Deriving is understood on the one hand to mean the outflow of deposits of the highly viscous and / or highly filled material under the action of a gas pressure. On the other hand, however, it can also happen that by diverting said deposits completely lose contact with the inner wall of the line and are transported in the gas stream. The synergy effects of reducing the viscosity and the simultaneous action of a gas pressure make it possible to clean the line. If a warm gas is introduced into the line already during the passage of the material, the flow rate of the material is increased, so that the formation of deposits is reduced. By introducing the warm gas not only the formation of newer deposits can be avoided, it can be removed even existing deposits. Consequently, the method can also be used for cleaning.

Advantageous embodiments of the invention are the subject of the dependent claims.

In particular, the gas is used exclusively for the transport of the material and the deposits. In the case of debris cleaning, the chemical and / or physical properties of the material of the deposits may change. The Material can be pyrolyzed, for example, during transport.

The introduction always takes place in the axial direction of the tube. The use of further auxiliary media for the mass transfer can advantageously be dispensed with.

• a) einen Tank zur Bereitstellung des hochviskosen Materials,
• b) die Zufuhrleitung zur Überführung des hochviskosen und/oder hochgefüllten Materials von dem Tank in eine Mischstation und
• c) die Mischstation zur Umsetzung des hochviskosen Materials in ein Polymer aufweist.

The above method can be used advantageously in a plant for polymer production, wherein the line is a supply line of a plant, for the production of a polymer, and wherein the plant at least

• a) a tank for providing the high-viscosity material,
• b) the supply line for transferring the highly viscous and / or highly filled material from the tank into a mixing station and
• c) has the mixing station for the implementation of the high-viscosity material in a polymer.

However, the gas is first heated in a gas heater, preferably in a water heater, in particular in an air heater, and then introduced via a gas line and a valve in the system.

For the operating state of the cleaning of the supply line, before the introduction of the hot gas interrupting the supply of highly viscous and / or highly filled material should be made in the supply line. A corresponding interruption can be carried out particularly advantageously by a three-way valve, so that the system from the operating state of the polymer production in the operating state of the cleaning, by introducing the warm gas, can be switched. By introducing the warm gas disassembly of the system is avoided in the operating state of the cleaning, it can be carried out a CIP process, ie a cleaning of the supply line in the assembled state.

In the operating state of the passage of the highly viscous and / or highly filled material through the segment of the supply line, a supply of the high-viscosity and / or highly-filled material into the supply line can take place when the warm gas is introduced. This feed can be continuous. Alternatively, the introduction of the warm gas may be intermittent with the supply of the highly viscous and / or highly filled material into the supply line.

To build up a corresponding gas pressure, it is advantageous if, prior to the introduction of the gas into the gas heater, a compression of the gas, preferably by a compressor, takes place.

An optimized cleaning of the pipe as well as a deposit-free transfer of the highly viscous and / or highly filled material depends on a number of factors. Thus, it is particularly advantageous if the temperature of the warm gas is between 40-100 ° C, preferably 60-95 ° C, particularly preferably 70-90 ° C.

It is also advantageous if the pressure of the warm gas is 2-10 bar, preferably 3-6 bar. Due to the increased pressure, a more optimized blowing out or discharging of the highly viscous and / or highly filled material takes place.

Along the supply line further components of the system, preferably a pump can be arranged. In this case, the segment to be cleaned can take place between the tank and the component, between the components or between the component and the mixing station. In this case, a cleaning of segments of the supply line, which are not directly adjacent to the tank particularly preferred because these segments are not cleanable or conditionable for recirculation of the material.

In principle, the hot gas may be introduced at one end of the conduit, for example via a separate port, and the pollutants of the material may be blown out or discharged at the opposite end of the conduit.

However, it is advantageous in some applications when the conduit has multiple supply ports to introduce hot gas into a segment of the conduit. As a result, the gas can be brought closer to the contaminated areas more targeted and the conduction of the gas can be made more targeted, which can lead to a reduction in the amount of gas to be made available.

It is also advantageous if the conduit has a plurality of discharge ports to permit the purging of the high viscosity and / or highly filled material from the selected segment of the conduit. As a result, a reduction of the contamination segments can be made possible, which are arranged downstream of the selected segment in the flow direction of the warm gas.

It is advantageous if the introduction of the warm gas into the line is pulsating. By the gas pressure surges act in addition to the heat of the gas higher mechanical forces on the impurities than is the case with a continuous gas flow. This allows for improved detachment of the deposits from the inner wall of the conduit with respect to a continuous gas flow.

The blowing out can advantageously be assisted by at least one segment of the duct having a gradient in the direction of flow of the warm gas. Under a blowing is to understand by definition, a flow of the material under the action of a gas pressure and / or a mass transport of the material in a gas stream. When the material flows off, the rate of dilution of the material can be additionally increased by the gradient of the pipe.

The cleaning process has proved to be particularly advantageous in the case of deposits which are formed by a highly viscous and / or highly filled material which contains at least 20% by weight, preferably at least 40% by weight, of one or more epoxy resins. The highly viscose and / or highly filled material may comprise at least 20% by weight, preferably between 30-60% by weight of fillers. The dynamic viscosity of the highly viscous and / or highly filled material is advantageously at least 3500 mPas (at 25 ° C and atmospheric pressure). Such a material may, for example, have stability, even when the conduit is oriented perpendicular to the ground. This means that even with a gradient of 90 °, the deposits remain on the inner wall of the pipe. This applies in particular to materials such as the material Stycast FT2850, Stycast FT5952, RT 675 (Wacker), (Dow Corning) DC3-6651 and DC3-600 according to their material specification at the time of filing (April 2012).

By the method according to the invention for cleaning, the viscosity can be advantageously reduced by introducing the warm gas by at least 300%, preferably at least 600%, more preferably at least 800%, so that a blowing is possible.

Due to the high natural availability, air is preferred as the gas, resulting in a low cost burden in the process. However, it may happen that the respective high-viscosity and / or highly-filled materials are sensitive to oxygen. In these cases, inert gases, especially carbon dioxide or nitrogen are recommended. To distinguish it from water vapor, the air used has an atmospheric humidity of less than 80%, preferably less than 50%.

Hereinafter, an embodiment will be described with reference to the accompanying drawings. It shows:

1 schematic structure of a method according to the invention and

2 Schematic structure of a method according to the prior art.

2 shows in simplified form a plant for the preparation of a polymeric product according to the prior art. In this case, the polymeric product is formed from at least one highly viscous and / or highly filled material.

For the purposes of the present invention, "highly viscous" is to be understood as meaning a material which has at least a viscosity of 2000 mPas (at 45 ° C. and under atmospheric pressure). The viscosity can preferably be determined by the rheometer "Rheostress 1" from Thermo Haake under stated conditions.

For the purposes of the present invention, "highly filled" is to be understood as meaning a material which has at least one filler fraction of at least 20% by weight, preferably 30-60% by weight. Fillers are in this context in particular Al (OH) ₃ . The viscosity can preferably be determined by the abovementioned viscometer of the company Rheometer under stated conditions.

For example, at the temperature of 46 ° C ± 1 ° C and normal pressure, the viscosity of Stycast 2850 averages, for example, 4100 mPas ± 400 mPas. At temperatures of 72 ° C ± 1 ° C the viscosity of Stycast 2850 is on average 1000 mPas ± 200 mPas. At temperatures of 85 ° C ± 1 ° C, the viscosity of Stycast 2850 is on average 600 mPas ± 120 mPas.

2 shows a first tank 1 , which has a first segment 2 a line - designed here as a supply line - for a highly viscous and / or highly filled material with a screw pump 3 connected is. The screw pump 3 is over a second segment of a supply line 4 with a mixer 5 connected. The mixer also has a supply line for the supply of a hardener and / or a catalyst from a storage reservoir 6 on. So far, a highly viscous and / or highly filled material from the first tank 1 over the first segment 2 the supply line of the screw pump 3 fed. To avoid segregation of the fillers and the material or adhesion of the highly viscous material is in the tank 1 arranged a stirrer which keeps the material in motion. Subsequently, the material via the screw pump 3 and the second segment of the supply line 4 in the mixing station or the mixer 5 transferred. It will, as in 2 shown schematically, in the transfer of screw pump 3 to mixers 5 overcome a height difference h1. In the mixing station 5 the material is another component, preferably a catalyst or a Hardening agent from the storage reservoir 6 added and reacted.

This system has proven itself in principle. However, the problem is that the fillers contained in the material or other components of the material settle and as residue in the segments 2 and 4 the supply line or remain in the line. This residue has in particular stability on a vertical plane. To prevent these deposits, the highly filled and / or highly viscous material between the screw pump 3 and the tank 1 circulated, for example by recycling by means of a return line, not shown. However, such a circulation is in the section of the second supply line 4 not possible, so that it comes in this area for depositing fillers on the inner line wall. This results in an inhomogeneous distribution between fillers and material or educt in the metered addition. Thus, it may happen, for example, that the ratio of the metered amount of material, due to the high filler content too small for the amount of metered hardener and catalyst precipitates, resulting in the uselessness of the polymeric product as a whole. In particular, this effect occurs in the preparation of a polymeric product at high concentration differences between the highly viscous and / or highly filled material and the metered hardener or catalyst, preferably provided that the amount of metered hardener and / or catalyst only one tenth of the amount of highly viscous and / or highly filled material, typically at ratios of 100: 8 or 100: 4 - of the highly viscous and / or highly filled material to the hardener or catalyst.

1 shows a plant for the preparation of a polymeric product B, on which the inventive method can be carried out. The system has two operating states. An operating state of the cleaning and an operating state of the production of the polymeric product, including the passage of the highly viscous and / or highly filled material A through a segment of a supply line. This plant has a first tank 11 , a first segment 12 a feed line, an optional unillustrated return line, a screw pump 13 , a second segment 14 the supply line, a third segment 15 a supply line and a mixing station 20 on. Between the second and the third segment 14 . 15 the supply line is a multi-way valve, preferably a three-way valve 17 arranged. From this goes a gas supply 18 and a gas heater 17 from. Before the gas heater is, not shown here, a compressor, a gas tank or a gas cylinder connected. In the gas heater, the gas is heated and with the three-way valve open 17 in the second segment 14 initiated the supply line. In the present case can be selected between the operating state of the cleaning or the passage of the material, wherein when passing through appropriate operation of the three-way valve, the supply of the material takes place intermittently with the introduction of the heated gas. To the mixer 20 , preferably runs a supply line 19 from a storage container 20 for metering in a hardener and / or catalyst C.

The following is the in the in 1 The cleaning procedure described in detail in the attached The application of the method to highly viscous highly filled materials has proved to be particularly advantageous. However, the process may also be applied to other high viscosity, immiscible or high viscosity, separable solid-liquid or liquid-liquid material compositions (eg, a high-viscosity educt with pigment solids).

First, a gas is pressurized to the gas heater via the compressor or gas cylinder 17 fed. The gas is heated. With appropriate circuit of the three-way valve 16 the warm gas gets into the segment 14 introduced the supply line. The viscosity of the deposits of the highly viscous and / or highly filled material located there is lowered in such a way that it becomes flowable. Due to the gas pressure of the gas, the material is subsequently blown out, so that the now flowable deposits via the mixing station 20 can be removed from the plant. In this operating condition no supply of the hardener and / or catalyst takes place 19 and no conversion to the polymer B. In this case, the second segment 14 a slope at an angle α of more than 5 degrees. Due to the slope in particular the plug formation is advantageously prevented. In this case, the slope may particularly preferably fall by 10-45%.

As an alternative to the operating state of the cleaning, the operating state of the production can be realized, in which a passage of a highly viscous and / or highly filled material from the tank 11 in the mixing station 20 is carried out. In this case, the three-way valve is controlled in an intermittent manner so that in a first interval, a supply of material takes place and in a second interval, an introduction to hot gas. This prevents the settling of deposits on the one hand and increases the speed of the material.

After the addition of the hardener and / or catalyst C, the product B can be applied to an electronic component, preferably an electronic circuit. The application of the product may also be a product / educt mixture. This is the Electronic component encapsulated and thus protected from environmental influences and interference. Subsequently, further steps can be taken to allow complete curing of the product.

Preferred highly viscous, in particular highly filled materials are, for example, a highly viscous filler-containing epoxy resin with a filler fraction of between 30 and 60% by weight and a viscosity of 4000-4500 mPas (at 25 ° C. and atmospheric pressure, ie in the range from 1.0 to 1.1 bar). , Preferably, a multi-component epoxy resin having the properties mentioned can also be used. A corresponding product produced by the process can be used as potting material for the encapsulation of electronic components.

By the method according to the invention, the production speed in the production of components with potted electronic elements can be considerably increased, since a complex cleaning of filler deposits can be dispensed with by disassembly of the plant or because this cleaning must be done at least less often. In addition, deposits are formed or even completely avoided by a corresponding passage of the material through a line according to the inventive method only to a reduced extent. This ensures the continuity of the manufacturing process. In addition, fewer rejects are produced, since no impurities remain after the procedure in the interconnections or pipelines

By supplying hot gas in the process according to the invention, the on-site cleaning of the plant can be made possible. Basically, cleaning, such as hot steam cleaning and the like, are known from other areas of life. In the present case, however, it is the removal of deposits of a highly viscous and / or highly filled material, wherein the gas not only cleans in the present case, but initially lowers the viscosity of the educt before it is removed.

The introduction of the warm gas can already already in the first segment 12 the supply line.

In order to capture as much as possible impurities, it is advantageous if the third segment 15 between the last component on the line - in 1 the screw pump 3 - And arranged behind the three-way valve 16 not more than 5% of the length of the second segment 14 having.

A corresponding line can be additionally optimized for the purification or the passage of highly viscous and / or highly filled materials by further constructive means.

For improved cleaning, a line can advantageously additionally have a layer of thermal insulation, preferably in the form of an insulating material. This layer is arranged on the outer wall of the conduit and is preferably an insulating foam. The isolation ensures that the material of the transfer line is also heated to the temperature of the educt. This does not lead to deposits on cool spots on the pipe.

Alternatively or additionally, the temperature of the conduit may be controlled by an external heating arrangement, e.g. be increased by a heating wire.

In addition, the cleaning can be improved by the line has a slope, preferably of at least 5 degrees, more preferably between 10-45 °.

It is also advantageous if the delivery of the hot gas is pulsating. These gas pressure surges and the associated pressure difference, the detachment of contaminants is supported by the inner wall of the tube.

LIST OF REFERENCE NUMBERS

1

 tank

2

 First segment of the supply line

3

 screw pump

4

 Second segment of the supply line

5

 mixing station

11

 tank

12

 First segment of the supply line

13

 screw pump

14

 Second segment of the supply line

15

 Third segment of the supply line

16

 Three-way valve

17

 gas heater

18

 gas supply

19

 reservoir

20

 mixing station

A

 highly viscous and / or highly filled material

B

 polymeric product

C

 Hardener and / or catalyst

α

 Angle of the gradient

QUOTES INCLUDE IN THE DESCRIPTION

This list of the documents listed by the applicant has been generated automatically and is included solely for the better information of the reader. The list is not part of the German patent or utility model application. The DPMA assumes no liability for any errors or omissions.

Cited patent literature

• DE 2332748 [0003]
• US 3040760 A1 [0004]

Claims (22)

Method for passing a highly viscous and / or highly filled material (A) through at least one segment ( 14 ) of a line or for cleaning deposits of a highly viscous and / or highly filled material (A) in at least one segment ( 14 ) of a pipe characterized by the following steps: A) introducing a hot gas at a temperature of at least 35 ° C into the segment ( 14 ) of the line and B) discharging the highly viscous and / or highly filled material (A) from the segment ( 14 ) of the line. A method according to claim 1, characterized in that the line is a supply line of a plant, for the production of a polymeric product (B), wherein the plant at least a) a tank ( 11 b) the supply line for transferring the highly viscous and / or highly filled material (A) from the tank ( 11 ) in a mixing station ( 20 ), and c) the mixing station ( 20 ) for converting the highly viscous material (A) into a polymeric product (B), wherein d) the system is a valve ( 16 ), for introducing a warm gas into the supply line, which previously in a gas heater ( 17 ), preferably in a water heater, in particular in an air heater was heated. A method according to claim 2, characterized in that the system comprises a quick coupling, for coupling and decoupling a gas heater ( 17 ), preferably continuous flow heater, in particular an air heater. A method according to claim 2 or 3, characterized in that the system has at least two operating states, wherein in the operating state of the cleaning of deposits of highly viscous and / or highly filled material (A) in the segment ( 14 ) of the supply line before the introduction of the warm gas, according to step A), an interruption of the supply of the highly viscous and / or highly filled material (A) takes place in the supply line. A method according to claim 2, characterized in that the system has at least two operating states, wherein in the operating state of passing the highly viscous and / or highly filled material (A) through the segment ( 14 ) of the supply line when introducing the warm gas, a supply of highly viscous and / or highly filled material (A) takes place in the supply line. A method according to claim 5, characterized in that the introduction of the warm gas takes place intermittently with the supply of the highly viscous and / or highly filled material (A) in the supply line. Method according to one of the preceding claims, characterized in that after deriving the highly viscous and / or highly filled material (A) from the segment ( 14 ) the line, a reaction of the highly viscous and / or highly filled material (A) with the addition of a curing agent and / or a catalyst (C), wherein the weight fraction of the added curing agent and / or catalyst (C) less than 10% of the weight of the highly viscous and / or highly filled material (A). Method according to one of the preceding claims, characterized in that before the heating of the gas in the gas heater ( 17 ), preferably in a continuous flow heater, in particular in an air heater, a compression of the gas, preferably by a compressor, takes place. Method according to one of the preceding claims, characterized in that the temperature of the warm gas is preferably between 40-100 ° C, preferably 60-95 ° C, particularly preferably 70-90 ° C. Method according to one of the preceding claims, characterized in that the pressure of the hot gas is between 2-10 bar, preferably 3-6 bar. Method according to one of the preceding claims, characterized in that the cleaning of the plant in the CIP process (cleaning in place) is performed. Method according to one of the preceding claims, characterized in that along the supply line further components of the system, preferably a pump ( 13 ), to be ordered. Method according to one of the preceding claims, characterized in that the line comprises a plurality of supply connections to supply hot gas into a selected segment ( 14 ) of the line. Method according to one of the preceding claims, characterized in that the line has a plurality of discharge connections for blowing out the highly viscose and / or highly filled material (A) from the selected segment ( 14 ) of the line for reducing the contamination of the selected segment ( 14 ) in the flow direction of the gas subsequent segments. Method according to one of the preceding claims, characterized in that the introduction of the warm gas is pulsating. Method according to one of the preceding claims, characterized in that for deriving the highly viscous and / or highly filled material at least one segment ( 14 ) the line is used with a slope in the direction of flow of the warm gas. Method according to one of the preceding claims, characterized in that as highly viscous and / or highly filled material (A) a material having at least 20 wt.%, Preferably at least 40 wt.% Of one or more casting resin, preferably epoxy resins, silicones and / or polyurethanes, is used. Method according to one of the preceding claims, characterized in that the high-viscosity and / or highly-filled material (A) is a material having at least 20 wt.%, Preferably between 30-60 wt.% Fillers is used. Method according to one of the preceding claims, characterized in that the dynamic viscosity η of the highly viscous and / or highly filled material (A) is at least 3500 mPas (at 25 ° C and atmospheric pressure). Method according to one of the preceding claims, characterized in that the viscosity is reduced by introducing the warm gas by at least 300%, preferably at least 600%, more preferably at least 800%. Method according to one of the preceding claims, characterized in that the highly viscous and / or highly filled material Stycast FT2850, Stycast FT5952, RT 675 (Wacker), DC3-6651 and DC3-600 (Dow Corning) is used. Method according to one of the preceding claims, characterized in that it is the gas is an inert gas or air.

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