• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
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    • 专利摘要:

    公开号:SU957771A3
    申请号:SU802882349
    申请日:1980-02-18
    公开日:1982-09-07
    发明作者:Рудольф Мейер Клаус；Гейнц Хорнунг Карл；Фельдманн Райнер；Смигерски Ганс-Юрген
    申请人:Хемише Верке Хюльс Аг (Фирма)；
    IPC主号:
    专利说明:

    The mixture of polyamide and ethanol is placed in a kettle with a stirrer and a heating jacket and heated to the dissolving temperature between 130 and preferably 140 + 2 ° C. Heating can be carried out with a coolant in a jacket or when using a large-volume reactor, preferably low or high pressure steam. The stirring speed during dissolution does not affect the particle size distribution. The solution is then brought to a precipitation temperature which is in the range of 100–125 ° C. preferably between 120 and. The temperature to be deposited depends on the size of the reactor, since as the reactor increases, the heat exchange surface per unit volume of the deposited heat is reduced. The process of cooling to temperature can be carried out by distilling off ethanol, with the cold condensate being taken out to avoid local supercooling (in this case, the distilled amount should be taken into account when calculating the quantitative ratio of polyamide ethanol), or by means of a reverse cooler, with the recycle condensate to avoid . local supercooling of the solution should have a boiling point, or by cooling through the wall, and the coolant must have a temperature which in the extreme case may be slightly lower than the desired precipitation temperature, or by combining both cooling possibilities. When using large reactors, cooling by distillation is preferred. Overcooling the contents of the jacket in comparison with the contents of the reactor can be as much as the medium is less suitable for heat transfer. leads to the formation of deposits on the wall and the adverse effect on the granulometric composition. Upon reaching the desired temperature, the precipitates are discontinued. Further flow of precipitation is beneficial if the internal temperature does not regulate and the deposition is polytropic, with one part emitting heat through the jacket and the reactor lid, while the other part causes a temporary increase in temperature in the reactor 0, . This mode is achieved by constant jacket temperature and constant heat loss through the reactor lid. The heat loss limit through the reactor lid is critical for the deposition rate. The duration of the precipitation process is 2-12 hours, preferably 5-7 hours. In order to avoid boiling into the reactor. an inert gas, preferably nitrogen, is introduced. It is important that during the precipitation a flow is formed by means of a stirrer. To obtain coarse powder for vortex deposition, it is necessary to set the flow at the border of the sedimentation of the deposited polyamide powder, which is achieved by a low number of revolutions of the agitator. To create a constant flow, it is necessary to avoid interfering insert elements. In order to obtain more fine powder, electrostatic field deposition requires turbulent flow, which is achieved by a correspondingly increased number of revolutions of the agitator. All known stirrer designs can be used to carry out the process, preferably paddle mixers with varying speeds. The dimensions of the mixers are in the ratio of the diameter of the reactor: a mixer diameter of 2: 1. At the end of the precipitation, the resulting suspension is cooled through a wall or by distillation and, after decanting or precipitating, the suspension is directly transferred to a dryer. In order to avoid the formation of a coarse-grained product during agglomeration, the drying must be carried out at the beginning of product flowability ((ethanol humidity 20% 1, under reduced pressure and wall temperature below, as well as with gentle mechanical movement, for example, in slow-running paddle dryers or dryers for polymer crumb When the flowability is achieved, mechanical movement can be increased and the temperature in the dryer can be increased above 100 to 150 C. Deposition can be carried out in the presence of such pigments as titanium dioxide, carbon black, Ba S04, ZnS, red cadmium, iron oxide or stabilizers, such as 4-hydroxy-3, 5-di-tert ..- butyl-phenyl propionic acid, hexamethylenediamine bisamine 4-hydroxy-3, 5-di-tert.-butyl- phenyl propionic acid, ester of propionic acid with aliphatic alcohol with 1-18 carbon atoms, tres-alkyl-phenyl-, tris-alkyl-, tris-aryl- or mixed esters of phosphorous acid, the alkyl-radical of which contains 1-16 atoms and is straight or branched. Example 1. 400 kg in the presence of 0.5 wt.% Of phosphoric acid of hydrolytically polymerized polylaurinolactam with a relative viscosity of 1.62, together with 2,200 l of methanol-denatured ethanol (water content of 1 wt.%) In a 3 m paddle equipped with a paddle stirrer ( Volume 3 m, diameter 1600 mm) is heated to 140 s. Then, by distilling off approximately 200 l of ethanol, which is fed into a separate container, the solution is cooled to Simultaneously in a jacket, I set a low-pressure steam with a temperature of 111.5 ° C, and nitrogen is pressed into the solution (2 bar ) and the number of equipment from the safety of the agitator / diameter 800 is reduced to 20 rpm./ min. and the Reynolds number is set to 3000. The temperature inside the actor drops to Ib / s for 2.5 hours, then rises again by 1 hour for 3 hours. With and after 9 hours in general, it switches to the corresponding temperature difference - О, 5®С / h. The resulting suspension is cooled through the jacket before and dried in a paddle dryer (diameter 1376 m at 2 rpm, 200 Torr and temperature in the jacket 90c to a residual moisture content of 0.2%. Measured particle size distribution,% by weight: 40 | To 0.28 80 (U 18 120 (u 79 l & Ofi 100 Example 2. In contrast to example 1, during distillation cooling, the supply of vapor to the reactor jacket is interrupted and the pressure is reduced to atmospheric. Then nitrogen (2 bar) is added to the solution and the number is reduced stirrer speeds up to 20 rpm, and set the Reynolds number to 3000. For 1.5 hours the round drops to, then again within one hour it rises by 0.5 ° C and, after 4.5 hours in general, changes to the corresponding temperature difference. The resulting suspension is treated as in Example 1. The measured particle size distribution, wt.%: 40 (110.3 80 / and 12.1 cl20fU78 160 (U97. I200 | U100 Example 3. 340 kg in the presence of 0.5 Bes.% Of phosphoric acid of hydrolytically polymerized polylaurinolactam, with a relative viscosity of 1.58, together with 2100 l of methanol-denatured ethanol (water content 1.7 wt.%) is heated in the reactor (volume 3 m,. diameter 1600 mm) to 140s. To obra-; 20.4 kg per 160 liters of dispersed TO {. The white pigmented polylaurinolactam solution is cooled by distilling 200 l of ethanol to. At the same time, low-pressure steam lowers the temperature in the jacket to 111.5 ° C. Then nitrogen (2 bar) is pressed onto the contents of the reactor and the blade mixer speed (diameter 800 mm) is lowered to 20 rpm, and the Reynolds number is set to 3000. Within 4 hours, the temperature in the reactor drops to 115.25 ° C, then rises again within 2.5 hours by 0.5 ° C and after a lapse of 9 hours in general, it switches to the corresponding temperature difference of 0.5 C / h. The treatment of the resulting suspension is carried out analogously to example 1. The following particle size distribution is obtained, wt.%: 440 / U0.38 80 / i3.14 120 / i49.3 il60 / U98.26 200 / U100 Example 4. 400 kg in the absence of phosphoric acid hydrolytically polymerized polylaurinolactam with a relative viscosity of 1.46 together with 2,200 liters of methanol denatured with methyl ethyl ketone (water content 1.1 veo.%) in a reactor equipped with a paddle stirrer (volume 3 m, diameter 1600 mm) is heated to. By distilling off approximately 200 l of ethanol, cool the solution to 117 ° C while simultaneously lowering the temperature in the jacket with low-pressure steam to 106.5 s, press nitrogen (2 bar) onto the solution and lower the speed of the paddle stirrer (diameter 800 mm) to 50 rpm. and the Reynolds number is set to 7500. The internal temperature drops within 2 hours to 115, then again within 2 hours it rises again by 1.25 ° C and after 6 hours it generally changes to the corresponding temperature difference. The treatment of the resulting suspension is carried out analogously to example 1. By means of a sieve analysis, the particle size distribution was established, wt.%: Example -5. 275 kg of a mixture from a part without phosphoric acid of a hydrolytically polymerized laurinelactam and a part of a copolyamide with a relative viscosity of 1.68 (80% of laurinelactam units and 20% of caprolactam units) together with 2,200 l of methanol denatured ethanol (water content 1.5 weight,%) equipped with a paddle stirrer reactor (volume J m, diameter 1600 mm) is heated to 140 ° C. The solution is cooled by distilling off approximately 200 liters of ethanol, while lowering the temperature in the jacket with low pressure steam. Pressurized nitrogen (1 bar) to the solution and the speed of the paddle stirrer (digester 800 mm) is set at 50 rpm. , the Reynolds number is set to 20,000. The internal temperature drops within 2 hours, remains constant for 1.5 hours and then switches to the corresponding temperature drop of 1.5 ° C per hour.
    The treatment of the obtained suspension is carried out as in Example 1 with the dryer lowered to the temperature of the jacket. .
    Installed particle size distribution, wt.% 8
    four
    20
    55
    100
    权利要求:
    Claims (1)
    [1]
    1. Patent of Germany No. 2545267, cl. C 08 C 77/02, published 1977.
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    同族专利:
    公开号 | 公开日
    DE2906647C2|1980-12-11|
    AU5571280A|1980-08-28|
    DE2906647B1|1980-04-17|
    EP0014772A1|1980-09-03|
    US4334056A|1982-06-08|
    CA1135448A|1982-11-09|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE2906647A|DE2906647C2|1979-02-21|1979-02-21|Process for the production of powdery coating agents !! based on polyamides with at least 10 aliphatically bonded carbon atoms per carbonamide group|
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