CN110170285A - Synthesize the method and application of devolatilizer and continuous synthesis devolatilization - Google Patents
Synthesize the method and application of devolatilizer and continuous synthesis devolatilization Download PDFInfo
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Abstract
本发明涉及树脂合成反应及脱挥生产技术领域,公开了一种合成脱挥器和连续合成脱挥的方法及应用。该反应器包括合成反应段(1)、脱挥段(2)和真空单元;其中,所述合成反应段(1)用于合成反应;所述脱挥段(2)具有空腔,用于所述合成反应段(1)中合成得到的合成产物的脱挥;所述真空单元用于提供所述合成反应段(1)和所述脱挥段(2)需要的真空度;所述合成反应段(1)的出口与所述脱挥段(2)的入口连接,使得在所述合成反应段(1)中合成得到的合成产物可直接落入所述脱挥段(2)进行脱挥。通过本发明的合成脱挥器实现连续化生产,汽化效率高、热量损失小、设备投资少,维护费用低。
The invention relates to the technical field of resin synthesis reaction and devolatilization production, and discloses a synthetic devolatilizer and a method and application for continuous synthesis and devolatilization. The reactor includes a synthesis reaction section (1), a devolatilization section (2) and a vacuum unit; wherein, the synthesis reaction section (1) is used for synthesis reaction; the devolatilization section (2) has a cavity for Devolatilization of the synthetic product synthesized in the synthesis reaction section (1); the vacuum unit is used to provide the vacuum degree required by the synthesis reaction section (1) and the devolatilization section (2); the synthesis The outlet of the reaction section (1) is connected with the inlet of the devolatilization section (2), so that the synthetic product synthesized in the synthesis reaction section (1) can directly fall into the devolatilization section (2) for devolatization. wave. The synthetic devolatilizer of the invention realizes continuous production, has high vaporization efficiency, small heat loss, low equipment investment and low maintenance cost.
Description
技术领域technical field
本发明涉及树脂合成反应及脱挥生产技术领域,具体涉及一种合成脱挥器和连续合成脱挥的方法及应用。The invention relates to the technical field of resin synthesis reaction and devolatilization production, in particular to a synthetic devolatilizer and a method and application for continuous synthesis and devolatilization.
背景技术Background technique
当前的树脂合成反应及脱除挥发性溶剂等生产技术过程中,通常采用先将原料送至反应釜中合成粗品树脂,然后再将含有挥发性溶剂的粗品树脂通过高温泵输送至常压蒸馏釜、常压蒸馏塔、常压脱色釜等设备中,再进一步脱挥、脱色。但上述树脂合成反应、溶剂脱除装置均存在不足之处,主要如下:1、单台树脂合成反应釜间歇操作,生产规模小、能耗高;2、后续设计常压蒸馏釜过程为间歇过程,增加了高温介质输送动力消耗,热量损失较大,并且无法满足连续生产树脂产品以及连续脱挥、脱色的要求;3、常压蒸馏塔、常压脱色釜在脱挥、脱色时,汽化效果没有负压状态下汽化效果好,也增加了加热介质热量消耗,并且常压蒸馏塔内塔板易损坏,设备维护费用增大。存在这些问题的原因是目前的技术无法将树脂合成反应与脱除挥发性溶剂、脱色等工艺过程有效的整合在一起,实现连续化单元操作。In the current production technology process such as resin synthesis reaction and removal of volatile solvents, the raw materials are usually sent to the reaction kettle to synthesize the crude resin, and then the crude resin containing the volatile solvent is transported to the atmospheric distillation kettle through a high temperature pump. , atmospheric distillation column, atmospheric pressure decolorization kettle and other equipment, and then further devolatilization and decolorization. However, the above-mentioned resin synthesis reaction and solvent removal device all have shortcomings, which are mainly as follows: 1. A single resin synthesis reactor operates intermittently, with small production scale and high energy consumption; 2. The subsequent design of the atmospheric distillation still process is a batch process , which increases the power consumption of high-temperature medium transportation, and the heat loss is large, and it cannot meet the requirements of continuous production of resin products and continuous devolatilization and decolorization; 3. Atmospheric pressure distillation towers and atmospheric pressure decolorization kettles in the process of devolatilization and decolorization, the vaporization effect Without negative pressure, the vaporization effect is good, and the heat consumption of the heating medium is also increased, and the trays in the atmospheric distillation column are easily damaged, and the equipment maintenance cost is increased. The reason for these problems is that the current technology cannot effectively integrate the resin synthesis reaction with the removal of volatile solvents, decolorization and other processes to achieve continuous unit operation.
发明内容SUMMARY OF THE INVENTION
本发明的目的是为了克服现有技术存在的树脂合成脱挥无法连续进行等的问题,提供一种连续化生产、汽化效率高、热量损失小,设备投资少,维护费用低的新型合成脱挥器和连续合成脱挥的方法。The purpose of the present invention is to overcome the problems of the prior art that the resin synthesis devolatilization cannot be carried out continuously, etc., and provides a novel synthetic devolatilization with continuous production, high vaporization efficiency, little heat loss, less equipment investment and low maintenance costs. A method of devolatilization for continuous synthesis and continuous synthesis.
为了实现上述目的,本发明一方面提供一种合成脱挥器,该反应器包括合成反应段、脱挥段和真空单元;In order to achieve the above object, one aspect of the present invention provides a synthesis devolatilizer, the reactor includes a synthesis reaction section, a devolatilization section and a vacuum unit;
其中,所述合成反应段用于合成反应;Wherein, the synthesis reaction section is used for synthesis reaction;
所述脱挥段具有空腔,用于所述合成反应段中合成得到的合成产物的脱挥;The devolatilization section has a cavity for devolatilization of the synthetic product synthesized in the synthesis reaction section;
所述真空单元用于提供所述合成反应段和所述脱挥段需要的真空度;The vacuum unit is used to provide the vacuum degree required by the synthesis reaction section and the devolatilization section;
所述合成反应段设置于所述脱挥段的上方,所述合成反应段的出口与所述脱挥段的入口连接,使得在所述合成反应段中合成得到的合成产物可直接落入所述脱挥段进行脱挥。The synthesis reaction section is arranged above the devolatilization section, and the outlet of the synthesis reaction section is connected with the inlet of the devolatilization section, so that the synthesis product synthesized in the synthesis reaction section can directly fall into the devolatilization section. The devolatilization section is used for devolatilization.
优选地,所述脱挥段的空腔的高度为4m以上,优选为5-7m。Preferably, the height of the cavity of the devolatilization section is above 4m, preferably 5-7m.
优选地,所述脱挥段的上部设置有挥发物出口,所述挥发物出口用于导出脱挥得到的挥发物。Preferably, the upper part of the devolatilization section is provided with a volatiles outlet, and the volatiles outlet is used to lead out the volatiles obtained by devolatilization.
优选地,所述挥发物出口连接一级以上的挥发物分离单元,所述挥发物分离单元包括依次连接的冷凝器和气液分离器;所述冷凝器的挥发物进口连接所述挥发物出口或者所述前一级挥发物分离单元的气液分离器的气相出口,所述冷凝器的挥发物出口连接所述气液分离器的入口。Preferably, the volatiles outlet is connected to one or more volatiles separation units, and the volatiles separation unit includes a condenser and a gas-liquid separator connected in sequence; the volatiles inlet of the condenser is connected to the volatiles outlet or The gas-phase outlet of the gas-liquid separator of the previous-stage volatile matter separation unit, and the volatile matter outlet of the condenser is connected to the inlet of the gas-liquid separator.
优选地,所述挥发物分离单元与所述真空单元连接,所述真空单元用于提供所述合成反应段、所述脱挥段和所述挥发物分离单元需要的真空度。Preferably, the volatiles separation unit is connected to the vacuum unit, and the vacuum unit is used to provide the vacuum degree required by the synthesis reaction section, the devolatilization section and the volatiles separation unit.
优选地,所述脱挥段的外部设置有夹套,所述合成反应段的外部设置有加热单元。Preferably, the outside of the devolatilization section is provided with a jacket, and the outside of the synthesis reaction section is provided with a heating unit.
优选地,所述合成反应段的顶部设置有物料进口,所述脱挥段的底部设置有物料出口。Preferably, the top of the synthesis reaction section is provided with a material inlet, and the bottom of the devolatilization section is provided with a material outlet.
优选地,所述合成反应段和所述脱挥段均设置为圆筒状,所述脱挥段的底部设置为倒锥形。Preferably, both the synthesis reaction section and the devolatilization section are set in a cylindrical shape, and the bottom of the devolatilization section is set in an inverted cone shape.
优选地,所述合成反应段的上部还设置有放空口。Preferably, the upper part of the synthesis reaction section is further provided with a vent.
本发明第二方面提供一种连续合成脱挥的方法,该方法使用上述本发明的合成脱挥器进行,其中,反应物料在所述合成反应段进行合成反应后,得到的合成产物直接落入所述脱挥段进行脱挥。The second aspect of the present invention provides a method for continuous synthesis and devolatilization, the method is carried out using the above-mentioned synthesis devolatilizer of the present invention, wherein after the reaction material is subjected to the synthesis reaction in the synthesis reaction section, the obtained synthesis product directly falls into the The devolatilization section is devolatilized.
优选地,所述合成反应段中的反应条件包括:温度为100-150℃,压力为0.1-0.3MPa;更优选地,温度为105-115℃,压力为0.1-0.2MPa。Preferably, the reaction conditions in the synthesis reaction section include: the temperature is 100-150°C, and the pressure is 0.1-0.3MPa; more preferably, the temperature is 105-115°C, and the pressure is 0.1-0.2MPa.
优选地,所述脱挥段(2)的脱挥条件包括:温度为200-250℃,压力为-0.098~-0.08MPa。Preferably, the devolatilization conditions of the devolatilization section (2) include: a temperature of 200-250° C. and a pressure of -0.098 to -0.08 MPa.
优选地,所述方法用于树脂的合成,更优选地,所述树脂为SMA功能化树脂。Preferably, the method is used for the synthesis of resin, more preferably, the resin is an SMA functionalized resin.
本发明第三方面提供上述本发明的合成脱挥器或者连续合成脱挥的方法在树脂制备中的应用。The third aspect of the present invention provides the application of the above-mentioned synthetic devolatilizer or the method for continuous synthetic devolatilization in resin preparation.
通过上述技术方案,本发明提供的合成脱挥器和连续合成脱挥的方法将合成反应与挥发物脱除过程利用一个装置完成,达到合成与脱挥的有效结合,实现了连续生产,从而降低了设备投资,减少了中间过程中产生的热量损失,提高汽化效率,可解决大规模生产中高效、连续生产的需求。本发明提供的合成脱挥器采用真空环境进料,挥发物脱除过程中采用负压系统逆向汽化,提高汽化效率。Through the above technical solutions, the synthetic devolatilizer and the method for continuous synthetic devolatilization provided by the present invention utilize a single device to complete the synthesis reaction and the volatile removal process, achieve an effective combination of synthesis and devolatilization, realize continuous production, and reduce The equipment investment is reduced, the heat loss generated in the intermediate process is reduced, and the vaporization efficiency is improved, which can meet the needs of high-efficiency and continuous production in large-scale production. The synthetic devolatilizer provided by the invention adopts a vacuum environment for feeding, and a negative pressure system is used for reverse vaporization in the process of removing volatiles, so as to improve the vaporization efficiency.
本发明提供的合成脱挥器通过有效控制树脂合成反应段反应温度、压力将树脂反应与挥发物脱除集成到一个装置内进行,取消了中间设备蒸馏釜、脱色釜、蒸馏塔等设备,降低了设备投资,避免了频繁清洗蒸馏塔器甚至拆卸塔节的维护工作,降低了维护费用。The synthetic devolatilizer provided by the invention integrates the resin reaction and volatiles removal into one device by effectively controlling the reaction temperature and pressure of the resin synthesis reaction section, and eliminates the intermediate equipment such as distillation kettle, decolorization kettle, distillation tower, etc. It saves the equipment investment, avoids the maintenance work of frequent cleaning of the distillation column or even dismantling the column section, and reduces the maintenance cost.
附图说明Description of drawings
图1是本发明的合成脱挥器的结构示意图。Fig. 1 is the structural representation of the synthetic devolatilizer of the present invention.
附图标记说明Description of reference numerals
1、合反应成段 2、脱挥段 3、冷凝器1. Synthesis reaction section 2. Devolatilization section 3. Condenser
4、气液分离器 5、物料进口 6、挥发物出口4. Gas-liquid separator 5. Material inlet 6. Volatile outlet
7、物料出口 8、第一导热油进口 9、第一导热油出口7. Material outlet 8. The first heat transfer oil inlet 9. The first heat transfer oil outlet
10、放空口 11、排净口 12、视镜口10. Vent port 11. Drain port 12. Sight glass port
13、压力表口 14、温度计口 15、夹套温度计口13. Pressure gauge port 14. Thermometer port 15. Jacket thermometer port
16、加强板 17、膨胀节 18、循环液进口16. Reinforcing plate 17. Expansion joint 18. Circulating fluid inlet
19、循环液出口 20、冷凝进口 21、冷凝出口19. Circulating liquid outlet 20. Condensing inlet 21. Condensing outlet
22、气相出口 23、真空口 24、溶剂出口22. Gas outlet 23. Vacuum port 24. Solvent outlet
25、第二导热油进口 26、第二导热油出口25. The second heat transfer oil inlet 26. The second heat transfer oil outlet
具体实施方式Detailed ways
在本文中所披露的范围的端点和任何值都不限于该精确的范围或值,这些范围或值应当理解为包含接近这些范围或值的值。对于数值范围来说,各个范围的端点值之间、各个范围的端点值和单独的点值之间,以及单独的点值之间可以彼此组合而得到一个或多个新的数值范围,这些数值范围应被视为在本文中具体公开。The endpoints of ranges and any values disclosed herein are not limited to the precise ranges or values, which are to be understood to encompass values proximate to those ranges or values. For ranges of values, the endpoints of each range, the endpoints of each range and the individual point values, and the individual point values can be combined with each other to yield one or more new ranges of values that Ranges should be considered as specifically disclosed herein.
本发明提供的合成脱挥器,如图1所示,该反应器包括合成反应段1、脱挥段2和真空单元;其中,所述合成反应段1用于合成反应;所述脱挥段2具有空腔,用于所述合成反应段1中合成得到的合成产物的脱挥;所述真空单元用于提供所述合成反应段1和所述脱挥段2需要的真空度;所述合成反应段1设置于所述脱挥段2的上方,所述合成反应段1的出口与所述脱挥段2的入口连接,使得在所述合成反应段1中合成得到的合成产物可直接落入所述脱挥段2进行脱挥。The synthesis devolatilizer provided by the present invention, as shown in FIG. 1 , the reactor includes a synthesis reaction section 1, a devolatilization section 2 and a vacuum unit; wherein, the synthesis reaction section 1 is used for synthesis reaction; the devolatilization section 2 has a cavity for devolatilization of the synthetic product synthesized in the synthesis reaction section 1; the vacuum unit is used to provide the vacuum degree required by the synthesis reaction section 1 and the devolatilization section 2; the The synthesis reaction section 1 is arranged above the devolatilization section 2, and the outlet of the synthesis reaction section 1 is connected to the inlet of the devolatilization section 2, so that the synthetic product synthesized in the synthesis reaction section 1 can be directly Fall into the devolatilization section 2 for devolatilization.
所述合成反应段1的结构没有特别的限定,只要能够提供合成反应所需的条件即可。优选地,所述合成反应段1的外部设置有加热单元,所述加热单元用于加热合成反应段1,提供合成反应的温度。所述加热单元可以包括设置于所述加热合成反应段1外部的加热管(例如加热排管),所述加热管的下部可以设置有第一导热油进口8,上部可以设置有第一导热油出口9。The structure of the synthesis reaction section 1 is not particularly limited, as long as the conditions required for the synthesis reaction can be provided. Preferably, a heating unit is provided outside the synthesis reaction section 1, and the heating unit is used to heat the synthesis reaction section 1 to provide the temperature of the synthesis reaction. The heating unit may include a heating pipe (such as a heating pipe) disposed outside the heating synthesis reaction section 1, the lower part of the heating pipe may be provided with a first heat transfer oil inlet 8, and the upper part may be provided with a first heat transfer oil. Exit 9.
根据本发明的一个具体的实施方式,所述合成反应段1可以具有管壳结构,其管程用于导入反应物料,壳程用于导入导热油等的加热介质。为了保证合成反应段1的结构稳定性,优选在所述加热单元的中部还设置有膨胀节17。另外,优选所述加热单元的上部还设置有放空口10,所述加热单元的下部还设置有排净口12。According to a specific embodiment of the present invention, the synthesis reaction section 1 may have a shell-and-tube structure, and the tube side is used for introducing reaction materials, and the shell side is used for introducing heating medium such as heat transfer oil. In order to ensure the structural stability of the synthesis reaction section 1 , an expansion joint 17 is preferably provided in the middle of the heating unit. In addition, preferably, the upper part of the heating unit is further provided with a vent 10, and the lower part of the heating unit is also provided with a clean outlet 12.
为了提供合成反应进行的时间,优选地,所述合成反应段1的高度为2-10m,优选为4-8m,更优选为6m。In order to provide the time for the synthesis reaction, preferably, the height of the synthesis reaction section 1 is 2-10m, preferably 4-8m, more preferably 6m.
在本发明中,所述脱挥段2的空腔使得合成产物在下落过程中处于减压加热环境中从而完成脱挥,因而采用本发明的合成脱挥器进行合成和脱挥时,脱挥过程不需要搅拌等即能够达到良好的效果,处理效率高,降低成本。优选地,所述脱挥段2的外部设置有夹套,所述夹套用于加热脱挥段2,提供脱挥需要的温度。所述夹套的上部可以设置有第二导热油出口26,下部可以设置有第二导热油进口25,所述夹套上还可以设置有夹套温度计口15,用于检测夹套内导热油的温度。为了提高脱挥段2的强度,优选在夹套内设置有加强板16,所述加强板16优选等距排列,其间距优选为100-500mm,更优选为200-400mm,例如350mm。In the present invention, the cavity of the devolatilization section 2 makes the synthetic product in a reduced-pressure heating environment during the falling process to complete the devolatilization. Therefore, when the synthetic devolatilizer of the present invention is used for synthesis and devolatilization, the devolatilization is performed. The process can achieve good results without stirring, etc., with high processing efficiency and reduced costs. Preferably, a jacket is provided on the outside of the devolatilization section 2, and the jacket is used to heat the devolatilization section 2 to provide the temperature required for devolatilization. The upper part of the jacket can be provided with a second heat-conducting oil outlet 26, the lower part can be provided with a second heat-conducting oil inlet 25, and the jacket can also be provided with a jacket thermometer port 15 for detecting the heat-conducting oil in the jacket. temperature. In order to improve the strength of the devolatilization section 2, reinforcing plates 16 are preferably arranged in the jacket. The reinforcing plates 16 are preferably arranged at equal distances, and the distance is preferably 100-500mm, more preferably 200-400mm, eg 350mm.
优选地,所述合成反应段1直接连设于所述脱挥段2的上方,例如可以通过法兰连接。并且,为了保证所述合成反应段1和所述脱挥段2的压力,需要使得所述合成反应段1和所述脱挥段2密封连接,例如可以设置橡胶垫圈进行密封。Preferably, the synthesis reaction section 1 is directly connected above the devolatilization section 2, for example, it can be connected by a flange. In addition, in order to ensure the pressure of the synthesis reaction section 1 and the devolatilization section 2, it is necessary to seal the synthesis reaction section 1 and the devolatilization section 2, for example, a rubber gasket can be provided for sealing.
为了提供充足的脱挥时间,优选地,所述脱挥段2的空腔高度为4m以上,优选为5-7m,更优选为5-6.5m。另外,所述脱挥段2的内径优选为1.0-2.0m,更优选为1.2-1.7m,进一步优选为1.5m。In order to provide sufficient devolatilization time, preferably, the cavity height of the devolatilization section 2 is 4m or more, preferably 5-7m, more preferably 5-6.5m. In addition, the inner diameter of the devolatilization section 2 is preferably 1.0-2.0 m, more preferably 1.2-1.7 m, and still more preferably 1.5 m.
根据本发明,优选地,所述合成反应段1的顶部设置有物料进口5,所述脱挥段2的上部设置有挥发物出口6,所述挥发物出口6用于导出脱挥得到的挥发物,所述脱挥段2的底部设置有物料出口7,所述物料出口7用于导出合成脱挥的产物。According to the present invention, preferably, a material inlet 5 is arranged at the top of the synthesis reaction section 1, and a volatile outlet 6 is arranged at the upper part of the devolatilization section 2, and the volatile outlet 6 is used to export the volatilization obtained by devolatilization. The bottom of the devolatilization section 2 is provided with a material outlet 7, and the material outlet 7 is used to derive the synthetic devolatilized product.
另外,所述合成反应段1优选设置为圆筒状,所述脱挥段2优选上部为圆柱形,下部为倒锥形。优选地,脱挥段2的上部高度为3.5-4m,脱挥段2的倒锥形下部顶角为50°-70°,更优选为60°,高度为1-2,更优选为1.5m。并且,所述脱挥段2上部优选采用椭圆封头受压,底部优选设置为倒锥形。优选所述脱挥段2的受压部件采用不锈钢制作。In addition, the synthesis reaction section 1 is preferably arranged in a cylindrical shape, and the devolatilization section 2 preferably has a cylindrical upper portion and an inverted cone-shaped lower portion. Preferably, the upper height of the devolatilization section 2 is 3.5-4m, the lower apex angle of the inverted cone of the devolatilization section 2 is 50°-70°, more preferably 60°, and the height is 1-2, more preferably 1.5m . In addition, the upper part of the devolatilization section 2 is preferably pressed with an elliptical head, and the bottom part is preferably set as an inverted cone. Preferably, the pressure-receiving parts of the devolatilization section 2 are made of stainless steel.
另外,所述脱挥段2的顶部优选设有视镜口12,便于观察树脂生成与脱挥状态,此外根据需要还优选设有温度计口14、压力表口13,所述温度计口14便于检测脱挥段内的温度,所述压力表口13便于检测脱挥段内的压力。所述温度计口14可以设置于脱挥段2的上部和/或下部,所述压力表口13可以设置于脱挥段2的上部。In addition, the top of the devolatilization section 2 is preferably provided with a sight glass port 12, which is convenient for observing the resin generation and devolatilization state. In addition, it is also preferable to have a thermometer port 14 and a pressure gauge port 13 as required, and the thermometer port 14 is convenient for detection. For the temperature in the devolatilization section, the pressure gauge port 13 is convenient for detecting the pressure in the devolatilization section. The thermometer port 14 may be arranged at the upper and/or lower portion of the devolatilization section 2 , and the pressure gauge port 13 may be arranged at the upper portion of the devolatilization section 2 .
根据本发明优选的实施方式,所述挥发物出口6连接一级以上的挥发物分离单元,所述挥发物分离单元包括依次连接的冷凝器3和气液分离器4;所述冷凝器3的挥发物进口20连接所述挥发物出口6或者所述前一级挥发物分离单元的气液分离器4的气相出口22,所述冷凝器3的挥发物出口21连接所述气液分离器4的入口。According to a preferred embodiment of the present invention, the volatile outlet 6 is connected to one or more volatile separation units, and the volatile separation unit includes a condenser 3 and a gas-liquid separator 4 that are connected in sequence; The volatiles inlet 20 is connected to the volatile outlet 6 or the gas-phase outlet 22 of the gas-liquid separator 4 of the previous stage volatiles separation unit, and the volatiles outlet 21 of the condenser 3 is connected to the gas-liquid separator 4 Entrance.
所述冷凝器3和所述气液分离器4均没有特别的限定,能够达到分离脱挥得到的气相中的挥发物即可。优选地,所述冷凝器3的上部设置有冷凝进口20,用于导入挥发物,所述冷凝器3的下部设置有冷凝出口21,用于导出冷凝后的挥发物。所述冷凝器3的外部可以设置冷却结构,例如可以使用夹套式冷却结构,该夹套的下部设置有循环液进口18,上部设置有循环液出口19,从而使得循环水与脱挥得到的气相逆流循环冷却。夹套式冷却结构中使用的循环液只要提供充足的冷却效果即可,可以为水、冷冻水等。所述气液分离器4可以为气液分离罐等,所述气液分离器4的底部设置有溶剂出口24,用于回收溶剂。The condenser 3 and the gas-liquid separator 4 are not particularly limited, as long as the volatiles in the gas phase obtained by devolatilization can be separated. Preferably, the upper part of the condenser 3 is provided with a condensation inlet 20 for introducing volatiles, and the lower part of the condenser 3 is provided with a condensation outlet 21 for leading out the condensed volatiles. The outside of the condenser 3 can be provided with a cooling structure, for example, a jacket type cooling structure can be used. The gas phase is cooled by countercurrent circulation. The circulating liquid used in the jacket cooling structure can be water, chilled water, etc. as long as it provides sufficient cooling effect. The gas-liquid separator 4 can be a gas-liquid separation tank or the like, and the bottom of the gas-liquid separator 4 is provided with a solvent outlet 24 for recovering the solvent.
使用两级挥发物分离单元时,在第一级挥发物分离单元中,气相挥发物经冷凝器3的管程并由壳程通入的循环水冷却,再通过气液分离器4分离液相挥发物;然后,气相部分进入第二级挥发物分离单元中,经冷凝器3管程并由壳程通入的冷冻水深度冷凝,从而有效冷凝挥发物;经第二级挥发物分离单元的冷凝器3冷凝下来的液相挥发物进入回收槽中。When using a two-stage volatiles separation unit, in the first-stage volatiles separation unit, the gas-phase volatiles pass through the tube side of the condenser 3 and are cooled by the circulating water introduced into the shell side, and then pass through the gas-liquid separator 4 to separate the liquid phase. Volatiles; then, the gas phase part enters the second-stage volatiles separation unit, and is deeply condensed by the chilled water introduced into the 3-stage condenser and from the shell-side, so as to effectively condense the volatiles; after the second-stage volatiles separation unit The liquid-phase volatiles condensed by the condenser 3 enter the recovery tank.
根据本发明的一个优选的实施方式,所述挥发物分离单元与所述真空单元连接,所述真空单元用于提供所述合成反应段1、所述脱挥段2和所述挥发物分离单元需要的真空度。在使用多个挥发物分离单元的情况下,将最后一个挥发物分离单元的挥发物出口作为真空孔23,并使所述真空孔23与所述真空单元连接。具体地,所述挥发物分离单元通过真空口23与所述真空单元连接。According to a preferred embodiment of the present invention, the volatile separation unit is connected to the vacuum unit, and the vacuum unit is used to provide the synthesis reaction section 1, the devolatilization section 2 and the volatile separation unit required vacuum. In the case of using multiple volatile separation units, the volatile outlet of the last volatile separation unit is used as the vacuum hole 23, and the vacuum hole 23 is connected to the vacuum unit. Specifically, the volatile separation unit is connected to the vacuum unit through a vacuum port 23 .
本发明第二方面提供一种连续合成脱挥的方法,该方法使用上述本发明的合成脱挥器进行;其中,反应物料在所述合成反应段1进行合成反应后,得到的合成产物直接落入所述脱挥段2进行脱挥。The second aspect of the present invention provides a method for continuous synthesis and devolatilization, which is carried out using the above-mentioned synthesis devolatilizer of the present invention; wherein, after the reaction material undergoes a synthesis reaction in the synthesis reaction section 1, the obtained synthesis product directly drops into the devolatilization section 2 for devolatilization.
在本发明中,经过合成反应段1合成的合成产物进入脱挥段2,含有合成产物的溶液通过脱挥段2外部导热油迅速被加热到脱挥所需的温度,以发泡的状态迅速进入脱挥器中,过量未反应的原料以及不参与反应的溶剂从脱挥器的顶部以气态形式排出,而脱气后熔融态合成产物则落入脱挥器底部,In the present invention, the synthetic product synthesized in the synthesis reaction section 1 enters the devolatilization section 2, and the solution containing the synthetic product is rapidly heated to the temperature required for devolatilization by the external heat-conducting oil of the devolatilization section 2, and rapidly in a foamed state Entering the devolatilizer, the excess unreacted raw materials and the solvent that does not participate in the reaction are discharged from the top of the devolatilizer in gaseous form, and the molten synthetic product after degassing falls into the bottom of the devolatilizer,
本发明的连续合成脱挥的方法可以用于制备树脂等同时需要合成及脱挥的反应中,能够极大提高制备的效率;优选用于合成树脂,更优用于合成SMA功能化树脂。具体地,进行SMA功能化树脂的合成时,反应物料包括:苯乙烯、丙烯睛和乙苯。将所述反应物料导入合成反应段1的流速可以根据合成反应段1的结构和需要的反应时间进行选择,例如可以为0.1-0.3m/s。The method for continuous synthesis and devolatilization of the present invention can be used in the preparation of resins and other reactions that require synthesis and devolatilization at the same time, and can greatly improve the efficiency of preparation; it is preferably used for synthetic resins, and more preferably used for synthesizing SMA functionalized resins. Specifically, when synthesizing the SMA functionalized resin, the reaction materials include: styrene, acrylonitrile and ethylbenzene. The flow rate of introducing the reaction material into the synthesis reaction section 1 can be selected according to the structure of the synthesis reaction section 1 and the required reaction time, for example, it can be 0.1-0.3 m/s.
根据本发明,所述合成反应段1中的反应条件可以包括:温度为100-150℃,压力为0.1-0.3MPa;优选地,温度为100-120℃,压力为0.1-0.3MPa;更优选地,温度为105-115℃,压力为0.1-0.2MPa,例如温度为110±5℃,温度为0.15MPa。根据本发明,所述脱挥段2的脱挥条件可以包括:温度为200-250℃,压力为-0.098~-0.08MPa;优选地,温度为210-230℃,压力为-0.098~-0.09MPa;更优选地,温度为220℃,压力为-0.095MPa。According to the present invention, the reaction conditions in the synthesis reaction section 1 may include: the temperature is 100-150°C, and the pressure is 0.1-0.3MPa; preferably, the temperature is 100-120°C, and the pressure is 0.1-0.3MPa; more preferably Ground, the temperature is 105-115°C, and the pressure is 0.1-0.2MPa, for example, the temperature is 110±5°C, and the temperature is 0.15MPa. According to the present invention, the devolatilization conditions of the devolatilization section 2 may include: the temperature is 200-250°C, and the pressure is -0.098~-0.08MPa; preferably, the temperature is 210-230°C, and the pressure is -0.098~-0.09 MPa; more preferably, the temperature is 220°C and the pressure is -0.095MPa.
为了提供上述反应和脱挥的条件,优选地,所述合成反应段1的加热单元中使用的导热油温度为120-200℃,优选为130-160℃,压力为0.1-0.5Mpa;所述脱挥段2的夹套中的导热油温度为230-320℃,优选为260-280℃,压力为0.05~0.15MPa。In order to provide the conditions for the above reaction and devolatilization, preferably, the temperature of the heat transfer oil used in the heating unit of the synthesis reaction section 1 is 120-200°C, preferably 130-160°C, and the pressure is 0.1-0.5Mpa; the The temperature of the heat transfer oil in the jacket of the devolatilization section 2 is 230-320°C, preferably 260-280°C, and the pressure is 0.05-0.15MPa.
本发明第三方面提供了上述本发明的合成脱挥器或者连续合成脱挥的方法在树脂制备中的应用。The third aspect of the present invention provides the application of the above-mentioned synthetic devolatilizer or the method for continuous synthetic devolatilization in resin preparation.
以下将通过实施例对本发明进行详细描述。The present invention will be described in detail below by means of examples.
采用如图1所示的合成脱挥器制备SMA功能化树脂,该反应器包括合成反应段1、脱挥段2、两级挥发物分离单元和真空单元。The SMA functionalized resin is prepared by a synthetic devolatilizer as shown in Figure 1, the reactor includes a synthesis reaction section 1, a devolatilization section 2, a two-stage volatile separation unit and a vacuum unit.
所述合成反应段1用于合成反应,其外部设置有由加热管构成的加热单元,加热单元的下部设置有第一导热油进口8,上部设置有第一导热油出口9。所述加热单元的上部还设置有放空口10,下部还设置有排净口12。所述加热单元的中部还设置有膨胀节17。The synthesis reaction section 1 is used for synthesis reaction, and is provided with a heating unit composed of a heating tube on the outside. The upper part of the heating unit is also provided with a vent 10 , and the lower part is also provided with a clean outlet 12 . An expansion joint 17 is also provided in the middle of the heating unit.
所述脱挥段2具有空腔,用于所述合成反应段1中合成得到的合成产物的脱挥,空腔的高度为5m,内径为1.5m。所述脱挥段2的外部设置有夹套,所述夹套用于加热脱挥段2,所述夹套的上部设置有用于导入导热油的第二导热油出口26和用于设置温度计的夹套温度计口15,下部设置有用于导出导热油的第二导热油进口25。所述夹套的内部设置有加强板16(水平绕夹套外周设置,纵向间隔350mm)。The devolatilization section 2 has a cavity for devolatilization of the synthetic product synthesized in the synthesis reaction section 1, the height of the cavity is 5m, and the inner diameter is 1.5m. The outside of the devolatilization section 2 is provided with a jacket, the jacket is used to heat the devolatilization section 2, and the upper part of the jacket is provided with a second heat-conducting oil outlet 26 for introducing heat-conducting oil and a clamp for setting a thermometer. The lower part of the thermometer port 15 is provided with a second heat-conducting oil inlet 25 for leading out the heat-conducting oil. The inside of the jacket is provided with a reinforcing plate 16 (which is horizontally arranged around the outer circumference of the jacket, with a longitudinal interval of 350 mm).
所述合成反应段1为圆柱形,所述脱挥段2的上部为圆柱形(内高3.5m),下部为倒锥形(内高3.5m,顶角60°),所述合成反应段1和所述脱挥段2上部均采用椭圆封头受压。所述合成反应段1的顶部设置有物料进口5,所述脱挥段2的上部设置有挥发物出口6,所述脱挥段2的底部设置有物料出口7,用于导出合成脱挥的产物。Described synthesis reaction section 1 is cylindrical, the upper part of described devolatilization section 2 is cylindrical (inner height 3.5m), the lower part is inverted cone (inner height 3.5m, apex angle 60°), described synthesis reaction section 1 and the upper part of the devolatilization section 2 both use elliptical heads to press. The top of the synthesis reaction section 1 is provided with a material inlet 5, the upper part of the devolatilization section 2 is provided with a volatiles outlet 6, and the bottom of the devolatilization section 2 is provided with a material outlet 7 for deriving synthetic devolatilization. product.
所述合成反应段1直接设置于所述脱挥段2的上方,形成合成脱挥器的本体,所述合成反应段1的出口通过法兰与所述脱挥段2的入口连接,使得在所述合成反应段1中合成得到的合成产物可直接落入所述脱挥段2进行脱挥。The synthesis reaction section 1 is directly arranged above the devolatilization section 2 to form the body of the synthesis devolatilizer, and the outlet of the synthesis reaction section 1 is connected to the inlet of the devolatilization section 2 through a flange, so that in the The synthetic product synthesized in the synthesis reaction section 1 can directly fall into the devolatilization section 2 for devolatilization.
两级挥发物分离单元串联后与所述挥发物出口6连接,用于挥发物的分离。各级挥发物分离单元均包括冷凝器3和气液分离器4,所述冷凝器3的上部设置有冷凝进口20,用于导入挥发物,所述冷凝器3的下部设置有冷凝出口21,用于导出冷凝后的挥发物,所述冷凝器3的外部设置夹套式冷却结构,该夹套的下部设置有循环液进口18,上部设置有循环液出口19。并且,第一级挥发物分离单元的冷凝器3的挥发物进口20连接所述挥发物出口6,第二级挥发物分离单元的冷凝器3的挥发物进口20连接第一级挥发物分离单元的气液分离器4的气相出口22。Two-stage volatile matter separation units are connected in series with the volatile matter outlet 6 for separation of volatile matter. Volatile separation units at all levels include a condenser 3 and a gas-liquid separator 4. The upper part of the condenser 3 is provided with a condensation inlet 20 for introducing volatiles, and the lower part of the condenser 3 is provided with a condensation outlet 21 for In order to export the condensed volatiles, a jacket cooling structure is arranged outside the condenser 3 , the lower part of the jacket is provided with a circulating liquid inlet 18 , and the upper part is provided with a circulating liquid outlet 19 . In addition, the volatile inlet 20 of the condenser 3 of the first-stage volatile separation unit is connected to the volatile outlet 6, and the volatile inlet 20 of the condenser 3 of the second-stage volatile separation unit is connected to the first-stage volatile separation unit The gas phase outlet 22 of the gas-liquid separator 4.
所述真空单元(真空泵)与第二级挥发物分离单元的气液分离器4的气相出口22连接,用于提供所述合成反应段1和所述脱挥段2需要的真空度。The vacuum unit (vacuum pump) is connected to the gas-phase outlet 22 of the gas-liquid separator 4 of the second-stage volatile matter separation unit, and is used to provide the vacuum degree required by the synthesis reaction section 1 and the devolatilization section 2 .
开启真空泵,通过物料进口5以0.2m/s的速度导入反应物料,在合成反应段1的夹套中导入140℃的导热油,使得合成反应的条件为温度110℃,时间5min,压力0.15MPa。合成反应得到的合成产物可直接落入脱挥段2中进行脱挥,在脱挥段2的加热单元通入270℃的导热油,使得脱挥的条件为温度220℃,时间0.5min,压力-0.095MPa。通过脱挥得到的产品从物料出口7导出,挥发物从挥发物出口6导入两级挥发物分离单元,在第一级挥发物分离单元的冷凝器3中导入冷凝水进行冷凝,然后在气液分离器4中进行气液分离,然后再在第二级挥发物分离单元的冷凝器3中导入冷冻水进行冷凝,然后在气液分离器4中进行气液分离。从两级挥发物分离单元的气液分离器4的溶剂出口24导出得到的溶剂。Turn on the vacuum pump, introduce the reaction material at a speed of 0.2m/s through the material inlet 5, and introduce 140°C heat-conducting oil into the jacket of the synthesis reaction section 1, so that the conditions of the synthesis reaction are temperature 110°C, time 5min, pressure 0.15MPa . The synthetic product obtained by the synthesis reaction can be directly dropped into the devolatilization section 2 for devolatilization, and the heating unit of the devolatilization section 2 is fed with heat-conducting oil at 270 °C, so that the conditions of the devolatilization are the temperature of 220 °C, the time of 0.5 min, and the pressure. -0.095MPa. The product obtained by devolatilization is led out from the material outlet 7, the volatiles are introduced into the two-stage volatiles separation unit from the volatiles outlet 6, and condensed water is introduced into the condenser 3 of the first-stage volatiles separation unit for condensation, and then in the gas-liquid The gas-liquid separation is carried out in the separator 4 , and then chilled water is introduced into the condenser 3 of the second-stage volatile matter separation unit for condensation, and then the gas-liquid separation is carried out in the gas-liquid separator 4 . The resulting solvent is drawn from the solvent outlet 24 of the gas-liquid separator 4 of the two-stage volatiles separation unit.
以上详细描述了本发明的优选实施方式,但是,本发明并不限于此。在本发明的技术构思范围内,可以对本发明的技术方案进行多种简单变型,包括各个技术特征以任何其它的合适方式进行组合,这些简单变型和组合同样应当视为本发明所公开的内容,均属于本发明的保护范围。The preferred embodiments of the present invention have been described above in detail, however, the present invention is not limited thereto. Within the scope of the technical concept of the present invention, a variety of simple modifications can be made to the technical solutions of the present invention, including the combination of various technical features in any other suitable manner. These simple modifications and combinations should also be regarded as the content disclosed in the present invention. All belong to the protection scope of the present invention.
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