WO2023273475A1 - 一种颜料低温均一化聚酰胺 -6 原位聚合反应装置及其工艺 - Google Patents
一种颜料低温均一化聚酰胺 -6 原位聚合反应装置及其工艺 Download PDFInfo
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- WO2023273475A1 WO2023273475A1 PCT/CN2022/084752 CN2022084752W WO2023273475A1 WO 2023273475 A1 WO2023273475 A1 WO 2023273475A1 CN 2022084752 W CN2022084752 W CN 2022084752W WO 2023273475 A1 WO2023273475 A1 WO 2023273475A1
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- 238000006116 polymerization reaction Methods 0.000 title claims abstract description 36
- 229920002292 Nylon 6 Polymers 0.000 title claims abstract description 18
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 16
- 239000000049 pigment Substances 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 41
- 239000000463 material Substances 0.000 claims description 24
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims description 16
- 239000000654 additive Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 5
- 230000008676 import Effects 0.000 claims description 4
- 235000009421 Myristica fragrans Nutrition 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 239000001115 mace Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000002861 polymer material Substances 0.000 claims description 3
- 239000000155 melt Substances 0.000 description 9
- 238000009826 distribution Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000010586 diagram Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/1812—Tubular reactors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
Definitions
- the invention relates to the technical field of in-situ polymerization of polyamide-6, in particular to a low-temperature homogeneous polyamide-6 in-situ polymerization reaction device for pigments and a process thereof.
- All polyamide-6 polymerization reactors are tubular reactors, which are generally divided into pre-polymerization reactors and post-polymerization reactors, both of which are tubular reactors up to tens of meters, also known as VK tubes.
- VK tubes tubular reactors up to tens of meters, also known as VK tubes.
- color paste and other additives need to be added to the polymerization reactor.
- the mixing of these materials and the raw material caprolactam into the pre-polymerization reactor is not sufficient and uneven, which will inevitably lead to the uneven reaction of these materials participating in the in-situ polymerization. Uniformity, resulting in uneven distribution of pigments and additives in the melt, and the homogeneity of the polymer in the pre-polymerization reactor is affected.
- the object of the present invention is to provide a pigment low-temperature homogeneous polyamide-6 in-situ polymerization reaction device and its process, which solves the problems raised in the background technology.
- a low-temperature homogeneous polyamide-6 in-situ polymerization reaction device for pigments including an online dynamic mixer, a pre-polymerizer, a post-polymerizer, and also includes tubes, homogeneous reaction Stirrer, deflector, drain pipe, the online dynamic mixer is connected to the front polymerizer, the front polymerizer is connected to the rear polymerizer, the tubes are installed inside the front polymerizer and the rear polymerizer, the The homogeneous reaction agitator is installed in the middle of the column tube, the homogeneous reaction agitator is arranged on the top of the front polymerization reactor, the baffle is arranged inside the front polymerizer, and the baffle is installed in the homogeneous reaction agitator bottom.
- the online dynamic mixer can monitor and make the mixing between caprolactam, color paste and additives more fully and uniformly.
- the structure of the online dynamic mixer is a pin mace type.
- the homogeneous reaction agitator is a material propulsion type agitator, which stirs the material evenly, and a deflector is arranged at the bottom of the homogeneous reaction agitator, and propels the material to toss up and down around the column tube while stirring, avoiding solid particles Scale deposits on the tube walls.
- the length of the single tube at the center of the tube array is the longest, and it is arranged gradually shortened in the radial direction, and the increased part is exposed outside the bottom plate of the tube tube, and the diameter of all the single tubes becomes smaller and the number increases, so that the heat transfer And the reaction is more uniform, the radial temperature difference of the melt is smaller, and the longitudinal flow distribution of the melt is improved.
- a pigment low-temperature homogeneous polyamide-6 in-situ polymerization process comprising the following steps:
- Step 1 First, add refined caprolactam, color paste and additives into an online dynamic mixer in a certain proportion and mix;
- Step 2 Import the mixed raw materials into the prepolymerizer for reaction, turn on the homogeneous reaction mixer, and stir the materials evenly. On the other hand, set a deflector at the bottom to push the materials up and down around the tube while stirring ;
- Step 3 Discharge the reacted water from the drain pipe above the front polymerizer, and export the reacted material from below;
- Step 4 Importing the reacted material of the front polymerizer from above the rear polymerizer to continue the polymerization reaction;
- Step 5 The final polymer material that has been reacted is exported from the bottom of the post-polymerizer to the injection strip section, and the reacted water is discharged from the drain above the post-polymerizer.
- the material is pushed and stirred evenly by setting the homogeneous reaction agitator.
- the deflector By setting the deflector at the bottom of the homogeneous reaction agitator, the material is pushed up and down around the tube while stirring, so as to avoid the deposition of solid particles on the tube wall Fouling.
- Fig. 1 is the structural representation of production device of the present invention
- Fig. 2 is a schematic diagram of the tube arrangement of the production device of the present invention.
- a low-temperature uniform polyamide-6 in-situ polymerization reaction device for pigments including an online dynamic mixer 1, a pre-polymerizer 2, and a post-polymerizer (3), and also includes Column pipe 4, homogeneous reaction agitator 5, deflector 6, drain pipe 7, described online dynamic mixer 1 is connected with front polymerizer 2, and described front polymerizer 2 is connected with rear polymerizer 3, and described row
- the pipe 4 is installed inside the front polymerizer 2 and the rear polymerizer 3, the homogeneous reaction agitator 5 is installed in the middle of the column tube 4, the homogeneous reaction agitator 5 is arranged on the top of the front polymerization reactor, and the diversion
- the plate 6 is arranged inside the front polymerizer 2 , and the deflector 6 is installed at the bottom of the homogeneous reaction mixer 5 .
- the online dynamic mixer 1 can monitor and make the mixing between caprolactam, color paste and additives more fully and uniformly, and provide certain help for the following homogeneous polymerization reaction.
- the structure of the online dynamic mixer 1 is a pin mace type.
- the homogeneous reaction agitator 5 is a material propulsion type agitator, and the material is stirred evenly, and a deflector 6 is arranged at the bottom of the homogeneous reaction agitator 5, and the material is pushed up and down around the column tube 4 while stirring, The deposition and fouling of solid particles on the 4 walls of the tubes are avoided.
- the length of the single tube at the center of the tube array 4 is the longest, and it is arranged gradually shortened in the radial direction.
- the heat transfer and reaction are more uniform, the radial temperature difference of the melt is smaller, and the longitudinal flow distribution of the melt is improved.
- a pigment low-temperature homogeneous polyamide-6 in-situ polymerization process comprising the following steps:
- Step 1 First, add refined caprolactam, color paste and additives into the online dynamic mixer 1 in a certain proportion and mix them;
- Step 2 Import the mixed raw materials into the pre-polymerizer 2 for reaction, turn on the homogeneous reaction mixer 5, and stir the materials evenly.
- a deflector 6 at the bottom to push the materials into the tube while stirring 4 toss up and down around;
- Step 3 discharge the reacted water from the drain pipe 7 above the front polymerizer 2, and export the reacted material from below;
- Step 4 importing the reacted material in the front polymerizer 2 from above the rear polymerizer 3 to continue the polymerization reaction;
- Step 5 The final polymer material that has been reacted is exported from the bottom of the post-polymerizer 3 to the injection strip section, and the reacted water is discharged from the drain pipe 7 above the post-polymerizer 3 .
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Polyamides (AREA)
Abstract
一种颜料低温均一化聚酰胺-6原位聚合反应装置及其工艺,包括:在线动态混合器(1)、前聚合器(2)、后聚合器(3),还包括列管(4)、均质反应搅拌器(5),导流板(6)、排水管(7),在线动态混合器(1)与前聚合器(2)连接,前聚合器(2)与后聚合器(3)连接,列管(4)安装在前聚合器(2)和后聚合器(3)内部,均质反应搅拌器(5)安装在列管(4)中间,均质反应搅拌器(5)设置在前聚合器(2)顶部,导流板(6)设置在前聚合器(2)内部,导流板(6)安装在均质反应搅拌器(5)底部。
Description
本发明涉及聚酰胺-6原位聚合技术领域,具体为一种颜料低温均一化聚酰胺-6原位聚合反应装置及其工艺。
聚酰胺-6聚合反应器都为管式反应器,一般分为前聚合反应器和后聚合反应器,均为高达几十米的管式反应器,亦称VK管。有色聚酰胺-6聚合时需加入大量的色浆和其他添加剂到聚合反应器中,这些材料与原料己内酰胺进入前聚合反应器时混合不充分不均匀,势必造成这些材料参与原位聚合的反应不均匀,造成颜料、添加剂在熔体中分布不均匀,前聚合反应器内聚合体的均一性就受到影响。
有色聚酰胺-6聚合时需加入大量的色浆和其他添加剂到聚合反应器中,这些材料与原料己内酰胺进入前聚合反应器时混合不充分不均匀,势必造成这些材料参与原位聚合的反应不均匀,造成颜料、添加剂在熔体中分布不均匀,前聚合反应器内聚合体的均一性就受到影响。
本发明的目的在于提供一种颜料低温均一化聚酰胺-6原位聚合反应装置及其工艺,解决了背景技术中提出的问题。
为实现上述目的,本发明提供如下技术方案:一种颜料低温均一化聚酰胺-6原位聚合反应装置,包括在线动态混合器、前聚合器、后聚合器,还包括列管、均质反应搅拌器,导流板、排水管,所述在线动态混合器与前聚合器连接,所述前聚合器与后聚合器连接,所述列管安装在前聚合器和后聚合器内部,所述均质反应搅拌器安装在列管中间,所述均质反应搅拌器设置在前聚合反应器顶部,所述导流板设置在前聚合器内部,所述导流板安装在均质反应搅拌器底部。
其中,所述在线动态混合器能够监控并使得己内酰胺、色浆和添加剂之间混合的更加充分均匀。
其中,所述在线动态混合器的结构为销钉狼牙棒型。
其中,所述均质反应搅拌器为物料推进型搅拌器,将物料搅拌均匀,在均质反应搅拌器底部设置导流板,在搅拌的同时推进物料在列管周围上下翻腾,避免了固体颗粒在列管壁沉积结垢。
其中,所述列管的中心处单管长度最长,并沿径向渐渐变短进行排列,增长的部分露在列管下底板外面,所有单管的直径变小,数量增加,使得传热和反应更均匀,熔体径向温差更小,改善熔体的纵向流动分布。
一种颜料低温均一化聚酰胺-6原位聚合反应工艺,包括以下步骤:
步骤1:首先将精己内酰胺、色浆和添加剂按一定比列加入到在线动态混合器中混合;
步骤2:将混合后的原料导入至前聚合器中反应,开启均质反应搅拌器,将物料搅拌均匀,另一方面在底部设置导流板,在搅拌的同时推进物料在列管周围上下翻腾;
步骤3:将反应后的水从前聚合器上方排水管排出,反应后的物料从下方导出;
步骤4:将前聚合器反应后的物料从后聚合器的上方导入继续聚合反应;
步骤5:将最后反应完成的聚合物料从后聚合器下方导出注带切片,反应后的水从后聚合器上方排水管排出。
与现有技术相比,本发明的有益效果如下:
1、通过设置在线动态混合器使得己内酰胺、色浆和添加剂之间混合的更加充分均匀,为后面的均一化聚合反应提供一定的帮助。
2、通过设置均质反应搅拌器将物料推进搅拌均匀,通过在均质反应搅拌器底部设置导流板,在搅拌的同时推进物料在列管周围上下翻腾,避免了固体颗粒在列管壁沉积结垢。
3、通过设置列管的中心处单管长度最长,并沿径向渐渐变短进行排列,增长的部分露在列管下底板外面,所有单管的直径变小,数量增加,使得传热和反应更均匀,熔体径向温差更小,改善熔体的纵向流动分布。
图1为本发明生产装置的结构示意图;
图2为本发明生产装置的列管示意图;
图中:1、在线动态混合器;2、前聚合器;3、后聚合器;4、列管;5、均质反应搅拌器;6、导流板;7、排水管。
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
请参阅图1,本发明提供一种技术方案:一种颜料低温均一化聚酰胺-6原位聚合反应装置,包括在线动态混合器1、前聚合器2、后聚合器(3),还包括列管4、均质反应搅拌器5,导流板6、排水管7,所述在线动态混合器1与前聚合器2连接,所述前聚合器2与后聚合器3连接,所述列管4安装在前聚合器2和后聚合器3内部,所述均质反应搅拌器5安装在列管4中间,所述均质反应搅拌器5设置在前聚合反应器顶部,所述导流板6设置在前聚合器2内部,所述导流板6安装在均质反应搅拌器5底部。
其中,所述在线动态混合器1能够监控并使得己内酰胺、色浆和添加剂之间混合的更加充分均匀,为后面的均一化聚合反应提供一定的帮助。
其中,所述在线动态混合器1的结构为销钉狼牙棒型。
其中,所述均质反应搅拌器5为物料推进型搅拌器,将物料搅拌均匀,在均质反应搅拌器5底部设置导流板6,在搅拌的同时推进物料在列管4周围上下翻腾,避免了固体颗粒在列管4壁沉积结垢。
其中,所述列管4的中心处单管长度最长,并沿径向渐渐变短进行排列,增长的部分露在列管4下底板外面,所有单管的直径变小,数量增加,使得传热和反应更均匀,熔体径向温差更小,改善熔体的纵向流动分布。
一种颜料低温均一化聚酰胺-6原位聚合反应工艺,包括以下步骤:
步骤1:首先将精己内酰胺、色浆和添加剂按一定比列加入到在线动态混合器1中混合;
步骤2:将混合后的原料导入至前聚合器2中反应,开启均质反应搅拌器5,将物料搅拌均匀,另一方面在底部设置导流板6,在搅拌的同时推进物料在列管4周围上下翻腾;
步骤3:将反应后的水从前聚合器2上方排水管7排出,反应后的物料从下方导出;
步骤4:将前聚合器2反应后的物料从后聚合器3的上方导入继续聚合反应;
步骤5:将最后反应完成的聚合物料从后聚合器3下方导出注带切片,反应后的水从后聚合器3上方排水管7排出。
前聚合器2同一位置熔体温度比较:
前聚合反应器 | 热媒温度(℃) | 前聚合器列管下同一位置熔体中心温(℃) |
带均质反应搅拌器的有色PA6原位聚合前反应器 | 278 | 251.2 |
不带均质反应搅拌器的普通PA6聚合前反应器 | 278 | 247.0 |
同一点反应温度差值△T | / | 4.2 |
带均质反应搅拌器5和不带均质反应搅拌器5生产线的列管下熔体温度,显然,使用均质反应搅拌器5后同位置的熔体温度高于普通聚合反应器的熔体温度,说明反应效率提高。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (4)
- 一种颜料低温均一化聚酰胺-6原位聚合反应装置,其特征在于包括:在线动态混合器(1)、前聚合器(2)、后聚合器(3),还包括列管(4)、均质反应搅拌器(5),导流板(6)、排水管(7),所述在线动态混合器(1)与前聚合器(2)连接,所述前聚合器(2)与后聚合器(3)连接,所述列管(4)安装在前聚合器(2)和后聚合器(3)内部,所述均质反应搅拌器(5)安装在列管(4)中间,所述均质反应搅拌器(5)设置在前聚合反应器顶部,所述导流板(6)设置在前聚合器(2)内部,所述导流板(6)安装在均质反应搅拌器(5)底部。
- 根据权利要求1所述的一种颜料低温均一化聚酰胺-6原位聚合反应装置,其特征在于:所述在线动态混合器(1)的结构为销钉狼牙棒型。
- 根据权利要求1所述的一种颜料低温均一化聚酰胺-6原位聚合反应装置,其特征在于:所述列管(4)的中心处单管长度最长,并沿径向渐渐变短进行排列,增长的部分露在列管下底板外面,所有单管的直径变小,数量增加。
- 一种颜料低温均一化聚酰胺-6原位聚合反应工艺,其特征在于:包括以下步骤:步骤1:首先将精己内酰胺、色浆和添加剂按一定比例加入到在线动态混合器(1)中混合;步骤2:将混合后的原料导入至前聚合器(2)中反应,开启均质反应搅拌器(5),将物料搅拌均匀,另一方面在底部设置导流板(6),在搅拌的同时推进物料在列管(4)周围上下翻腾;步骤3:将反应后的水从前聚合器(2)上方排水管(7)排出,反应后的物料从下方导出;步骤4:将前聚合器(2)反应后的物料从后聚合器(3)的上方导入继续聚合反应;步骤5:将最后反应完成的聚合物料从后聚合器(3)下方导出注带切片,反应后的水从后聚合器上方排水管(7)排出。
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