阅读说明：本技术 一种锦纶6聚合试验装置 (Nylon 6 polymerization test device ) 是由 封其都 陈建新 陈亮 严栋 王冬晟 于 2019-10-16 设计创作，主要内容包括：本发明公开了一种锦纶6聚合试验装置,包括中间储罐,添加剂配制罐,动态混合器,前聚合器,后聚合器,切粒机,双螺杆挤出机,预萃取罐,萃取塔,湿切片料仓,干燥转鼓,混料转鼓,热合包装机,所述中间储罐连接到动态混合器,所述添加剂配制罐连接到动态混合器,所述动态混合器连接到前聚合器,所述前聚合器连接后聚合器,所述后聚合器可连接到切粒机,所述后聚合器亦可连接到双螺杆挤出机,所述双螺杆挤出机连接到切粒机,所述切粒机连接到预萃取罐,所述预萃取罐连接到萃取塔,所述萃取塔连接到湿切片料仓,如今产业化生产,无法用于新产品研发和多品种、多添加的试验,物料损耗大,灵活度不够,而且产业化生产能耗大,研发成本巨大,无法承受。(The invention discloses a polyamide-6 polymerization test device, which comprises an intermediate storage tank, an additive preparation tank, a dynamic mixer, a front polymerizer, a rear polymerizer, a granulator, a double-screw extruder, a pre-extraction tank, an extraction tower, a wet slicing bin, a drying rotary drum, a mixing rotary drum and a heat seal packaging machine, wherein the intermediate storage tank is connected to the dynamic mixer, the additive preparation tank is connected to the dynamic mixer, the dynamic mixer is connected to the front polymerizer, the front polymerizer is connected to the rear polymerizer, the rear polymerizer can be connected to the granulator, the rear polymerizer can also be connected to the double-screw extruder, the double-screw extruder is connected to the granulator, the granulator is connected to the pre-extraction tank, the pre-extraction tank is connected to the extraction tower, the extraction tower is connected to the wet slicing bin, the polyamide-6 polymerization test device can not be used for research and development of new, The test of adding more, the material loss is big, and the flexibility ratio is not enough, and the industrial production energy consumption is big moreover, and research and development cost is huge, can not bear.)

1. A polyamide-6 polymerization test device comprises an intermediate storage tank (1), an additive preparation tank (2), a dynamic mixer (3), a front polymerizer (4), a rear polymerizer (5), a granulator (6), a twin-screw extruder (7), a pre-extraction tank (8), an extraction tower (9), a wet slicing bin (10), a drying drum (11), a mixing drum (12) and a heat sealing packaging machine (13), wherein the intermediate storage tank (1) is connected to the dynamic mixer (3), the additive preparation tank (2) is connected to the dynamic mixer (3), the dynamic mixer (3) is connected to the front polymerizer (4), the front polymerizer (4) is connected to the rear polymerizer (5), the rear polymerizer (5) is connected to the granulator (6), the rear polymerizer (5) is also connected to the twin-screw extruder (7), and the twin-screw extruder (7) is connected to the granulator (6), the granulator (6) is connected to a pre-extraction tank (8), the pre-extraction tank (8) is connected to an extraction tower (9), the extraction tower (9) is connected to a wet chip bin (10), the wet chip bin (10) is connected to a dryer drum (11), and the dryer drum (11) is connected to a mixing drum (12).

2. The polyamide-6 polymerization test device according to claim 1, characterized in that: the materials in the intermediate storage tank and the additive preparation tank are connected with the dynamic mixer through a plunger pump.

3. The polyamide-6 polymerization test device according to claim 1, characterized in that: the temperature in the front polymerizer is 260 ℃ and 280 ℃, the pressure is 0.1-0.3MPa, and the biphenyl steam jacket is 0.05-0.1 MPa.

4. The polyamide-6 polymerization test device according to claim 1, characterized in that: the front polymerizer is connected to the rear polymerizer through a gear pump.

5. The polyamide-6 polymerization test device according to claim 1, characterized in that: the temperature of the upper section of the post polymerizer is 260-280 ℃, the temperature of the lower section of the post polymerizer is 235-250 ℃, the pressure is normal pressure or negative pressure, the biphenyl steam jacket of the upper section is 0.05-0.1MPa, and the biphenyl jacket of the lower section is 0.2-0.6 MPa.

6. The polyamide-6 polymerization test device according to claim 1, characterized in that: the pre-extraction tank is connected with the extraction tower through a slurry pump.

7. The polyamide-6 polymerization test device according to claim 1, characterized in that: the steam jacket in the extraction tower is 105 ℃ and 115 ℃, and the air pressure is 0.05-0.3 MPa.

8. The use method of the polyamide-6 polymerization test device according to claim 1, characterized in that: the method comprises the following steps:

s1, circularly pumping raw material liquid caprolactam into a middle storage tank (1) from a polymerization workshop, adding an additive into an additive preparation tank (2), connecting materials in the middle storage tank and the additive preparation tank to a dynamic mixer (3) through a plunger pump, fully and uniformly mixing in the dynamic mixer (3), adding the materials into a front polymerizer (4) for hydrolysis ring opening and partial addition polymerization, wherein the molecular weight of a reaction product is about 8000-10000, adding the reaction product into a rear polymerizer (5) through a gear pump, and further completing addition polymerization and chain balance reaction to generate a polyamide 6 polymer melt, the molecular weight of which is about 11000-15000;

s2 and S ① are used for discharging the polymer melt quantitatively through a gear pump, casting the polymer melt into strips in a casting head, and cooling and pelletizing the strips in a quenching tank of a pelletizer (6) to form nylon 6 chips;

②, discharging the polymer melt into a double-screw extruder (7), adding some modifier into the double-screw extruder (7), cooling the obtained product in a quenching tank of a granulator (6), and granulating to form polyamide-6 chips;

s3, removing ultra-long slices and powder in a vibrating screen, then falling into a pre-extraction tank (8) for pre-extraction, then pumping the slices and water into an extraction tower (9) by using a slurry pump, wherein the slices are arranged from top to bottom in the extraction tower (9), hot desalted water is used for carrying out countercurrent extraction on the slices from bottom to top to remove monomers and oligomers contained in the slices, and extraction water flows out from the top of the tower and then continuously flows to the pre-extraction tank (8) for carrying out pre-extraction on the slices;

s4, conveying the slices and water to a dehydrator positioned on the upper part of the wet slicing bin (10) through a slurry pump for dehydration, and then entering the wet slicing bin (10) for temporary storage;

wet section in wet section feed bin (10) is dried in vacuum suction system inhales drying drum (11), puts into compounding rotary drum (12) of below after the drying is accomplished and keeps in temporarily, and the slicing output of 3 ~ 10 days can probably be deposited to compounding rotary drum (12), and the packing is waited to examine to the misce bene.

Technical Field

The invention relates to the field of polymerization test devices, in particular to a polyamide-6 polymerization test device.

Background

At present, the maximum capacity of a single caprolactam polymerization pipe in China reaches 400 tons/day, but an industrial production line for polymerizing the chinlon cannot perform product tests, mainly has large loss and can consume a large amount of capacity, if the test is performed by taking the capacity of 100 tons per day, the cost loss per day is millions of yuan, enterprises are hard to bear, and a large amount of manpower and material resources are wasted.

If an industrial production line is used for research and development, the research and development flexibility degree is reduced, some data cannot be adjusted, tests of multiple varieties and multiple additives cannot be carried out, and the research and development of new products are only delayed.

Disclosure of Invention

The invention aims to provide a polyamide-6 polymerization test device to solve the problems in the background technology.

In order to achieve the purpose, the invention provides the following technical scheme: a polyamide-6 polymerization test device comprises an intermediate storage tank, an additive preparation tank, a dynamic mixer, a front polymerizer, a rear polymerizer, a granulator, a double-screw extruder, a pre-extraction tank, an extraction tower, a wet slicing bin, a drying rotary drum, a mixing rotary drum and a heat seal packaging machine, the intermediate storage tank is connected to a dynamic mixer, the additive preparation tank is connected to the dynamic mixer, the dynamic mixer is connected to a front polymerizer, the front polymerizer is connected to a rear polymerizer, the rear polymerizer is connectable to a pelletizer, the post mixer may also be connected to a twin screw extruder, which is connected to a pelletizer, the pelletizer is connected to a pre-extraction tank, the pre-extraction tank is connected to an extraction tower, the extraction tower is connected to a wet chip bin, the wet chip bin is connected to a dryer drum, and the dryer drum is connected to a compounding drum.

The caprolactam is circularly pumped to an intermediate storage tank from a polymerization workshop, and the caprolactam and various additives are proportionally pumped into a dynamic mixer through a metering pump.

Wherein, the mixture is fully and uniformly mixed in the dynamic mixer and then is added into a pre-polymerizer.

Wherein the temperature in the front polymerizer is 260 ℃ and 280 ℃, the pressure is 0.1-0.3MPa, the biphenyl steam jacket is 0.05-0.1MPa, and the mixture is subjected to hydrolytic ring opening and partial addition polymerization in the front polymerizer.

Wherein the molecular weight of the reaction product is about 8000-10000, and the reaction product is conveyed to a post-polymerization reactor by a gear pump.

Wherein the temperature of the upper section in the post polymerizer is 260-280 ℃, the temperature of the lower section is 235-250 ℃, the pressure is normal pressure or negative pressure, the biphenyl steam jacket of the upper section is 0.05-0.1MPa, the biphenyl jacket of the lower section is 0.2-0.6MPa, the reaction product further completes addition polymerization and chain balance reaction in the post polymerizer to generate a polyamide 6 polymer melt, and the molecular weight is about 11000-15000.

Wherein the polymer melt is metered out with a gear pump and cast into a strand in a casting head.

Wherein, the polymer melt is extruded and pelletized by a double-screw extruder, and various modifiers can be added in the process, so that the development flexibility is enhanced.

And cooling and pelletizing the strip in a quenching tank of a pelletizer to form nylon 6 slices, and removing ultra-long slices and powder in a vibrating screen.

Wherein the slices fall into a pre-extraction tank for pre-extraction, and the slices are pumped into an extraction tower together with water by a slurry pump.

Wherein, the steam jacket in the extraction tower is 105 ℃ and 115 ℃, and the air pressure is 0.05-0.3 MPa.

Wherein, in the extraction tower, the slices are extracted from top to bottom, and hot desalted water is used for carrying out countercurrent extraction on the slices from bottom to top, so that monomers and oligomers contained in the slices are removed.

The extraction water flows out from the top of the tower and then flows to the pre-extraction tank, and pre-extraction is carried out on slices, so that the cost is saved.

And the extraction water contains a certain amount of caprolactam monomer, and is conveyed to a concentrated solution recovery system of a polymerization workshop through an extraction water pump, and is changed into recovered caprolactam concentrated solution after evaporation and concentration, and the recovered caprolactam concentrated solution is recycled by the polymerization workshop, so that the cost is saved.

And the slices and water are pumped to a dehydrator positioned on the upper part of the wet slice bin by a slice cement slurry for dehydration and then enter the wet slice bin for temporary storage.

And after drying, the wet slices are placed into the mixing drum below for temporary storage and mixing.

Wherein the mixing drum can be stored for 3-10 days with slice production capacity.

Wherein, dry section is weighed after the misce bene and is packed and wait to examine.

The use method of the chinlon 6 polymerization test device comprises the following steps:

s1, circularly pumping raw material liquid caprolactam into a middle storage tank from a polymerization workshop, adding an additive into an additive preparation tank, connecting materials in the middle storage tank and the additive preparation tank to a dynamic mixer through a plunger pump, fully and uniformly mixing in the dynamic mixer, adding the materials into a front polymerizer for hydrolytic ring opening and partial addition polymerization, wherein the molecular weight of a reaction product is about 8000-10000, and the reaction product is added into a rear polymerizer through a gear pump to further finish addition polymerization and chain balance reaction to generate a polyamide 6 polymer melt with the molecular weight of about 11000-15000.

S2 and S ① are used for discharging polymer melt quantitatively through a gear pump, casting the polymer melt into strips in a casting head, cooling the strips in a quenching tank of a granulator, and granulating to form nylon 6 chips, ② is used for discharging the polymer melt into a double-screw extruder, some modifying agent can be added into the double-screw extruder, and the obtained product is cooled in the quenching tank of the granulator, and is granulated to form the nylon 6 chips.

S3, removing the ultra-long slices and powder in a vibrating screen, then falling into a pre-extraction tank for pre-extraction, then pumping the slices and water into an extraction tower by a slurry pump, carrying out countercurrent extraction on the slices from top to bottom in the extraction tower by hot desalted water from bottom to top, removing monomers and oligomers contained in the slices, and continuously flowing extraction water to the pre-extraction tank after flowing out from the top of the tower, and carrying out pre-extraction on the slices.

And S4, conveying the slices and water to a dehydrator positioned on the upper part of the wet slice bin through a slurry pump for dehydration, and entering the wet slice bin for temporary storage. Wet section in the wet section feed bin is dried in sucking the drying drum through vacuum suction system, puts into the compounding drum of below after the drying and keeps in temporarily, and the compounding drum can deposit 3 ~ 10 days's section production capacity probably, and the misce bene is packed and is examined the inspection.

The invention has the beneficial effects that:

the invention relates to a polyamide-6 polymerization test device, a polymerization modification small test platform has small capacity, various test auxiliaries can be added, a multipoint adding method is adopted, the flexibility is enhanced, the daily loss is very low, about 1500 yuan, the research and development cost is greatly reduced, and the capacity loss is reduced. In addition, the technological process of the nylon-6 polymerization test device is highly simulated for an industrialized polymerization production line, and if new products are successfully researched and developed, the technology and the process can be directly applied to the industrialized production line.

Drawings

FIG. 1 is a schematic view of the apparatus of the present invention;

in fig. 1: 1-an intermediate storage tank; 2-additive preparation tank; 3-a dynamic mixer; 4-a pre-polymerizer; 5-a post-polymerizer; 6-a granulator; 7-twin screw extruder; 8-a pre-extraction tank; 9-an extraction column; 10-a wet slicing bin; 11-a dryer drum; 12-a mixing drum; 13-heat sealing packaging machine.

Detailed Description

So that the manner in which the features and aspects of the present invention can be understood in detail, a more particular description of the invention, briefly summarized above, may be had by reference to embodiments, some of which are illustrated in the appended drawings.

Referring to fig. 1, a polyamide 6 polymerization test apparatus comprises an intermediate storage tank 1, an additive preparation tank 2, a dynamic mixer 3, a front polymerizer 4, a rear polymerizer 5, a granulator 6, a twin-screw extruder 7, a pre-extraction tank 8, an extraction tower 9, a wet chip bin 10, a drying drum 11, a mixing drum 12, a heat seal packer 13, wherein the intermediate storage tank 1 is connected to the dynamic mixer 3, the additive preparation tank 2 is connected to the dynamic mixer 3, the dynamic mixer 3 is connected to the front polymerizer 4, the front polymerizer 4 is connected to the rear polymerizer 5, the rear polymerizer 5 is connected to the granulator 6, the rear polymerizer 5 is also connected to the twin-screw extruder 7, the granulator 7 is connected to the granulator 6, the granulator 6 is connected to the pre-extraction tank 8, the pre-extraction tank 8 is connected to the extraction tower 9, the extraction tower 9 is connected to the wet chip bin 10, the wet chip silo 10 is connected to a dryer drum 11, and the dryer drum 11 is connected to a mixing drum 12.

Caprolactam is pumped to an intermediate storage tank 1 from a polymerization plant in a circulating manner, and the caprolactam and various additives are proportionally pumped into a dynamic mixer 3 through a metering pump. The mixture was thoroughly mixed in the dynamic mixer 3 and then fed into the pre-polymerizer 4. Hydrolytic ring opening and partial polyaddition are carried out in the front polymerizer 4, and the reaction product is transferred to the rear polymerizer 5 by a gear pump, and has a molecular weight of about 8000-10000. The reaction product further completes the addition polymerization and chain equilibrium reaction in the post-polymerizer 5 to form a polymer melt with a molecular weight of about 11000-15000.

The polymer melt was metered out by means of a gear pump and cast into a strand in a casting head. Or extruding and granulating 7 by a double-screw extruder, and adding various modifying agents in the process. Cooling and granulating in a quenching tank of a granulator 6 to form nylon 6 slices, and removing ultra-long slices and powder in a vibrating screen.

The slices fall into a pre-extraction tank 8 for pre-extraction, then the slices and water are pumped into an extraction tower 9 by a slurry pump, the slices are extracted from top to bottom, and hot desalted water is used for carrying out countercurrent extraction on the slices from bottom to top, so that monomers and oligomers contained in the slices are removed. The slices and water are pumped to a dehydrator positioned on the upper part of the wet slice bin 10 by a slice cement slurry pump for dehydration, and then enter the wet slice bin 10 for temporary storage. Wet section inhales in the drying rotary drum 11 through vacuum suction system in wet section feed bin 10 and dries, puts into the compounding rotary drum 12 of below after the drying and keeps in temporarily and mixes, and compounding rotary drum 12 can deposit 3 ~ 10 days probably the section production volume, and the packing of weighing after the dry section misce bene that obtains at last is waited to examine.

Wherein the temperature in the front polymerizer 4 is 260 ℃ and 280 ℃, the air pressure is 0.1-0.3MPa, and the biphenyl steam jacket is 0.05-0.1 MPa.

Wherein the temperature of the upper section in the post polymerizer 5 is 260-280 ℃, the temperature of the lower section is 235-250 ℃, the pressure is normal pressure or negative pressure, the biphenyl steam jacket of the upper section is 0.05-0.1MPa, and the biphenyl jacket of the lower section is 0.2-0.6 MPa.

Wherein, the steam jacket 105 and the pressure in the extraction tower 9 are 115 ℃ and 0.05-0.3 MPa.

Wherein, the extraction water flows out from the top of the tower and then flows to the pre-extraction tank 8, and pre-extraction is carried out on the slices, thus saving the cost.

And the extraction water contains a certain amount of caprolactam monomer, and is conveyed to a concentrated solution recovery system of a polymerization workshop through an extraction water pump, and is changed into recovered caprolactam concentrated solution after evaporation and concentration, and the recovered caprolactam concentrated solution is recycled by the polymerization workshop, so that the cost is saved.

The working principle is as follows: a use method of a chinlon 6 polymerization test device comprises the following steps:

s1, circularly pumping raw material liquid caprolactam into an intermediate storage tank 1 from a polymerization workshop, adding an additive into an additive preparation tank 2, connecting materials in the intermediate storage tank and the additive preparation tank to a dynamic mixer 3 through a plunger pump, fully and uniformly mixing in the dynamic mixer 3, adding the materials into a pre-polymerizer 4 for hydrolysis ring opening and partial polyaddition reaction, wherein the molecular weight of a reaction product is about 8000-10000, and the reaction product is added into a post-polymerizer 5 through a gear pump to further complete polyaddition and chain equilibrium reaction to generate a polyamide 6 polymer melt, and the molecular weight is about 11000-15000.

S2 and S ① are used for discharging polymer melt quantitatively through a gear pump, casting the polymer melt into strips in a casting head, cooling the strips in a quenching tank of a granulator 6 and granulating the strips to form polyamide 6 chips, ② is used for discharging the polymer melt into a double-screw extruder 7, a certain amount of modifier can be added into the double-screw extruder 7, and the obtained product is cooled in the quenching tank of the granulator 6 and granulated to form the polyamide 6 chips.

S3, removing ultra-long slices and powder in a vibrating screen, then falling into a pre-extraction tank 8 for pre-extraction, then pumping the slices and water into an extraction tower 9 by a slurry pump, slicing the slices in the extraction tower 9 from top to bottom, carrying out countercurrent extraction on the slices from bottom to top by hot desalted water to remove monomers and oligomers contained in the slices, and continuously flowing extraction water to the pre-extraction tank 8 after flowing out from the top of the tower, wherein the slices are pre-extracted.

And S4, pumping the slices and water to a dehydrator positioned at the upper part of the wet slice bin 10 through a slurry pump for dehydration, and entering the wet slice bin 10 for temporary storage. Wet section in the wet section feed bin 10 is dried in sucking the drying drum 11 through vacuum suction system, puts into the compounding rotary drum 12 of below after the drying and keeps in temporarily, and the compounding rotary drum 12 can deposit 3 ~ 10 days probably the section production volume, and the packing is examined to the misce bene.

Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.