CN108586728A - A kind of film level nylon 6 slice and its production method - Google Patents
A kind of film level nylon 6 slice and its production method Download PDFInfo
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- CN108586728A CN108586728A CN201810538790.7A CN201810538790A CN108586728A CN 108586728 A CN108586728 A CN 108586728A CN 201810538790 A CN201810538790 A CN 201810538790A CN 108586728 A CN108586728 A CN 108586728A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
- C08G69/16—Preparatory processes
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Abstract
The present invention relates to a kind of film level nylon 6 slice and its production methods, after being purified to the extraction concentrate of recycling, it is homogenized after being mixed with solid material, additive is added, it is sent into after preheating using high pressure pre-polymerization after gas certainly the depolymerizing reactor high temperature and pressure depolymerization of stirring, gather decompression afterwards, extracted after underwater cutpellet, dry, cool down, obtains film level nylon 6 slice.Obtained film level nylon 6 slice relative viscosity can be controlled in 3.2 ± 0.030, viscosity deviation is controlled≤± 0.030, the weight % of hot water extractables content≤0.3, the wherein weight % of cyclic dimer≤0.05, the weight % of content of residual water≤0.04, coloration is 5~3.5 ± 1, has higher quality.
Description
Technical field
The present invention relates to 6 industrial production technology of nylon, especially a kind of film level nylon 6 slice and its production method.
Background technology
With the rapid development of economy in China, per capita consuming level and living standard increasingly improve, super to promote
Universal and tourist industry the fast development in city, the packaging dosage of all kinds of commodity sharply increase.
It is 6 film of BOPA biaxial tension nylons of raw material with nylon 6, is handled by biaxial tension in the process that forms a film,
The orientation on strand is strengthened, crystallinity is made to increase, improves mechanical property, and glossiness and transparency and right
Barrier properties for gases liquid is accordingly improved, and BOPA film polymer molecules are in plane orientation state, therefore thin with other packagings
Film is compared with very high puncture-resistant intensity, fracture-resistant is high, impact resistance is good, tensile strength is high, soft cold-resistant and heat-resisting etc.
Advantage；It saves cost, meet environmental requirement；It can be in wider (- 60~150 DEG C) long-time services of temperature range；Electrical insulating property
It can be good；Surface gloss is high, and refractive index increases, and has good transparency；It is strong to the barrier property of grease and gas, it is suitable for packaging
The oxidizable rotten food such as meat, fish, fatty foods, marine product, guarantor's perfume require high food, vegetable product etc., guarantee the quality
Phase relatively leads to common one times of packaging material length or more.
Existing film level nylon 6 slice is susceptible to fisheye and rupture of membranes in membrane process, and reason is in nylon 6 slice
Impurity component do not adapt to the deformation requirement during membrane, these ingredients are mainly cyclic dimer, cross polymers, carbide
And gel etc..During wound membrane, the film product to contact with each other is easy adhesion, influences to store and transport, typically in membrane
Increase filter, filter effect is general, influences yield, and membrane finished product excellence rate is not high.
Invention content
Problem to be solved by this invention is to overcome the shortcomings of the prior art, provide a kind of film level nylon 6 slice and
Its production method.
Nylon 6 is divided into injection grade, wire drawing grade, coating grade, transparent stage, health generally according to the difference of ingredient and performance
Grade, spinning-grade, fibre-grade, extrusion grade, flame retardant grade, booster stage, flexibilized grade, heatproof grade, cold-resistant grade, antibacterial grade, film-grade etc., no
6 product of nylon at the same level cannot be used with, generally require and carry out proprietary technological design according to requirements.In the present invention, film grade Buddhist nun
6 slice of dragon carries out exclusive design for the requirement of film product stretch processes, following compared to having with conventional nylon 6 slice
It is different：The relative viscosity control that film level nylon 6 is sliced in the present invention 3.2 ± 0.030, the control of viscosity deviation≤± 0.030,
The weight % of the weight % of hot water extractables content≤0.3, wherein cyclic dimer≤0.05, the weight of content of residual water≤0.04
% is measured, coloration is -5~-3.5 ± 1 degree.Relative viscosity is the viscosity of opposite 96% concentrated sulfuric acid.
In the present invention, the extraction water in pre-extracted tower and extraction tower recycles caprolactam by four-effect evaporation, is extracted
Concentrate, initial extraction water include 1-10 weight % caprolactams, and 87~96 weight % water, remaining is impurity, this part is miscellaneous
Matter is that product is caused to occur fisheye, major cause of failure in two-phase drawing process, and on the one hand extracting water recovering process can be with
Reduce the caprolactam unit consumption of production nylon 6 slice, save production cost, on the other hand, in extraction water there are it is a variety of cross polymers,
Colloid, carbide, the dimer of precipitation and other machinery impurity, when this partial impurities back to production initiating terminal, prepolymerization,
Polymerization stage can have adverse effect on the process of reaction afterwards.
Although extraction water can not be effectively reduced miscellaneous by improving the content of monomer caprolactam after evaporation and concentration
Matter ingredient finds that while concentrating monomer caprolactam, the proportion of impurity component increases instead in actual production.
For this purpose, applicant will extract after concentrate mixes with fresh caprolactam, while outer circulation, cyclic system are beaten with pumping
It is heated equipped with vapor heat exchanger in system, in the metal sintering for the difference alarming device with pressure that the outlet setting filtering accuracy of pump is 20u
Viscous filter, filter can switch online, and packed tower of the kettle top equipped with condensable reflux removes moisture removal, is purified in kettle by control
The temperature (100-140 DEG C) and pressure (45-55kpa) of melt, by purifying, the mixture water content control that kettle comes out is heavy in 5-30
% is measured, since most of impurity components bring reaction system by being dissolved in water, the water content by controlling mixture reaches
The purpose of impurity and purification.Temperature (100-140 DEG C) and pressure (45-55kpa) are preferred control condition, in this temperature and pressure
Under the conditions of, the solubility highest of impurity.
In the present invention, additive includes chain terminating agent, nucleating agent and anti-blocking agent but is not limited to three of the above, wherein being nucleated
Agent and anti-blocking agent are to meet the technological requirement of downstream product biaxial tension so that the film that biaxial tension obtains is in wound membrane
When do not stick together.
In the present invention, using gas from stirring depolymerizing reactor at high temperature under high pressure depolymerization extraction concentrate in it is oligomeric
Object, the pre-polymerization reactor carried out later is different with the reaction condition in polymer reactor, is high-pressure section in pre-polymerization reactor
Part, interior polymer reactor is condition of negative pressure, pressure Different Effects reaction process and product, and early period, pressure was higher, is more conducive to anti-
It should be carried out to positive direction, the later stage the low more is conducive to the water discharge that reaction generates, and promotes reaction, improves conversion ratio.
In the present invention, the bubble agitation that depolymerizing reactor is generated using moisture boiling has no need to install blender, saves
Cost-saving；Polymer reactor is stirred using scraping plate film formation, and moisture in polymer is made to be easy to evaporate, and reduces energy consumption.
In the present invention, what fondant filter removal generated in melt pipe and polymerization pipe crosses polymers, carbide and gel
Equal impurity, prevent the generation of fisheye and rupture of membranes during membrane.
In the present invention, slice discharges after carrying out pre-extracted in pre-extracted tower through Alfa Laval nozzle, compared to existing skill
Slush pump conveying technique in art can hit blade wheel of slurry pump to avoid slice and generate damaged and dust, solve unshrouded impeller
Slush pump is inefficient, waste of energy and slush pump are easily stuck by tape, need to frequently stop and cause production discontinuous, cause to be sliced
The problem of quality fluctuation.The impurity such as dimer, tripolymer in the effect of pre-extracted mainly extraction slice, extraction tower it is main
Effect extracts unreacted monomer, and the two is separated latter two extraction tower and tilted using different technique, and extraction is more targeted.
Conventional direct single extraction tower operation, the impurity such as dimer, tripolymer are compared in such a way that pre-extracted is combined with extraction tower
It can extract more thorough, content can be lower, is conducive to being smoothed out for later stage membrane, avoids fisheye and rupture of membranes.
Concrete scheme is as follows：
A kind of production method of film level nylon 6 slice, includes the following steps：
Step 1)：Caprolactam is heated to melting, caprolactam larger storage tank is sent into, adds to the caprolactam larger storage tank
Enter the extraction concentrate of purified treatment, the good additive of the liquid A and configured in advance obtained after homogenizing processing is sent into preheater, institute
State additive accounts for the liquid A gross weight 0.05~3%；
Step 2)：Preheater is heated to 90~150 DEG C, and resulting material is sent into cracking reactor, at 210~250 DEG C, 100
Simultaneously simultaneously addition polymerization, polycondensation reaction occur for material open loop under~300kpa, and the bubble generated using the boiling of material reaches stirring thing
The effect of material；
Step 3)：The material that step 2) is obtained is sent into pre-polymerization reactor, at 235~280 DEG C, under 100~300kpa
Material continues that addition polymerization, polycondensation reaction occurs, and the mixed vapour of generation is sent into packed tower and carries out spray recycling monomer caprolactam；
Step 4)：The material that step 3) is obtained is sent into polymer reactor, at 270~290 DEG C, material under 5~-70kpa
Continue to occur addition polymerization, polycondensation reaction, the mixed vapour of generation be sent into the packed tower described in step 3) carry out spray recycling monomer oneself
Lactams；
Step 5)：The material that step 4) is obtained is sent into fondant filter, removes the polymers excessively in material, carbide and coagulates
Glue carries out pelletizing, is sliced under water later；
Step 6)：The slice that step 5) is obtained is sent into pre-extracted tower, and setting pump forced circulation extracts in the pre-extracted tower
Water intaking, slice discharges after carrying out pre-extracted in pre-extracted tower through Alfa Laval nozzle, is in column in extraction tower into extraction tower
Plug flow is extracted, and is collected the extraction water in pre-extracted tower and extraction tower and is sent to extraction water evaporization process recycling caprolactam, obtains
To extraction concentrate described in step 1), the slice after the extraction of gained carries out centrifugal dehydration；
Step 7)：Step 6) centrifugal dehydration is obtained slice to be dried, film level nylon 6 slice is obtained after cooling.Into one
Step, purified extraction concentrate includes 70~95% caprolactams in the step 1), and 5~30% water extract concentrate
Account for the 10~35% of liquid A gross weight.
Further, additive includes chain terminating agent, nucleating agent and anti-blocking agent, wherein chain terminating agent in the step 1)
For benzoic acid, anti-blocking agent is silica, activated Calcium carbonate, talcum powder, barium sulfate, active titanic dioxide, acrylate
At least one of grain, polystyrene pellet, using liquid caprolactam as solvent.
Further, the step 1) includes 1a) it will be heated to melting after the crushing of solid caprolactam, it is sent into caprolactam
Larger storage tank, 1b) the solid caprolactam of 30~70 weight % is added into extraction concentrate, it stirs and dissolves each other in purification kettle, together
When with pump play outer circulation, heated equipped with vapor heat exchanger in the circulatory system, in the mistake of the outlet setting difference alarming device with pressure of pump
Filter, the top installation packed tower for purifying kettle remove moisture removal by condensing reflux, will purify the mixture water content control of kettle out
System is sent into caprolactam larger storage tank in 5-30 weight %, the liquid A obtained after homogenizing processing, 1c) match by liquid A and in advance
The additive set is sent into preheater.
Further, step 1b) described in vapor heat exchanger heating temperature be 100-140 DEG C, pressure difference warning device control
Pressing pressure is in 45-55kpa.
Further, monomer caprolactam is recycled in the step 3) in packed tower and is back to the cracking in the step 2)
Reactor.
Further, polymer reactor is stirred using scraping plate film formation in the step 4), mixing speed 50-200rpm.
Further, extraction water and chipping qualities ratio are 0.9~1.1 in pre-extracted tower in the step 6), in extraction tower
Extraction water is 0.9~1.1 with chipping qualities ratio.
Further, temperature dry in the step 7) is 120~140 DEG C, and the dry time is 24-60h.
The film level nylon 6 slice that the production method that the present invention also protects the film level nylon 6 to be sliced is prepared, phase
It is 3.2 ± 0.030 to viscosity, hot water extractables content is less than or equal to 0.3 weight %, and cyclic dimer content is less than or equal to
0.04%.
Advantageous effect：Film level nylon 6 slice production method of the present invention extracts condensed water by purification, and cooperation is split
Solution, pre-polymerization and polymerization technique design and fondant filter removal of impurities, pre-extracted tower and extraction tower separately extract, and solve extraction
Product stretches the fisheye occurred and breakage problem in water recovering process.Obtained film level nylon 6 slice relative viscosity is controllable
3.2 ± 0.030, the control of viscosity deviation is ≤± 0.030, the weight % of hot water extractables content≤0.3, wherein cyclic dimer
The weight % of object≤0.05, the weight % of content of residual water≤0.04, coloration is -5~-3.5 ± 1, has higher quality.
Specific implementation mode
Technical solution of the present invention is further elaborated with reference to embodiment.Particular technique or item are not specified in embodiment
Part person carries out according to technology or condition described in document in the art or according to product description.Agents useful for same or instrument
Production firm person is not specified in device, and being can be with conventional products that are commercially available.
Embodiment 1
The production method of film level nylon 6 slice includes the following steps：
Step 1)：It is heated to melting after solid caprolactam is crushed, it is big to obtain fresh caprolactam feeding caprolactam
Storage tank；The solid caprolactam of 50 weight % is added into extraction concentrate, stirs and dissolves each other in purification kettle, while being beaten outside with pump
It recycles, is heated equipped with vapor heat exchanger in the circulatory system, the filter of difference alarming device with pressure is set in the outlet of pump, controls and steams
The temperature of vapour heat exchanger heating is 120 DEG C, and pressure difference warning device control pressure purifies the top installation packed tower of kettle in 50kpa
Moisture removal is removed by condensing reflux, the mixture water content control of kettle out will be purified in 5 weight %, caprolactam content 90
Weight %, the mixture come out according to purification kettle：Fresh caprolactam mass ratio is 1:4 are sent into caprolactam larger storage tank；
Change the difference between processing adjustment different batches raw material, the good additive of obtained liquid A and configured in advance is sent into preheater, institute
It includes the chain terminating agent benzoic acid for accounting for liquid A gross weight 1% to state additive, accounts for the Conventional nucleating agents of liquid A gross weight 0.5%, accounts for liquid
The anti-blocking agent silica of body A gross weights 0.5%；
Step 2)：Preheater is heated to 90 DEG C, and resulting material is sent into cracking reactor, and at 210 DEG C, material is opened under 300kpa
Simultaneously simultaneously addition polymerization, polycondensation reaction occur for ring, and the bubble generated using the boiling of material achievees the effect that stir material；
Step 3)：The material that step 2) is obtained is sent into pre-polymerization reactor, and at 280 DEG C, material is after supervention under 300kpa
Raw addition polymerization, polycondensation reaction, the mixed vapour of generation are sent into packed tower and carry out reflux recycle-water, the remaining object of recycle-water in packed tower
Material is back to the cracking reactor in the step 2)；
Step 4)：The material that step 3) is obtained is sent into polymer reactor, and polymer reactor is stirred using scraping plate film formation, stirred
It is 150rpm to mix speed, and at 290 DEG C, material continues that addition polymerization, polycondensation reaction occurs under -30kpa, and the mixed vapour of generation is sent into step
It is rapid 3) described in packed tower carry out reflux recycling monomer；Wherein step 2) is total by depolymerization, open loop, polymerization to raw material in step 4)
Meter about 20 hours；
Step 5)：The material that step 4) is obtained is sent into fondant filter, removes the polymers excessively in material, carbide and coagulates
Glue carries out pelletizing, is sliced under water later；
Step 6)：The slice that step 5) is obtained is sent into pre-extracted tower, and setting pump forced circulation extracts in the pre-extracted tower
It fetches water, extraction water and chipping qualities ratio are 0.9 in pre-extracted tower:1, it is sliced after extracting about 5h in pre-extracted tower through Alfa Laval
Nozzle discharges, and into extraction tower, about 9h is extracted in plug flow in extraction tower, extraction water and chipping qualities ratio in extraction tower
It is 0.9:1, it collects the extraction water in pre-extracted tower and extraction tower and is sent to extraction water evaporization process recycling caprolactam, obtain step
1) the extraction concentrate extracts the monomer for containing about 5 weight % in concentrate, and it is de- that the slice after the extraction of gained carries out centrifugation
Water；
Step 7)：Step 6) centrifugal dehydration is obtained slice to be dried, 120 DEG C of dryings, 60 hours postcoolings obtain film grade
Nylon 6 slice.
Embodiment 2
The preparation process of film level nylon 6 slice is with embodiment 1, and difference lies in step 1) is added 70 into extraction concentrate
The temperature of the solid caprolactam of weight %, vapor heat exchanger heating is 140 DEG C, and pressure difference warning device control pressure is in 45-
55kpa, purification kettle come out the mixture being purified, the mixture that purification kettle comes out：Fresh caprolactam mass ratio is 1:2 send
Enter in caprolactam larger storage tank, obtain liquid A, additive includes the chain terminating agent benzoic acid for accounting for liquid A gross weight 1%, accounts for liquid A
The Conventional nucleating agents of gross weight 1% account for the anti-blocking agent active titanic dioxide of liquid A gross weight 1%；Preheater is heated in step 2)
150 DEG C, resulting material be sent into cracking reactor, at 230 DEG C, under 200kpa material open loop and simultaneously addition polymerization, polycondensation reaction occurs；
Pre-polymerization reactor temperature is 260 DEG C in step 3), 100kpa；The temperature of polymer reactor is 280 DEG C in step 4) ,-
The speed of 30kpa, scraping plate film formation stirring are 50-200rpm, and step 2) arrives raw material in step 4) and passes through depolymerization, open loop, polymerization altogether
Meter about 16 hours；Extraction water and chipping qualities ratio are 1 in pre-extracted tower in step 6):1, about 10h is extracted, extraction water in extraction tower
It is 1 with chipping qualities ratio:1, about 10h is extracted, the temperature dried in step 7) is 120~140 DEG C, and the dry time is 24-
60h。
Embodiment 3
The preparation process of film level nylon 6 slice is with embodiment 1, and difference lies in step 1) is added 30 into extraction concentrate
The temperature of the solid caprolactam of weight %, vapor heat exchanger heating is 100 DEG C, and pressure difference warning device control pressure is in 45-
55kpa will purify the mixture water content control of kettle out in 15 weight %, and purification kettle comes out the mixture being purified, only
Change the mixture that kettle comes out：Fresh caprolactam mass ratio is 1:2 are sent into caprolactam larger storage tank, obtain liquid A, additive
Chain terminating agent benzoic acid including accounting for liquid A gross weight 0.03%, accounts for the Conventional nucleating agents of liquid A gross weight 0.01%, it is total to account for liquid A
Weigh 0.01% anti-blocking agent talcum powder；Preheater is heated to 120 DEG C in step 2), and resulting material is sent into cracking reactor,
220 DEG C, under 200kpa material open loop and simultaneously addition polymerization, polycondensation reaction occurs；Pre-polymerization reactor temperature is 235 in step 3)
DEG C, 100kpa；The temperature of polymer reactor is 290 DEG C, -70kpa in step 4), and the speed of scraping plate film formation stirring is 50rpm, step
It is rapid 2) about 16 hours total by depolymerization, open loop, polymerization to raw material in step 4)；In step 6) in pre-extracted tower extraction water with cut
Tablet quality ratio is 0.9:1, about 10h is extracted, extraction water and chipping qualities ratio are 0.9 in extraction tower:1, extract about 10h.
Embodiment 4
The preparation process of film level nylon 6 slice is with embodiment 1, and difference lies in step 1) is added 60 into extraction concentrate
The temperature of the solid caprolactam of weight %, vapor heat exchanger heating is 130 DEG C, and pressure difference warning device control pressure is in 45-
55kpa will purify the mixture water content control of kettle out in 30 weight %, and purification kettle comes out the mixture being purified, only
Change the mixture that kettle comes out：Fresh caprolactam mass ratio is 1:2 are sent into caprolactam larger storage tank, obtain liquid A, additive
Chain terminating agent benzoic acid including accounting for liquid A gross weight 1%, accounts for the Conventional nucleating agents of liquid A gross weight 0.5%, accounts for liquid A gross weight
0.1% anti-blocking agent acrylate particles；Preheater is heated to 140 DEG C in step 2), and resulting material is sent into cracking reactor,
At 240 DEG C, under 300kpa material open loop and simultaneously addition polymerization, polycondensation reaction occurs；Pre-polymerization reactor temperature is 270 in step 3)
DEG C, 300kpa；The temperature of polymer reactor is 280 DEG C, -50kpa in step 4), and the speed of scraping plate film formation stirring is 200rpm；
It is about 16 hours total by depolymerization, open loop, polymerization that step 2) arrives raw material in step 4)；In step 6) in pre-extracted tower extraction water with
Chipping qualities ratio is 1.1:1, about 10h is extracted, extraction water and chipping qualities ratio are 1.1 in extraction tower:1, extract about 10h.
Comparative example 1
The present embodiment is substantially the same manner as Example 1, and difference lies in steps 1) in the present embodiment to be added into extraction concentrate
The solid caprolactam of 50 weight % is uniformly mixed obtained mixture and is sent into caprolactam larger storage tank, without purified treatment.
Comparative example 2
The present embodiment is substantially the same manner as Example 1, and difference lies in polymer reactors in the present embodiment step 4) to grasp for normal pressure
Make.
Comparative example 3
The present embodiment is substantially the same manner as Example 1, and difference lies in the materials for obtaining step 4) in the present embodiment step 5)
Underwater cutpellet is directly carried out, is operated without fondant filter.
Comparative example 4
The present embodiment is substantially the same manner as Example 1, and difference lies in carried out using conventional extraction tower in the present embodiment step 6)
Extracting operation, extraction water are 0.9 with chipping qualities ratio：1 ratio is extracted about 20 hours.
Performance comparison
Nylon 6 slice made from embodiment and comparative example is subjected to viscosity test, it is opposite using determination of ubbelohde viscometer
Viscosity (opposite 96% concentrated sulfuric acid).Hot water extractables assay is measured using extraction pot using difference weight method.Cyclic dimer
Assay is measured using digital refractometer.Content of residual water is measured using karl Fischer Moisture Meter.Colorimetric detection uses aberration
Instrument measures.Measurement result is shown in Table 1.
Nylon 6 slice product made from embodiment and comparative example is measured to stretching on same biaxially oriented film board
Intensity, elongation at break etc., stretching experiment testing standard ASTM638.Measurement result is shown in Table 2.
Commercially available slice is presently commercially available expensive goods in Tables 1 and 2.
1 nylon 6 slice performance test results table of table
2 nylon 6 slice biaxial tension test result table of table
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail can carry out a variety of simple variants to technical scheme of the present invention within the scope of the technical concept of the present invention, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case of shield, it can be combined by any suitable means.In order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (10)
1. a kind of production method of film level nylon 6 slice, it is characterised in that：Include the following steps：
Step 1)：Caprolactam is heated to melting, is sent into caprolactam larger storage tank, is added to the caprolactam larger storage tank net
Change the extraction concentrate of processing, the good additive of the liquid A and configured in advance obtained after homogenizing processing is sent into preheater, described to add
Agent is added to account for the 0.05~3% of the liquid A gross weight；
Step 2)：Preheater is heated to 90~150 DEG C, and resulting material is sent into cracking reactor, at 210~250 DEG C, 100~
Simultaneously simultaneously addition polymerization, polycondensation reaction occur for material open loop under 300kpa, and the bubble generated using the boiling of material reaches stirring material
Effect；
Step 3)：The material that step 2) is obtained is sent into pre-polymerization reactor, at 235~280 DEG C, material under 100~300kpa
Continue that addition polymerization, polycondensation reaction occurs, the mixed vapour of generation is sent into packed tower and carries out reflux recycling monomer caprolactam；
Step 4)：The material that step 3) is obtained is sent into polymer reactor, and at 270~290 DEG C, material continues under 5~-70kpa
Occur addition polymerization, polycondensation reaction, the mixed vapour of generation is sent into the packed tower described in step 3) and carries out reflux recycling monomer acyl in oneself
Amine；
Step 5)：The material that step 4) is obtained is sent into fondant filter, removes in material and crosses polymers, carbide and gel,
It carries out pelletizing under water later, is sliced；
Step 6)：The slice that step 5) is obtained is sent into pre-extracted tower, and pump forced circulation extraction water is arranged in the pre-extracted tower,
Slice discharges after carrying out pre-extracted in pre-extracted tower through Alfa Laval nozzle, is in plug flow in extraction tower into extraction tower
It is extracted, collects the extraction water in pre-extracted tower and extraction tower and be sent to extraction water evaporization process recycling caprolactam, walked
Rapid 1) the described extraction concentrate, the slice after the extraction of gained carry out centrifugal dehydration；
Step 7)：Step 6) centrifugal dehydration is obtained slice to be dried, film level nylon 6 slice is obtained after cooling.
2. the production method of film level nylon 6 slice according to claim 1, it is characterised in that：Purification in the step 1)
Aqueous 5~30 weight % of extraction concentrate afterwards, extraction concentrate account for the 10~35% of liquid A gross weight.
3. the production method of film level nylon 6 slice according to claim 1, it is characterised in that：Addition in the step 1)
Agent includes chain terminating agent, nucleating agent and anti-blocking agent, and wherein chain terminating agent is benzoic acid, and anti-blocking agent is silica, activity
At least one of calcium carbonate, talcum powder, barium sulfate, active titanic dioxide, acrylate particles, polystyrene pellet, with liquid
Intimate lactams is as solvent.
4. the production method of film level nylon 6 slice according to claim 1, it is characterised in that：The step 1) includes 1a)
It is heated to melting after solid caprolactam is crushed, is sent into caprolactam larger storage tank, 1b) it is added 30~70 into extraction concentrate
The solid caprolactam of weight % is stirred in purification kettle and is dissolved each other, while playing outer circulation with pump, is changed equipped with steam in the circulatory system
The filter of difference alarming device with pressure is arranged in the outlet of pump in hot device heating, and the top installation packed tower for purifying kettle passes through condensation
Moisture removal is removed in reflux, will purify the mixture water content control of kettle out in 5-30 weight %, is sent into caprolactam larger storage tank,
Obtained liquid A after homogenizing processing, 1c) the good additive of liquid A and configured in advance is sent into preheater.
5. the production method of film level nylon 6 slice according to claim 4, it is characterised in that：Step 1b) described in steam
The temperature of heat exchanger heating is 100-140 DEG C, and pressure difference warning device control pressure is in 45-55kpa.
6. the production method of film level nylon 6 slice according to claim 1, it is characterised in that：Filler in the step 3)
Monomer caprolactam is recycled in tower is back to the cracking reactor in the step 2).
7. the production method of film level nylon 6 slice according to claim 1, it is characterised in that：Polymerization in the step 4)
Reactor is stirred using scraping plate film formation, mixing speed 50-200rpm.
8. the production method of film level nylon 6 slice according to claim 1, it is characterised in that：Extract in advance in the step 6)
It is 0.9~1.1 to take extraction water and chipping qualities ratio in tower, and extraction water and chipping qualities ratio are 0.9~1.1 in extraction tower.
9. the production method of film level nylon 6 slice according to claim 1, it is characterised in that：It is dry in the step 7)
Temperature be 120~140 DEG C, the dry time be 24-60h.
10. the film grade nylon being prepared with the production method of the film level nylon 6 slice described in any one of claim 1-9
6 slices, relative viscosity are 3.2 ± 0.030, and hot water extractables content is less than or equal to 0.3 weight %, cyclic dimer content
Less than or equal to 0.04%.
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| CN110117360A (en) * | 2019-06-25 | 2019-08-13 | 福建中庚环境技术有限公司 | A kind of MC nylon industry metaplasia production complete set of equipments |
| CN110436692A (en) * | 2019-08-30 | 2019-11-12 | 温州邦鹿化工有限公司 | A kind of recycling concentration liquor treating process routinely spinning nylon 6 slice production for semi-gloss |
| CN111269412A (en) * | 2020-02-14 | 2020-06-12 | 东华大学 | Method for recycling caprolactam |
| CN114057621A (en) * | 2021-11-29 | 2022-02-18 | 东华大学 | Method for efficiently depolymerizing waste polyamide 6 and application thereof |
| CN114133558A (en) * | 2021-12-01 | 2022-03-04 | 江苏弘盛新材料股份有限公司 | Preparation method of anti-crystal-point film-grade nylon 6 slice |
| CN114230854A (en) * | 2021-12-01 | 2022-03-25 | 江苏弘盛新材料股份有限公司 | Method for recycling nylon-6 slices |
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2018
- 2018-05-30 CN CN201810538790.7A patent/CN108586728A/en not_active Withdrawn
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110117360A (en) * | 2019-06-25 | 2019-08-13 | 福建中庚环境技术有限公司 | A kind of MC nylon industry metaplasia production complete set of equipments |
| CN110436692A (en) * | 2019-08-30 | 2019-11-12 | 温州邦鹿化工有限公司 | A kind of recycling concentration liquor treating process routinely spinning nylon 6 slice production for semi-gloss |
| CN110436692B (en) * | 2019-08-30 | 2022-12-06 | 温州邦鹿化工有限公司 | Treatment process of recovered concentrated solution for producing semi-gloss conventional spinning nylon 6 slices |
| CN111269412A (en) * | 2020-02-14 | 2020-06-12 | 东华大学 | Method for recycling caprolactam |
| CN114057621A (en) * | 2021-11-29 | 2022-02-18 | 东华大学 | Method for efficiently depolymerizing waste polyamide 6 and application thereof |
| CN114133558A (en) * | 2021-12-01 | 2022-03-04 | 江苏弘盛新材料股份有限公司 | Preparation method of anti-crystal-point film-grade nylon 6 slice |
| CN114230854A (en) * | 2021-12-01 | 2022-03-25 | 江苏弘盛新材料股份有限公司 | Method for recycling nylon-6 slices |
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