CN203973820U - Device for the manufacture of homogeneous polyamide granules - Google Patents

Device for the manufacture of homogeneous polyamide granules Download PDF

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Publication number
CN203973820U
CN203973820U CN201420172559.8U CN201420172559U CN203973820U CN 203973820 U CN203973820 U CN 203973820U CN 201420172559 U CN201420172559 U CN 201420172559U CN 203973820 U CN203973820 U CN 203973820U
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valve
polyamide
pressure
cutting speed
polymer
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利恩·曼斯特
唐纳德·J·福斯特
康纳利斯·M·冯克
罗伯特·W·麦克奈尔
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Invista North America LLC
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Scientific & Technical Corp Of English Weida
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Abstract

The utility model provides the device for the manufacture of homogeneous polyamide granules, comprises HIGH PRESSURE TREATMENT container, cutter and process controller.Described container can comprise pressure controller and extrude valve.Described cutter is arranged on the downstream of extruding valve, and is configured to the polyamide polymer extruded from HIGH PRESSURE TREATMENT container of cutting to form polyamide granules.Described process controller can comprise the pressure control module being connected with pressure controller, for controlled pressure controller; The cutting speed module being connected with cutter, for controlling cutting speed; And with extrude the valve module of extruding that valve is connected, for controlling, extrude valve.Described device is configured to certain productive rate through extruding the bar of the polyamide extruded polymer of valve, and described bar is cut with certain cutting speed and manufactures the polyamide polymer of homogeneous in batches.

Description

Device for the manufacture of homogeneous polyamide granules
Technical field
The utility model relates to the device of the homogeneous particle of producing polyamide polymer.
Background technology
At the particular types fatty polyamide that repeats to have between amide units at least 85% aliphatic key, be described as nylon polyamide.Known these aliphatic polyamides are derivative from dicarboxylic acids and other derivative (as acid anhydrides, acid amides, acyl halide, half ester and diester) that can form the dicarboxylic acids of acid amides, conventionally react with primary amine or secondary amine.More specifically, by monomer (as dicarboxylic acids and diamines), form aliphatic polyamide polymers, known is by primary diamines or secondary diamine (being connected to the diamines at least on each nitrogen with a hydrogen) and dicarboxylic acids, maybe to be formed having reacted of derivative of the dicarboxylic acids of acid amides.The example of reaction process is as follows:
-[NH-R'-NH-CO-R-CO]- n-+nH 2O
Wherein R and R' represent bivalent hydrocarbon radical, and n represents the quantity of repetitive and the quantity of hydrone.
In group (R and R ') separately, the quantity of carbon atom is named " construction unit " of polymer derivative from a molecule of each diacid and diamines.Therefore,, by hexa-methylene-1, the polyamide of 6-diamines and adipic acid is " nylon 6,6 " (polyhexamethylene adipamide).
Fibre-forming polyamide can form the preparing of dicarboxylic acid derivatives of acid amides by (being generally 180 ℃ to 300 ℃) and heating the diamines of equimolar amounts substantially and dicarboxylic acids or heating under polycondensation reaction condition.This product has fiber and forms character, wherein can realize sufficiently high molecular weight.
The characteristic of a given polyamide can change in sizable scope, and may depend on molecular weight.To a certain extent, this polyamide characteristic is subject to the impact of the character of its end group, and this depends on excessive which kind of reactant that used, diamines or dicarboxylic acids.
Two features of fibre-forming polyamide relate to its high-melting-point and low solubility.Fibre-forming polyamide by being derived compared with the amine of simple types and acid institute is opaque solid always almost, and described opaque solid can melt or become transparent at a quite definite temperature.The fine polyamide of shape lower than its fusing point, when detecting with X ray, generally presents the positive evidence of the crystal structure of sharp-pointed X-ray crystal powder diffraction pattern, large bulk state.The density of these polyamide is conventionally between 1.0 and 1.2, and more specifically, the density of nylon 6,6 is considered to 1.14 gram per centimeters at present 3.
The same with other polycondensation products, polyamide generally comprises the separate unit of very approximate structure.The mean size of these separate units, the mean molecule quantity of polymer are deliberately controlled in certain limited field.Polymerisation is more further carried out, and mean molecule quantity (and inherent viscosity) will be higher.
If equimolar amounts is used reactant completely, under the condition that can make volatile products overflow, continue for a long time polymerization and heating, and can obtain the polyamide of very high molecular weight.Yet if the arbitrary reactant of excessive use, polymerization proceeds to certain a bit, then substantially stops.The time point that polymerization stops may depending on the amount of diamines or the binary acid (or derivative) of excessive use.
The easy method of preparing polyamide comprises: by mix diamines and the dicarboxylic acids of approximately chemical equivalent in liquid, prepare a salt, described liquid may be selected to be the poor solvent to product salt.If needed, can take by the solvent crystallization from suitable subsequently the salt of purifying separation from liquid.These diamines-dicarboxylates are crystalloid, and have definite fusing point.Their water solubles, and can from some alcohol and alcohol-aqueous mixtures, carry out crystallization easily.
From diamines-dicarboxylate, preparing fibre-forming polyamide can carry out in many ways.Do not having under the condition of solvent or diluent, and under the condition of the water generating, this salt can be heated to reaction temperature (180 ℃ to 300 ℃) in allowing to remove reaction.With it, manufacturing before the object of filament and other shape, may need polyamide to be placed under reduced pressure, for example, be equivalent under the absolute pressure of 50 to 300 millimetress of mercury (67 to 400 millibars).This can, before making polymer cure, complete by the emptying reactor of preparing polyamide very easily.
In the ordinary course of things, in above-mentioned polyamide forming process, necessarily require not add catalyst.For example, yet some phosphorous material (metal phosphinate hydrochlorate and phosphate) plays catalytic action to a certain extent as everyone knows.Use the catalyst adding sometimes to the material of preparing HMW, to give extra advantage.
The commercialization preparation of most of linear condensation things, polyamide is usually directed to heat monomer parent material, to cause the condensation of progressive polymer.This process is carried out in several stages conventionally, comprises in the middle of removing volatile matter and forms low-molecular-weight, low viscous polymeric liquid.At various vacuum and the time of staying and temperature, process this low-molecular-weight, low viscous polymeric liquid so that polymer can reach required final molecular weight and viscosity.
Although desired final molecular weight and viscosity generally can realize, the homogeneity that obtains consistent polymeric material during casting may go wrong.Therefore, finding and utilize multiple technologies manufacture to have the polymeric material of the homogeneity of improvement, is the progress in this area.
Utility model content
The utility model relates to the device for the production of homogeneous polyamide granules.In one embodiment, the device for the production of the homogeneous particle of polyamide polymer can comprise HIGH PRESSURE TREATMENT container, cutter and process controller.Described HIGH PRESSURE TREATMENT container can comprise extrude valve and pressure controller (as imported valve, discharge valve, heating component or except in autoclave for regulating any other device of extruding valve of pressure).Described cutter can be configured to the polyamide polymer extruded from HIGH PRESSURE TREATMENT container of cutting to form polyamide granules.Described process controller can comprise pressure control module for controlled pressure controller, for controlling the cutting speed module of cutting speed and for controlling the valve module of extruding of extruding valve.Described device can be configured to certain output by extruding the bar of the polyamide extruded polymer of valve, and with certain cutting speed, cuts described bar and become batch ground to manufacture a polyamide granules for homogeneous.Again, homogeneity is to measure the average quality of a collection of particle, and it is described average quality in 10% that described a collection of particle has the Individual Quality of at least 95% individual particles.In another embodiment, homogeneity is to measure the average quality of a collection of particle, and it is described average quality in 5% that described a collection of particle has the Individual Quality of at least 99% individual particles.
Accompanying drawing explanation
Below in conjunction with nonrestrictive accompanying drawing, understand better the utility model, wherein:
Figure 1A is according to the sectional view of the spendable HIGH PRESSURE TREATMENT container of embodiment of the present utility model;
Figure 1B is according to the sectional view of the spendable HIGH PRESSURE TREATMENT container of embodiment of the present utility model;
Fig. 2 is wherein according to the schematic diagram of the system of the spendable device of the present utility model of embodiment of the present utility model.
Fig. 3 is according to the figure of the sample casting of the polyamide of an embodiment of the present utility model.
The section weight that Fig. 4 is the target slice weight for the polyamide polymer by manufacturing according to the disclosed method of embodiment of the present utility model and output are than the figure of time.
The output of the standardization cutting speed that Fig. 5 is the target slice weight for the polyamide by manufacturing according to the disclosed method of embodiment of the present utility model/valve and the figure of AC pressure ratio time.
The section weight that Fig. 6 is the target slice weight for the polyamide by manufacturing according to the disclosed method of embodiment of the present utility model and output are than the figure of time.
The output of the standardization cutting speed that Fig. 7 is the target slice weight for the polyamide polymer by manufacturing according to the disclosed method of embodiment of the present utility model/valve and the figure of AC pressure ratio time.
Fig. 8 for for the particle weight of the polyamide polymer by manufacturing according to the control methods of embodiment of the present utility model and output than the figure of time.
It should be noted that above-mentioned figure is only the exemplary expression of embodiment of the present utility model, does not form any restriction by described figure to scope of the present utility model.
The specific embodiment
Although detailed description has below comprised a lot for the details of illustrating the purpose of this utility model, person of skill in the art will appreciate that a lot of variations of details below and be modified in the scope of embodiment disclosed in the utility model.
Therefore, embodiment has below illustrated the utility model without loss of generality, and the utility model is not brought to restriction.Before describing the utility model in more detail, be to be understood that the utility model is not limited to described specific embodiment, this is because this embodiment can change.It is also understood that the term that used is only for the object of describing specific implementations here, be not intended to limit, this is because scope of the present utility model is only limited to the appended claims.Unless otherwise prescribed, all technical terms and the scientific terminology that used here has the identical implication of implication of conventionally understanding with the those of ordinary skill in the art in field described in the utility model.
As the singulative " " and " this " that are used in this description and appended claim comprise plural object, unless context separately has clear and definite miscellaneous stipulations.Therefore, for example " polyamide " comprises multiple polyamide.
In the disclosure, " comprising ", " containing " and " having " etc. can have according to united states patent law gives their meaning and can mean " comprising " etc., and is conventionally interpreted as open term.Term " by ... form " be enclosed term, and only comprise the device listed especially, method, component, parts, structure, step etc. according to the meaning of united states patent law.When will " substantially by ... form " or when the device that comprises for the utility model such as " basic composition ", method, component, parts, structure, step etc., it relates to and the similar element of disclosure herein, but it can comprise extra building stone, form component, method step etc.But, with corresponding device disclosed herein, compound, method etc. Comparatively speaking, these extra devices, method, component, parts, structure, step etc. can not affect in fact foundation characteristic and the novel features of device, compound, method etc.In details more, when will " substantially by ... form " or when the device that comprises for the utility model such as " basic composition ", method, component, parts, structure, step etc., it has meaning and these terms according to united states patent law, given is open, as long as record basic or the content changing that novel features is not recorded by being greater than, it allows to be greater than recorded content and exists.When using open-ended term, during as " comprising " or " comprising ", should be appreciated that, as clearly state, also directly supported term " substantially by ... composition " and term " by ... composition ".
Term " polymerisable compound " or " polymerizable solution " refer to the component of adding according to the agitated autoclave of embodiment of the present utility model, when it processes in autoclave under specific temperature and pressure curve, formation can be extruded or be gathered in and polyamide polymer for further using.
Term " polyamide salt " refers to the salt being included in polymerisable compound (together with other additives), and described polymerisable compound provides the basic polymerizable material that is used to form polyamide polymer.If for example polyamide polymer is nylon 6,6, salt can be prepared by adipic acid and hexamethylene diamine.Other additive also can be present in polyamide solution, or introduces before reaction vessel, or is incorporated in reaction vessel.For example, conventionally titanium dioxide is introduced directly in container, yet before polymerisable compound is incorporated into container, introduces other additives, such as catalyst, fluorescent whitening agent, defoamer etc., although do not require this order or the even existence of these additives.
Term " cycle " relates to the stage of the batch polymerization processing mainly being limited by the pressure curve in container.Period 1 (cycle 1) occurs in the beginning of batch processed, and at this moment pressure is just raised to relatively high pressure from relatively low pressure.Occur in relatively high pressure is kept to a period of time second round (cycle 2).Period 3 occurs when (cycle 3) is reduced to relatively low pressure along with relatively high pressure.Period 4 (cycle 4) is along with relatively low pressure being kept to a period of time and occurring.Period 5 (cycle 5) is along with the polymer of preparation is extruded and occurred in container.The term " period 4 " that the utility model is used, " cycle 4 " and " cycle before casting " can replace mutually.
Phrase, such as " being suitable for providing ", " being enough to cause " or " being enough to produce " etc. relates to the reaction condition relevant to time, temperature, solvent, reactant density etc. in the context of synthetic technology, can change reaction condition so that the useful quantity of product or the output of product to be provided, this is in the scope of the experimenter's of this area common skill.Be, needed product is for being only that product or parent material are consumed completely with there is no need, and the needed product providing can separated or otherwise further use.
Should be understood that, ratio, concentration, amount or other data can be explained with the form of a scope here.It should be understood that using this range format is for convenience and simplicity.And therefore, should explain not only to comprise the data parameters clearly stating as the end points of scope in mode flexibly, and if each numerical value and subrange comprise " approximately ' X ' is to about ' Y ' ", also comprise all individual data parameters or be included in the subrange in described scope.In order to illustrate, the concentration range of " approximately 0.1% to approximately 5% " should be interpreted as, not only comprise that clearly approximately 0.1 % by weight of explanation is to the concentration of approximately 5 % by weight, be also included within single concentration in illustrated scope (for example 1%, 2%, 3% and 4%) and subrange (for example 0.5%, 1.1%, 2.2%, 3.3% and 4.4%).In one embodiment, term " about " can comprise according to the tradition of the significant digits of data parameters and rounding off.In addition, phrase " approximately ' X ' is to ' Y ' " comprises " approximately ' X ' arrives approximately ' Y ' ".
Here the term " about " used, when relating to data parameters or scope, it allows the variation to a certain degree in certain numerical value or scope, for example the end points of explained numerical value or the scope explained 10% with interior or on the other hand 5% with interior variation.
In addition, with enumerate or the mode of Ma Kushi group describe feature of the present utility model or aspect place, person of skill in the art will appreciate that, therefore also according to any single key element of the key element of Ma Kushi group or subbase group, the utility model has been described.For example, if the group that X is described to select free bromine, chlorine and iodine to form, as enumerated separately, claim and X that to have described X be completely bromine are the claim of bromine and chlorine.For example, feature of the present utility model or aspect according to this place of describing of enumerating, person of skill in the art will appreciate that, therefore also according to any combination of any single key element of the key element of Ma Kushi group or subbase group, the disclosure has been described.Therefore, if the group that X is described to select free bromine, chlorine and iodine to form, and Y would be described to the group of selecting free methyl, ethyl and propyl group to form, describes completely and supported that X is the claim that bromine and Y are methyl.
As used herein, all constituent contents provide with the form of percentage by weight, unless otherwise stated.When relating to component solution, percentage refers to the percentage by weight of the component that comprises solvent (for example water), except as otherwise noted.
As used herein, the molecular weight of all polymer (Mw) is weight average molecular weight, except as otherwise noted.
When reading the disclosure, it will be evident to one skilled in the art that, here each independent embodiment of describing and illustrate has independently parts and feature, these independently parts and feature be easy to any character separation of other several embodiments or in conjunction with and do not deviate from scope of the present utility model or spirit.
Conventionally, the device for the manufacture of homogeneous polyamide granules can comprise HIGH PRESSURE TREATMENT container, cutter and process controller.Described HIGH PRESSURE TREATMENT container can comprise pressure controller and extrude valve.Described cutter can be in the downstream of extruding valve, and can be configured to polyamide polymer that cutting extrudes from HIGH PRESSURE TREATMENT container to form polyamide granules.Described process controller can comprise the pressure control module for controlled pressure controller that is connected with pressure controller, be connected with cutter for the cutting speed module of controlling cutting speed with extrude that valve is connected for controlling the valve module of extruding of extruding valve.Described device can be configured to by the output with certain by extruding the bar of the polyamide extruded polymer of valve, and cuts with certain cutting speed the polyamide granules that described bar is manufactured a collection of homogeneous.Again, homogeneity is to measure the average quality of a collection of particle, and it is in 10% that described a collection of particle has at least 95% the Individual Quality of individual particles and the difference of described average quality.In another embodiment, homogeneity is to measure the average quality of a collection of particle, and it is in 5% that described a collection of particle has at least 99% the Individual Quality of individual particles and the difference of described average quality.
In another embodiment, device for the production of the homogeneous particle of polyamide polymer can comprise cutting tool, for the bar of the polyamide extruded to the proportional cutting speed cutting of output of polyamide with essence to realize the homogeneity of polymer beads; And adjustment instrument, for adjusting one or more technological parameters to keep the homogeneity of polyamide granules.More specifically, described device can comprise adjustment instrument, for adjusting the first technological parameter in response to the change of interchangeable the second technological parameter to keep the homogeneity of polyamide granules, described the first technological parameter selects free cutting speed, extrude the group that valve opening and container pressure form, described the second parameter choosing freely by cutting speed, extrude the group that valve opening and container pressure form.Homogeneity is to measure the average quality of a collection of particle, and it is described average quality in 10% that described a collection of particle has the Individual Quality of at least 95% individual particles.In another embodiment, homogeneity is to measure the average quality of a collection of particle, and it is described average quality in 5% that described a collection of particle has the Individual Quality of at least 99% individual particles.
It should be noted that each of these discussion can be considered to be applied in each embodiment, no matter whether it came into question clearly in the context of this embodiment when apparatus and method of the present utility model are discussed.Therefore, for example, when the polyamide polymer of discussing about described device, these discussion also can be used in interchangeable device, and vice versa.
Turn back to now device of the present utility model, generally, can in comprising the paradigmatic system of polyamide, use the utility model manufacture method, casting method, device etc.In one embodiment, polyamide polymer can comprise, substantially nylon 6,6, consists of, or consists of nylon 6,6.Nylon 6,6 can be straight polymer, or also can be modified by the additive of any amount, and described additive comprises fluorescent whitening agent, dyestuff etc.Usually, the manufacture method relating in the utility model can comprise continuous method and batch method, except as otherwise noted.These methods are carried out conventionally in reaction vessel, for example autoclave.In one embodiment, manufacture method can be a batch method.There is no particular limitation, and as described in the utility model, this batch of method is generally 5 periodic methods.
With reference to nylon 6,6, according to the typical batch of production scale of embodiment of the present utility model, can be about 1000Kg to about 3000Kg, and can, at a batch production period, in autoclave, circulate approximately 100 to 120 minutes particularly.Also can use batch production scale and time beyond above-mentioned scope, this depends on the selection of equipment and polymer, or other Considerations in those skilled in the technology concerned's ken.Generally, the salt that can be used as of the nylon of polyamide adds.In one embodiment, nylon can be nylon 6,6 salt, and the amount in can the scope of approximately 50 % by weight to 95 % by weight is present in polyamide.
In the polymerization of polyamide of the present utility model, can use kinds of processes parameter, comprise temperature and pressure.In one embodiment, temperature can be in the scope of approximately 190 ℃ to approximately 290 ℃, and the spontaneous pressure during some cycle or other pressure can be at approximately 250 pound per square inch absolute values (psia) to the scopes of approximately 300 pound per square inch absolute values (psia).In addition, in another embodiment, during some cycle, can under the vacuum condition of pressure that is less than 10torrg, heat.In certain embodiments, when in vacuum during the cycle, further heated polymerizable thing.Conventionally, as those skilled in the art will appreciate that after consideration the utility model, when polymer temperature is enough, can start vacuum process.In certain embodiments, spendable minimum pressure can be low to moderate about 150torra, for example about 200mbara.
Generally, the method for the present utility model for the production of polyamide granules can realize by autoclave and extrude/cutting process.In one embodiment, described method can or for example, start from the polyamide solution that provides the aqueous solution of the polyamide salt (nylon 6,6 salt) to high pressure container handling to prepare by concentrated slurry.Optionally, can dilute described slurry and become more concentrated by evaporation step.In one embodiment, can, according to the known method of prior art, from the aqueous solution of monomer hexamethylene diamine and adipic acid, prepare slurry.In another concrete embodiment, when nylon 6,6 monomer solutions are the form of caprolactam water solution, described slurry can contain a small amount of nylon 6 monomers.In one embodiment, HIGH PRESSURE TREATMENT container can be heated to subsequently approximately 230 ℃ (or other function temperature) and make inner spontaneous pressure rise.Optionally by delustering agent, titanium dioxide (TiO 2) inject autoclave and as the monomer mixture of water-borne dispersions.
Polyamide solution or multiviscosisty slurry mix can be heated to approximately 245 ℃ (or some other function temperature) subsequently in autoclave.When in this temperature, the pressure of autoclave can be reduced to atmospheric pressure, and by further reducing pressure by vacuum in a known way, to form daiamid composition.The described autoclave that maintenance contains daiamid composition under this temperature and/or pressure approximately 30 minutes.For example then this step is further heated to polyamide polymer composition approximately 285 ℃, and drying nitrogen is introduced to HIGH PRESSURE TREATMENT container in autoclave, and by introducing drying nitrogen to approximately 4 to the absolute pressure of the about 5bar described autoclave that pressurizes.
Polyamide polymer described in the utility model also can be prepared with catalyst.In one embodiment, in polyamide, can there is 10ppm(weight) to 1000ppm(weight) catalyst of amount in scope.On the other hand, catalyst can 10ppm(weight) to 100ppm(weight) amount in scope exists.Do not limit, the salt that catalyst can comprise phosphoric acid, phosphorous acid, hypophosphoric acid, arylphosphonic acid, arylphosphinic acid, these compounds with and composition thereof.In one embodiment, catalyst is sodium hypophosphite, manganese hypophosphite, phenyl sodium phosphite, phosphenylic acid sodium, phenyl potassium phosphite, phosphenylic acid potassium, diphenyl phosphorous acid hexamethylene diamine salt, tolyl potassium phosphite or its mixture.On the one hand, catalyst can be sodium hypophosphite.
Can improve according to the outward appearance whiteness of the disclosed polyamide of embodiment of the present utility model and daiamid composition by adding fluorescent whitening agent.These polyamide can show permanent whiteness and improve, and can be by keeping this whiteness to improve as the operation of thermal finalization.In one embodiment, in polyamide, can there is the fluorescent whitening agent of the amount in the scope of 0.01 % by weight to 1 % by weight.On the one hand, fluorescent whitening agent can be titanium dioxide.
In addition, can prepare these polyamide polymers with antioxidative stabilizer, antibacterial additives etc.In addition, can prepare polyamide polymer with antigassing additive.In one embodiment, in polyamide, can there is 1ppm(weight) to 500ppm(weight) scope in the antigassing additive of amount.
According to the disclosed polyamide polymer of embodiment of the present utility model, be born acid dyeable, but also can come these polymer of modification or copolymer by the copolymerization dye of positive ion in polymer, and convert it into basic dyeing form.These modifications make composition accept especially the dyeing with basic-dyeable fibre.
Forward now Figure 1A and 1B to, it has shown the cross sectional representation of two exemplary agitated autoclave.These figure are unnecessary to be drawn in proportion, and does not show each and all details common in agitated autoclave, but selects optionally to have shown schematically showing of the feature relevant especially to the utility model.Therefore, in the present embodiment, in figure separately, agitated autoclave 10 can comprise HIGH PRESSURE TREATMENT container 20 and agitator or spiral 22.Although shown agitator and spiral, it is dispensable.Described container comprises chamber wall 24, it typically is electroplating container wall, and described chamber wall and/or other structures is set to support heating component 26a and the 26b of one or more types.In the present embodiment, 26a has shown external jacket heating component, and 26b has shown inner heating component.It should be noted that the heating component in Figure 1A is placed in relatively close agitator place, this is more typical; And heating component in Figure 1B is placed in more close chamber wall place, this is more typical for non-agitating type autoclave.But, as described in, the position of heating element heater can lead to those skilled in the art is considering that the utility model determines afterwards.In another embodiment, two positions, all can there is heating element heater, near chamber wall with near agitator.
External jacket heating component 26a can be used for the raising polymerizable components that contains in container or the temperature of polymer, be attached to the inner surface of chamber wall and/or agitator and inner heating component 26b especially can be used for stoping polymer to become.As shown in Figure 1A, except having shown inner heating component, also have a pair of renewal rod (refresher bars), it works with novel polymer more together with central stirrer or spiral 22.Agitator work to be so that polymer is moved up along core, and when stirring the polymer of fusing, excellent by upgrade the polymer of fusing from sidewall surfaces removing polymer with described a pair of renewal.The heat transfer of this set in can improvement system, and can reduce the height of the eddy current being caused by agitator.
Although it should be noted that and schematically show inner heating component 26b on sectional view, it will be appreciated that the inside heating component that can use any shape or structure.It is also to be noted that described heating component can be constructed or be arranged to portability any fluid of the prior art (comprising gas and/or liquid), is used to autoclave that heat is provided.Also shown imported valve 28 and autoclave air vent 30, and described imported valve 28 and autoclave air vent 30 can be used as pressure controller and use or use separately (with heating component 26a together with 26b, it also can controlled pressure) together with coming.Do not show pressue device or pressure source, still will be understood that when wanting impressed pressure and can have described pressue device or pressure source.Or, intelligible as this area, can increase pressure by adding heat, and by the emptying pressure that reduces.Further, the bottom of HIGH PRESSURE TREATMENT container is valve openings 32.This figure do not show and extrudes valve, but this to be the polymer prepared in autoclave be extruded for the further position of processing.It is also to be noted that, as will be understood by the skilled person in the art, regardless of the description of these imports, valve, air vent etc. and the position of demonstration, with shown comparing, can use these or other port, for any object of user design differently.
It should be noted that and provide this exemplary HIGH PRESSURE TREATMENT container that forms polyamide polymer in autoclave only for exemplary object, as producing polyamide polymer with other technical process, autoclave and additive of any amount.No matter how polymer is prepared in autoclave, this point in the method for describing is generally main purpose of the present utility model, casts the polymer from aggregation container.
As described in the utility model, the utility model provides the polyamide polymer of extruding by cutting and has adjusted the apparatus and method that kinds of processes parameter forms the homogeneous particle of polyamide polymer.Especially, device of the present utility model allows to regulate the first technological parameter in response to the change of above-mentioned other a kind of technological parameter, and described the first technological parameter comprises cutting speed, extrudes valve opening and container pressure.In addition, on the one hand, can adjust two technological parameters in response to the 3rd technological parameter.In one embodiment, although adjustable any technological parameter or two technological parameters, the technological parameter being conditioned can be or can comprise container pressure.On the other hand, the technological parameter being conditioned can be maybe can comprise and extrude valve opening.On the other hand, the technological parameter being conditioned can be maybe can comprise cutting speed.
Forward now Fig. 2 to, device for the manufacture of homogeneous polyamide granules can comprise container 20, as being similar to the autoclave as shown in Figure 1A and/or Figure 1B, described container 20 comprises pressure controller (it can be the form of inlet line/valve 28, discharge pipe/valve 30 and/or heating component 26).Although it should be noted that the heating component that has shown external jacket, can replace with or increase inner heating component.Also shown and extruded valve 34 for what polymer was extruded to structure extrudes by Die and mould plate or other.Described device also can comprise cutter 36, and described cutter is configured to have the cutting speed of the polyamide granules that is applicable to cutting homogeneous.For example, described cutter can be revolution cutter, and it is configured to cut very fast during by it when the polymer being extruded.Described device also can comprise process controller 60, and it can comprise pressure control module 70, cutting speed module 80 and extrude valve module 90.Described device also can comprise plate 38, slurry collection equipment 40, slurry pipeline 42 and drier/circulator 44.
In the further description of the process controller 60 about described device, can automatically implement with multiple module 70,80,90 general utility functions or the processing step of automation equipment.For example, can control imported valve 28, autoclave ventilating opening 30 and heating component 26 by pressure control unit 70, with the adjusting of authorized pressure.Can control cutter 36 by cutting speed module 80.Can control and extrude valve 34 by extruding valve module 90.Other module (not shown)s that can exist, include but not limited to agitator module, drier module, heating component module etc.Described module can be worked simultaneously, to cause the mode of the polyamide granules of homogeneous that automated system is provided.
Fig. 3 has set forth the figure of explanation embodiment, and in an embodiment, these modules are worked simultaneously and realized the remarkable homogeneity according to embodiment of the present utility model.Particularly, Fig. 3 has illustrated the casting figure according to the technological parameter of the device of embodiment of the present utility model.Particularly, this figure provides during casting as the autoclave pressure of passing through single batch casting method of the function of time, from the output of the polyamide polymer of autoclave, has linearizingly extruded valve figure, and cutting speed.As shown in the figure, regulate kinds of processes parameter that substantially invariable output is provided under high cutting speed, and the automatic mode that also keeps high throughput rate when keeping particle homogeneity is provided thus.
In the chart of Fig. 3, also should be noted that and changed cutting speed, and cutting speed and output is substantially proportional,, when output rises or decline (as shown in the chart), cutting speed rises equally respectively and declines.Because term " substantially " relates to output or relative coupling proportional with cutting speed, it may be defined as any matching degree, under this matching degree, the average quality of a collection of particle of homogeneous is that to have the Individual Quality of at least 95% individual particles be described average quality to described a collection of particle in 10%.By basic coupling cutting speed, to the relatively moving of output, can keep homogeneity.As a result, pressure controller has kept output in rational scope with the use of extruding valve, for realizing effective sectility face.For example, in the efficient system of the high yield providing in the pressure by applicable and linear valve aperture, cutting speed can be carried out to relative coupling with output.Should notice that cutting speed also rises when output rises.
Turn back to Fig. 2, as described in the utility model, the pressure of container 20 can be spontaneous, or can generate from external pressure source.In addition, can regulate pressure with heat, pressure source (not shown) and/or air vent 30.Extrude valve 34 general control apertures, polyamide polymer is extruded from described opening.In some respects, extrude valve opening and can be called as the linear aperture of extruding valve." linearity " used herein refer to be equivalent to described valve opening (opening region) than the mathematic(al) manipulation of the percentage of the material of extruding by opening.For example, " linearity " aperture of 50% refers to from 100%(100% and refers to the heap(ed) capacity while opening valve completely) total amount in from opening, extrude 50% material, even if valve opening (opening region) the obtained aperture that may not be 50%.It should be noted that when valve and do not set and approach 100% while opening, have the control of the output of more polyamide polymer far away.When valve proximity 70% or 80% aperture, the control of output is significantly reduced.For example, the aperture of valve is changed to 50% pair of output from 40% and there is relatively significant effect, and valve is reached to 90% pair of output from 80%, there is very little effect.Therefore, it is desirable to keep valve as far as possible in the scope of approximately 30% to 70% aperture, and more typically during polymer casting process, remain in 35% to 60% scope.In order to complete this target, can change pressure and/or cutting speed and keep valve opening in the preferred range.Although described these, these are not what be strict with.This has been to provide a kind of mechanism, to keep the maximum flexibility about the aperture of squeezing valve.
Be back to the multiple adjusting of technological parameter, can in response to the variation of other technological parameters, carry out the adjusting of described kinds of processes parameter, should be noted that the adjusting of technological parameter can be carried out successively or simultaneously (or carrying out successively) within the overlapping time.In one embodiment, can regulate in response to the variation of the 3rd technological parameter more than one technological parameter.In order to provide embodiment to illustrate that why these technological parameters can benefit from change, once should be noted that from HIGH PRESSURE TREATMENT container and start extrusion, the polyamide polymer conventionally wherein containing does not also finish its polymerization process completely.Therefore, polyamide polymer can continue further multiviscosisty during extrusion.Have been found that under this condition and can not keep simply output and prior particle homogeneity by independent increase pressure.Similarly, only further open and extrude valve 34 and also can always not make up fully the polymer of multiviscosisty.In addition,, even by controlling together two in these parameters, adjust cutting speed if not the variation based on output, the homogeneity of polyamide granules also can suffer damage.
About described adjusting, device of the present utility model allows the more effective adjusting to output, and mates to provide the former homogeneity not realizing in conjunction with cutting speed and output.Particularly, there are two variablees that affect actual production: i) extrude valve opening, the raising of aperture causes the raising of output, and ii) autoclave pressure, the raising of autoclave pressure also causes the raising of output.Extrude valve opening and be applicable to the measured output of Fast Correction.But, by the aperture of four corner, keep constant output normally very limited.In addition,, while reducing autoclave pressure during casting, in autoclave, may there is the significant bubble of polymer.This makes autoclave pressure be not suitable as the Main Means of controlling output.In order to overcome these two, become quantitative limitation, with valve, export to control output.Then, each valve opening is exported when above in the target limiting, and just further increases the pressure of autoclave.With a plurality of variablees, control output more efficient than conventional art far away.Further, embodiment of the present utility model allows cutting speed to mate to provide the particle homogeneity that there is no realization before with output.
Therefore, device of the present utility model comprises by the pressure, the valve opening of variation and the cutting speed of variation that change controls productive rate, and therefore controls particle homogeneity, realizes the particle of homogeneous with effective means.Therefore, in a specific embodiment, exemplary output can be in the scope of 2 to 10 tphs or 5 to 9 tphs, or more particularly, 6 to 8 tphs.Exemplary pressure during extruding can be at 0 to 12 bar, 1 to 10 bar, or in the scope of 5 to 10 bar.Exemplary valve opening level can be in 30% to 70% scope, or in 45% to 65% scope.Use the exemplary cutting speed of helical cutters or other similar rotary cutters in 100 to 2000RPM scope, 400 to 1800RPM, or in 600 to 1500RPM scope.Conventionally, during casting, these technological parameters are remained within the scope of these, and by adjust described parameter within the scope of these, can realize the homogeneity of polyamide granules.Although stated above-mentioned these, also can use the technological parameter beyond these scopes, as long as can keep as particle homogeneity described in the utility model.
Can by extruding valve 34 apertures, control output at least in part, can control cutting speed by cutter 36, and can come controlled pressure to control output by one or more pressure controllers 26,28,30.Although adjustable, surpass the homogeneity that a technological parameter maintains polyamide granules, in a concrete embodiment, pressure and/or cutting speed can allow operation in linear aperture is 30% to 70%, 35 to 65% or 40% to 60% scope to extrude valve.In addition, for desirable efficiency is provided, in one embodiment, in large system, output can be at least 5 tons/hour, or at least 7 tons/hours, and adjusting process parameter can maintain target output and changes in interior scope at 10 quality %.
Process controller 60 is generally connected with container network with cutter 36 by computer, other computing equipments or other network equipments.Device of the present utility model can be the automatics of using multiple module.In one embodiment, in response to cutting speed or the change of extruding the aperture of valve 34, pressure control module 70 capable of regulating pressure controllers 26,28,30.On the one hand, in response to cutting speed and the change of extruding the aperture of valve, pressure control module capable of regulating pressure controller.In another embodiment, in response to pressure or the change of extruding the aperture of valve, the cutting speed of cutting speed module 80 capable of regulating cutters 36.On the one hand, in response to pressure and the change of extruding the aperture of valve, cutting speed module capable of regulating cutting speed.In another embodiment, in response to the change of cutting speed or pressure, extrude valve module capable of regulating and extrude valve.On the one hand, in response to the change of cutting speed and pressure, extrude valve module capable of regulating and extrude valve.Similarly, module of the present utility model can be worked through process controller simultaneously, during casting, to be enough to provide the mode of the polyamide granules of consistent and homogeneous to carry out adjusting process parameter.
As further instruction, for example, in order to contribute to be identified for technological parameter (pressure, valve opening, the activity of proper level and cutting speed), can carry out forecast production based on any amount of technology, described technology comprises the assessments such as assessment of using optical evaluation, operating weight and/or volume assessment (in container and/or after extruding), the Energy Transfer based on the relevant polymer being extruded casting water around.Concrete reference energy transmission technology, this casting method can comprise to be used casting production forecast or distributes for the dynamic value of the production adjusting process parameter at polyamide granules.For example, assessment casting output can comprise temperature and the flow velocity of measuring casting water, so calculates heat transmission associated with casting output subsequently.
As further instruction, in order more specifically to emphasize the independence of its enforcement, some functional units of describing in this description are called as " module ".For example " module " can be to implement as hardware circuit, described hardware circuit comprises the semiconductor can be purchased off the shelf, transistor or other discrete elements of super large-scale integration (Very Large Scale Integration, the VLSI) circuit of customization or grid array, for example logic chip.Module can also be implemented on programmable hardware device, such as field-programmable grid array, programmable logic array, PLD etc. of described programmable hardware device.Module also can implemented for the software of carrying out by polytype processor.The module of the identification of executable code for example can comprise one or more blocks of computer instructions, and it can be used as object, program or function and organize.Yet the executable code of the module of identification does not need physically together, but can comprise the different instruction that is stored in diverse location, described diverse location comprises module, and when logic links together, realizes the above-mentioned object for module.
In fact, the module of executable code can be single instruction or a lot of instruction, and is even distributed in several different code fragments, between distinct program and cross over several memory devices.Similarly, in module, can and described operating data be described in this identification, and can any suitable form embody operating data, and organize described operating data by the data structure of suitable type.Can individual data set collect operating data, or can be in different position distribution operating datas, described different position comprises different storage device.Described module can be passiveness or positive, comprises the medium that can operate to carry out required function.
Embodiment
Embodiment 1-polyamide granules #1
In the commercially available autoclave of nylon 6,6 each cycles that are 1200kg in production capacity, be filled with the aqueous solution of adipic acid and hexamethylene diamine.Temperature is risen to 280 ℃ from 150 ℃, and implement polymerization according to circular treatment.As shown in Figure 4, control the chipping qualities that output and cutting speed provide homogeneous.Target slice quality is 23mg/ particle.Significantly, the figure of Fig. 4 has shown that the maximum deviation of section weight is for to be less than about 0.5mgr with respect to target slice weight, has obtained the homogeneity of approximately 97.8% during whole service process.As shown in Figure 5, by controlling cutting speed, valve output and autoclave (autoclave, AC) pressure, realize this homogeneity.
Embodiment 2-polyamide granules #2
In the commercially available autoclave of nylon 6,6 each cycles that are 1200kg in production capacity, be filled with the aqueous solution of adipic acid and hexamethylene diamine.Temperature is risen to 280 ℃ from 150 ℃, and implement polymerization according to circular treatment.As shown in Figure 5, control the chipping qualities that output and cutting speed provide homogeneous.Target slice quality is 28mg/ particle.Significantly, the figure of Fig. 6 has shown that the maximum deviation of section weight is for to be less than about 0.75mgr with respect to target slice weight, has obtained the homogeneity of approximately 97.3% during whole service process.As shown in Figure 5, by controlling cutting speed, valve output and autoclave (autoclave, AC) pressure, realize this homogeneity.
The polyamide granules of the non-homogeneous of embodiment 3-
By being filled with the aqueous solution of adipic acid and hexamethylene diamine, prepare autoclave.Temperature is risen to 280 ℃ from 150 ℃, and implement polymerization according to circular treatment.As shown in Figure 8, contrary with the utility model, with static cutting speed, pressure and valve, export to process particle, obtained the just profound curve of chipping qualities as the function of casting time.Significantly, when target slice quality is 23mgr/ particle, maximum deviation surpasses 5mg, causes being less than 78% homogeneity.
Although, with for architectural feature and/or the theme of the present utility model that operated specific language description, it should be understood that, the theme being limited by the accompanying claims is not necessarily limited to specific feature as described above and operation.But above-described specific feature and action are disclosed as the exemplary form implementing the claims.Can carry out a plurality of improvement and substituting setting and not depart from the spirit and scope of described technology.

Claims (7)

1. for the manufacture of a device for the polyamide granules of homogeneous, comprising:
HIGH PRESSURE TREATMENT container, comprising:
Pressure controller, and
Extrude valve;
Be arranged on the cutter of extruding valve downstream, be applicable to the polyamide polymer extruded from HIGH PRESSURE TREATMENT container of cutting to form polyamide granules; And
Process controller, comprising:
The pressure control module being connected with pressure controller, for controlled pressure controller,
The cutting speed module being connected with cutter, for controlling cutting speed; And
With extrude the valve module of extruding that valve is connected, for controlling, extrude valve,
Wherein, configure described device by with certain productive rate through extruding the bar of the polyamide extruded polymer of valve, and described bar cut with certain cutting speed and manufacture the polyamide granules of homogeneous in batches.
2. device according to claim 1, is characterized in that, described container is non-agitated autoclave.
3. device according to claim 1, is characterized in that, described container is agitated autoclave.
4. device according to claim 1, is characterized in that, described process controller comes network to be connected in described cutter and described container by computer.
5. device according to claim 1, is characterized in that, described pressure controller comprises one or more discharge valves, imported valve or heating component.
6. device according to claim 1, is characterized in that, described process controller keeps 30% to 70% the linear aperture of extruding valve.
7. device according to claim 1, is characterized in that, described polyamide polymer is nylon 6,6.
CN201420172559.8U 2013-05-01 2014-04-10 Device for the manufacture of homogeneous polyamide granules Expired - Lifetime CN203973820U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104129009A (en) * 2013-05-01 2014-11-05 英威达科技公司 Polyamide casting for producing uniform pellets
CN109015434A (en) * 2018-07-05 2018-12-18 盐城市丰实金属磨料有限公司 A kind of nylon ball and preparation method thereof and purposes

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104129009A (en) * 2013-05-01 2014-11-05 英威达科技公司 Polyamide casting for producing uniform pellets
CN104129009B (en) * 2013-05-01 2018-07-03 英威达纺织(英国)有限公司 For producing the casting of the polyamide of uniform particle
CN109015434A (en) * 2018-07-05 2018-12-18 盐城市丰实金属磨料有限公司 A kind of nylon ball and preparation method thereof and purposes

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