CN104129009B - For producing the casting of the polyamide of uniform particle - Google Patents
For producing the casting of the polyamide of uniform particle Download PDFInfo
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- CN104129009B CN104129009B CN201410143762.7A CN201410143762A CN104129009B CN 104129009 B CN104129009 B CN 104129009B CN 201410143762 A CN201410143762 A CN 201410143762A CN 104129009 B CN104129009 B CN 104129009B
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- cutting speed
- pressure
- valve
- polyamide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/12—Making granules characterised by structure or composition
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
- B29B7/58—Component parts, details or accessories; Auxiliary operations
- B29B7/72—Measuring, controlling or regulating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/74—Mixing; Kneading using other mixers or combinations of mixers, e.g. of dissimilar mixers ; Plant
- B29B7/7461—Combinations of dissimilar mixers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
- B29B7/34—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
- B29B7/38—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/80—Component parts, details or accessories; Auxiliary operations
- B29B7/88—Adding charges, i.e. additives
- B29B7/90—Fillers or reinforcements, e.g. fibres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
- B29B9/065—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion under-water, e.g. underwater pelletizers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/12—Making granules characterised by structure or composition
- B29B9/14—Making granules characterised by structure or composition fibre-reinforced
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/06—Polyamides derived from polyamines and polycarboxylic acids
Abstract
The present invention provides for providing the method and apparatus of uniform polyamide granules.In one embodiment, the method for producing the uniform particle of polyamide polymer may include following steps：The polyamide polymer bar of extrusion is cut with the essence cutting speed proportional to the yield of polyamide polymer, to realize the homogeneity of polymer beads；And one or more technological parameters are adjusted to keep the homogeneity of polyamide granules.
Description
Technical field
The present invention relates to the method for the uniform particle of production polyamide polymer and for manufacturing uniform polyamide
The device of grain.
Background technology
Particular types fatty polyamide at least 85% aliphatic key between amide units are repeated is described as Buddhist nun
Imperial polyamide.These known aliphatic polyamides are the derivatives from dicarboxylic acids and other dicarboxylic acids for forming amide（Such as
Acid anhydrides, amide, acyl halide, half ester and diester）It is derived, is usually reacted with primary amine or secondary amine.More specifically, by monomer（Such as
Dicarboxylic acids and diamines）To form aliphatic polyamide polymers, it is known that be by primary diamines or secondary diamine（It is connected on each nitrogen at least
There are one the diamines of hydrogen for tool）It reacts to complete with the derivative of dicarboxylic acids or the dicarboxylic acids that amide can be formed.Reaction stream
The example of journey is as follows：
HOOC-R-COOH+H2N-R'-NH2
-[NH-R'-NH-CO-R-CO]-n-+nH2O
Wherein R and R' represents bivalent hydrocarbon radical, and n represents the quantity of repetitive unit and the quantity of hydrone.
By respective group（R and R '）The quantity of middle carbon atom is spread out to name from a molecule of each diacid and diamines
" structural unit " of raw polymer.Therefore, it is " nylon 6,6 " by the polyamide of hexa-methylene -1,6- diamines and adipic acid（It is poly-
Hexamethylene adipamide）.
Fibre-forming polyamide can be by under the conditions of polycondensation reaction（Generally 180 DEG C to 300 DEG C）Heating substantially etc. rubs
The diamines and dicarboxylic acids of your amount or heating can form preparing for the dicarboxylic acid derivatives of amide.The product is formed with fiber
Property, wherein sufficiently high molecular weight can be realized.
The characteristic of one given polyamide can change, and be likely to be dependent on molecular weight in sizable range.
To a certain extent, which is influenced by the property of its end group, and this depends on which kind of has been excessively used
Reactant, diamines or dicarboxylic acids.
Two features of fibre-forming polyamide are related to its high-melting-point and low solubility.Derived by the amine compared with simple types and acid
And almost always opaque solid, the opaque solid can be at a quite determining temperature for the fibre-forming polyamide come
It melts or becomes transparent.Less than the shape fibre polyamide of its fusing point, when with X-ray detection, sharp X-ray is generally presented
Crystal powder diffraction pattern, bulk state crystal structure positive evidence.The density of these polyamide usually 1.0 and 1.2 it
Between, more specifically, the density of nylon 6,6 is presently believed to be 1.14 gram per centimeters3。
The same with other polycondensation products, polyamide generally comprises the separate unit of very approximate structure.These separate singles
The mean size of member, the average molecular weight of polymer are deliberately controlled in the range of certain limitation.Polymerisation is more into one
Step carries out, average molecular weight（And inherent viscosity）It will be higher.
If complete equimolar amounts uses reactant, under conditions of it may be such that volatile products effusion, long lasting for
Polymerization and heating, and the polyamide of very high molecular weight can be obtained.However, if any reactant is excessively used,
Polymerization proceeds to certain point, then substantially stops.The time point that polymerization stops is likely to be dependent on the diamines being excessively used or two
First acid（Or derivative）Amount.
A kind of easy method for preparing polyamide includes：By the diamines and dicarboxyl that mix about chemical equivalent in a liquid
Acid prepares salt, and the liquid may be selected to be the poor solvent to product salt.It if desired, then can be by from suitable solvent
It crystallizes to purify the salt detached from liquid.These diamines-dicarboxylates are crystalloid, and have determining fusing point.They can
Water is dissolved in, and can easily be crystallized from certain alcohol and alcohol-aqueous mixtures.
Fibre-forming polyamide is prepared from diamines-dicarboxylate to carry out in many ways.In no solvent or diluent
Under the conditions of existing, and under conditions of the water generated during removal is allowed to react, which can be heated to reaction temperature（180℃
To 300 DEG C）.Before filament and other shapes of object being manufactured using it, it may be necessary to polyamide is placed under reduced pressure,
For example, it is equivalent to 50 to 300 millimetress of mercury（67 to 400 millibars）Absolute pressure under.This can lead to before polymer is cured
It crosses emptying and prepares the reaction kettle of polyamide very easily to complete.
Under normal circumstances, it necessarily requires not add catalyst in above-mentioned polyamide forming process.It is well known, however, that
Certain phosphorous materials（Such as metal phosphinate hydrochlorate and phosphate）Play a degree of catalytic action.Use the catalyst of addition
Sometimes the advantages of additional is imparted to the material for preparing high molecular weight.
The commercialization preparation of most of linear condensation objects, polyamide is usually directed to heating monomer starting material, to cause gradually
Into polymer condensation.This process usually carries out in several stages, including forming low point by removing volatile matter come intermediate
The polymeric liquid of son amount, low viscosity.Various vacuum degrees and residence time and at a temperature of handle the low molecular weight, low viscosity
Polymeric liquid is so that polymer can reach required final molecular weight and viscosity.
Although desired final molecular weight and viscosity can generally be realized, consistent gather is being obtained during casting
The homogeneity of condensation material is it is possible that problem.Thus, it is found that and there is improved homogeneity to manufacture using multiple technologies
Polymeric material is the progress in this field.
Invention content
The present invention relates to for producing the method and apparatus of uniform polyamide granules.In one embodiment, for giving birth to
The method for producing the uniform particle of polyamide polymer may include following steps：With substantially with the yield of polyamide polymer into than
The cutting speed of example cuts the bar of the polyamide polymer of extrusion, to realize the homogeneity of polymer beads；And it adjusts
Whole one or more technological parameter is to keep the homogeneity of polyamide granules.More specifically, the method includes in response to that can replace
The change of second technological parameter in generation adjusts the first technological parameter to keep homogeneity, and first technological parameter is selected from by cutting
The group that speed, extrusion valve opening and container pressure are formed is cut, second parameter is selected from by by cutting speed, extrusion valve
The group that door aperture and container pressure are formed.Homogeneity is to measure the average quality of a collection of particle, and a batch particle has
The Individual Quality of at least 95% individual particles is within the 10% of the average quality.In another embodiment, homogeneity is
The average quality of a collection of particle is measured, the Individual Quality of a batch particle at least 99% individual particles is described average
Within the 5% of quality.
In another embodiment, it is a kind of for the device that manufactures uniform polyamide granules may include high pressure processing vessels,
Cutter and process controller.The high pressure processing vessels may include squeezing out valve and pressure controller（Such as imported valve, discharge
Any other device of valve, heating component or the extrusion valve in addition to being used to adjust pressure in autoclave）.The cutter
It can be configured to the polyamide polymer that cutting squeezed out from high pressure processing vessels to form polyamide granules.The process controller can
Including being used for the pressure control module of control pressure controller, for the cutting speed module that controls cutting speed and for controlling
Squeeze out the extrusion valve module of valve.Described device may be configured to certain yield by squeezing out the polyamide extruded polymerization of valve
The bar of object, and the bar is cut with certain cutting speed and manufactures uniform polyamide to manufacture in batch
Grain.Again, homogeneity is to measure the average quality of a collection of particle, of a batch particle at least 95% individual particles
Weight is within the 10% of the average quality.In another embodiment, homogeneity is to measure the average matter of a collection of particle
Amount, the Individual Quality of a batch particle at least 99% individual particles are within the 5% of the average quality.
Description of the drawings
The present invention is more fully understood below in conjunction with unrestricted attached drawing, wherein：
Figure 1A is the sectional view of the high pressure processing vessels according to workable for the embodiment of the present invention；
Figure 1B is the sectional view of the high pressure processing vessels according to workable for the embodiment of the present invention；
Fig. 2 is the wherein schematic diagram of the system of workable the device of the invention according to an embodiment of the invention.
Fig. 3 is the figure cast according to the sample of the polyamide of an embodiment of the invention.
Fig. 4 is the target of polyamide polymer for being manufactured by disclosed method according to an embodiment of the invention
The coupon weight of coupon weight and yield are than the figure of time.
Fig. 5 is for the target slice weight of the polyamide manufactured by disclosed method according to an embodiment of the invention
The standardization cutting speed of amount/valve output and the figure of AC Pressure versus times.
Fig. 6 is for the target slice weight of the polyamide manufactured by disclosed method according to an embodiment of the invention
The coupon weight of amount and yield are than the figure of time.
Fig. 7 is the target of polyamide polymer for being manufactured by disclosed method according to an embodiment of the invention
The standardization cutting speed of coupon weight/valve output and the figure of AC Pressure versus times.
Fig. 8 is for the particle weight of the polyamide polymer manufactured by control methods according to an embodiment of the invention
Amount and yield are than the figure of time.
It should be noted that above-mentioned figure is only the illustrative expression of embodiments of the present invention, pass through the figure pair
The scope of the present invention does not form any restriction.
Specific embodiment
Although detailed description below contains many details for the purpose of illustrating the invention, the skill of this field
Art personnel can understand many change and modification of hereafter details in the range of embodiment disclosed in this invention.
Therefore, embodiment hereafter illustrates the present invention without loss of generality, and limitation is not brought to the present invention.
It is more fully described before the present invention, it should be understood that the present invention is not limited to described specific embodiment, this is because should
Embodiment can change.It is also understood that term used herein above is only the purpose for description particular implementation, and
It is not intended to be limiting, this is because the scope of the present invention is only limited to the appended claims.Unless otherwise prescribed, made here
There are all technical terms and scientific terms those of ordinary skill in the art with field of the present invention to be generally understood
The identical meaning of meaning.
If "one" and " this " of the singulative used in this specification and the appended claims are including multiple
Object is counted, unless the context otherwise specific miscellaneous stipulations.Thus, for example " polyamide " includes a variety of polyamide.
In the disclosure, "comprising", " containing " and " with " etc. can be with assigning their meaning according to United States patent law
And it may imply that " comprising " etc., and be generally interpreted as open term.Term " Consists of " is enclosed art
Language, and device, method, component, component, structure, step for being expressly set out etc. are only included according to the meaning of United States patent law.When
Device that " substantially by ... form " or " constituting substantially " etc. is included for the present invention, method, component, component, structure, step
Whens rapid etc., it is related to the element similar with disclosure herein, but it may include additional building stone, constituent component, method
Step etc..But with corresponding device disclosed herein, compound, method etc. in comparison, these additional device, sides
Method, component, component, structure, step etc. will not substantially influence the foundation characteristic of device, compound, method etc. and novelty spy
Sign.In more details, when " substantially by ... form " or " constituting substantially " etc. is included for the present invention device, method,
Whens component, component, structure, step etc., it is open to have the meaning assigned according to United States patent law and these terms
, as long as the basic or novel features recorded allow to be more than recorded content not by more than recorded content changing
In the presence of, but except removing the embodiment of the prior art..When using open-ended term, during such as "comprising" or " comprising ", it should be understood that
, as clearly stated, also direct support term " substantially by ... form " and term " Consists of ".
Term " polymerisable compound " or " polymerizable solution " are referred in stirring high pressure according to an embodiment of the invention
The component added in kettle, when being handled in autoclave under specific temperature and pressure curve, formation can be extruded or be received
It cuts and is used for the polyamide polymer further used.
Term " polyamide salt " refers to be included in polymerisable compound（Together with other additives）In salt, it is described to gather
Polymeric composition provides the basic polymerizable material for being used to form polyamide polymer.If such as polyamide polymer is nylon
6,6, then salt can be prepared by adipic acid and hexamethylene diamine.Other additives also are present in polyamide solution or anti-
It answers and introduces or be introduced into reaction vessel before container.For example, usually titanium dioxide is introduced directly into container, however
Before polymerisable compound is introduced into container, other additives, such as catalyst, fluorescent whitening agent, antifoaming agent etc. are introduced, to the greatest extent
Pipe does not require this sequence or the even presence of these additives.
Term " period " is related to the stage mainly handled by the batch polymerization that the pressure curve in container limits.Period 1
（Period 1）The beginning of batch processed is happened at, at this moment pressure is just raised to relatively high pressure from relatively low pressure.Second round（Period 2）
It is happened at and relatively high pressure is kept into for a period of time.Period 3（Period 3）Occur when being reduced to relatively low pressure with relatively high pressure.
Period 4（Period 4）Occur with relatively low pressure is kept for a period of time.Period 5（Cycle 5）With what will be prepared
Polymer is squeezed out out of container and is occurred.Terminology used in the present invention " period 4 ", " period 4 " and " period before casting " can phases
Mutually replace.
Phrase, such as " being suitable for providing ", " being enough to cause " or " being enough to generate " etc. relate in the context of synthetic method
And with the relevant reaction condition such as time, temperature, solvent, reactant density, changeable reaction condition is to provide reaction product
Useful quantity or the yield of reaction product, this is in the range of the common skill of the experimenter of this field.Must not
Strategic point is that for required reaction product to be only that reaction product or starting material are totally consumed, what is provided is required
Reaction product can be detached or otherwise be further used.
It should be understood that ratio, concentration, amount or other data can be stated in the form of a range here.It should
Understand, the use of this range format is for convenience and simplicity.And it therefore, should explain in a flexible way with not
But the data parameters that the endpoint including such as range clearly states, and if each numerical value and subrange include, " about ' X ' is to big
About ' Y ' " then also includes all individual data parameter or the subrange in the range.In order to illustrate " about 0.1%
Concentration range to about 5% " should be interpreted, not only include the concentration of about 0.1 weight % to about 5 weight % clearly demonstrated,
The single concentration being included in illustrated range（Such as 1%, 2%, 3% and 4%）And subrange（Such as 0.5%, 1.1%,
2.2%th, 3.3% and 4.4%）.In one embodiment, term " about " may include the tradition of the effective digital according to data parameters
Rounding-off.In addition, phrase " about ' X ' to ' Y ' " includes " about ' X ' to about ' Y ' ".
Term " about " used herein above when being related to data parameters or range, allows in certain numerical value or range
A degree of variation, such as within the 10% of the numerical value stated or the endpoint for the range stated or on the other hand
Change within 5%.
In addition, by enumerate or Markush group in a manner of describe the present invention features or aspect place, this field
Technical staff will be appreciated that, thus also according to Markush group element any single element or subbase group and describe this
Invention.For example, if X is described as, selected from the group being made of bromine, chlorine and iodine, as individually enumerating, X being fully described
Claim and X for bromine are the claim of bromine and chlorine.For example, the features or aspect in the present invention are retouched according to this enumerate
The place stated, those skilled in the art will be appreciated that, therefore any single element of the element also according to Markush group
Or subbase group any combination and describe the disclosure.Therefore, if X is described as selected from the group being made of bromine, chlorine and iodine, and
Y is described as selecting the group of free methyl, ethyl and propyl composition, then is fully described and supports the power that X is bromine and Y is methyl
Profit requirement.
As used herein, all constituent contents are provided in the form of weight percent, unless otherwise stated.When being related to
During component solution, percentage refers to including solvent（Such as water）Component weight percent, unless otherwise indicated.
As used herein, the molecular weight of all polymer（Mw）It is weight average molecular weight, unless otherwise indicated.
When reading the disclosure, it is it is obvious to those skilled in the art that described and illustrated herein
Each individual embodiment have independent component and feature, these independent components and feature are easy to several with other
Any character separation of embodiment is combined without departing from the scope or spirit of the invention.Any described method can institute
The sequence of the situation of description is implemented or is implemented with feasible in logic any other sequence.
In general, the method for the uniform particle of production polyamide polymer may include following steps：With substantial and polyamide
The yield of polymer proportional cutting speed cuts the bar of the polyamide polymer of extrusion, to realize polymer beads
Homogeneity；And one or more technological parameters are adjusted to keep the homogeneity of polyamide granules.Specifically, the method can
The first technological parameter is adjusted to keep homogeneity including the change in response to the second alternative technological parameter, described first
Technological parameter is selected from the group being made of cutting speed, extrusion valve opening and container pressure, the second technological parameter choosing
The group being freely made of cutting speed, extrusion valve opening and container pressure.Homogeneity is to measure being averaged for a collection of particle
Quality, the difference of Individual Quality and the average quality of a batch particle at least 95% individual particles for 10% with
It is interior.In another embodiment, homogeneity is to measure the average quality of a collection of particle, and a batch particle is at least 99%
The difference of the Individual Quality of individual particles and the average quality is within 5%.
Similarly, it is a kind of to may include high pressure processing vessels, cutter and mistake for manufacturing the device of uniform polyamide granules
Range controller.The high pressure processing vessels may include pressure controller and squeeze out valve.The cutter can be configured to cutting from
The polyamide polymer that high pressure processing vessels squeeze out is to form polyamide granules.The process controller may include controlling pressure
The pressure control module of force controller, the cutting speed module for controlling cutting speed and the extrusion for control extrusion valve
Valve module.Described device may be configured to by with certain yield by squeezing out the strip of the polyamide extruded polymer of valve
Object, and the bar is cut to manufacture the uniform polyamide granules of a batch with certain cutting speed.Again, homogeneity is to survey
The average quality of a collection of particle of amount, the Individual Quality of a batch particle at least 95% individual particles are the average matter
Within the 10% of amount.In another embodiment, homogeneity is to measure the average quality of a collection of particle, and a batch particle has
Within the difference 5% of the Individual Quality of at least 99% individual particles and the average quality.It should be noted that when discussing this hair
During bright device and method, these discuss each can be considered to be applied in each embodiment, no matter whether it at this
It is clearly discussed in the context of embodiment.Thus, for example, when discussing the polyamide polymer about described device,
These discussion can also be used in method, and vice versa.
Referring back to apparatus and method of the present invention, under normal circumstances, can make in the paradigmatic system comprising polyamide
With manufacturing method of the present invention, casting method, device etc..In one embodiment, polyamide polymer may include, substantially by Buddhist nun
Dragon 6,6 forms or is made of nylon 6,6.Nylon 6,6 can be straight polymer or also can be by any number of additive
And be modified, the additive includes fluorescent whitening agent, dyestuff etc..Usually, the manufacturing method being related in the present invention can wrap
The method for including continuous method and batch, unless otherwise indicated.These methods carry out usually in reaction vessel, such as high pressure
Kettle.In one embodiment, manufacturing method can be batch method.There is no particular limitation, and as described herein, which leads to
It is often 5 periodic methods.
Referring particularly to nylon 6,6, typical batch production scale according to an embodiment of the invention can be about 1000Kg
To about 3000Kg, and can be recycled in autoclave about 100 to 120 minutes during batch produces.It can be used on above range
Batch production scale and time in addition, this depends on the selection of equipment and polymer or in those skilled in the technology concerned
Knowledge in other Considerations.Under normal circumstances, the nylon of polyamide as salt add in.In an embodiment party
In formula, nylon can be 6,6 salt of nylon, and amount that can be in the range of about 50 weight % to 95 weight % is present in polyamide.
Kinds of processes parameter can be used in the polymerization of the polyamide of the present invention, including temperature and pressure.In an implementation
In mode, temperature can be in the range of about 190 DEG C to about 290 DEG C, and spontaneous pressure during certain periods or other pressure can
In about 250 pound per square inch absolute values（psia）To about 300 pound per square inch absolute values（psia）In the range of.In addition,
In another embodiment, it during certain periods, can be heated under the vacuum condition of the pressure less than 10torrg.
In some embodiments, when in vacuum cycle, not heating polymer further.In general, as those skilled in the art is examining
It can understand after considering the present invention, when polymer temperature is enough, vacuum process can be started.In some embodiments, it is workable
Minimum pressure can be down to about 150torra, for example, about 200mbara.
It under normal circumstances, can be by autoclave and squeezing out/cutting through for producing the method for the present invention of polyamide granules
Journey is realized.In one embodiment, the polyamides that the method can be by concentrating slurry or from high pressure processing vessels be provided to
Amine salt（Such as nylon 6,6 salt）Aqueous solution start come the polyamide solution prepared.Optionally, the slurry can be diluted and passed through
Evaporation step becomes more to concentrate.It in one embodiment, can be according to method known in the art, from monomer hexamethylene diamine
Slurry is prepared with the aqueous solution of adipic acid.In another particular embodiment of the invention, when 6,6 monomer solution of nylon is in oneself
During the form of amide aqueous solution, the slurry contains a small amount of 6 monomer of nylon.In one embodiment, high pressure processing vessels
About 230 DEG C then can be heated to（Or other function temperature）So that internal spontaneous pressure rises.Optionally by delustering agent, two
Titanium oxide（TiO2）Inject autoclave and as in the monomer mixture of water-borne dispersions.
Polyamide solution or thickened slurry mixture then can be heated to about 245 DEG C in autoclave（Or other certain work(
It can temperature）.When in the temperature, the pressure of autoclave can be reduced to atmospheric pressure, and by a known way using vacuum come into
One step reduces pressure, to form daiamid composition.It is kept at the temperature and/or pressure containing described in daiamid composition
Autoclave about 30 minutes.Such as the then step, polyamide polymer composition is further heated to about 285 in autoclave
DEG C, and drying nitrogen is introduced into high pressure processing vessels, and by introduce the absolute pressure of drying nitrogen to about 4 to about 5bar come
Pressurize the autoclave.
Catalyst can also be used to prepare in polyamide polymer of the present invention.In one embodiment, polyamide
In 10ppm may be present（Weight）To 1000ppm（Weight）In the range of amount catalyst.On the other hand, catalyst can be with 10ppm
（Weight）To 100ppm（Weight）In the range of amount exist.Do not limit, catalyst may include phosphoric acid, phosphorous acid, hypophosphoric acid,
Arylphosphonic acid, arylphosphinic acid, these compounds salt and its mixture.In one embodiment, catalyst is time phosphorus
Sour sodium, manganese hypophosphite, phenylphosphonous acid sodium, phosphenylic acid sodium, phenylphosphonous acid potassium, phosphenylic acid potassium, diphenyl phosphorous acid oneself
Diamine salts, tolyl potassium phosphite or its mixture.On the one hand, catalyst can be sodium hypophosphite.
Polyamide disclosed according to the embodiment of the present invention and polyamide group can be improved by adding fluorescent whitening agent
Close the appearance whiteness of object.These polyamide can show permanent whiteness and improve, and can be kept by the operation of such as thermal finalization
The whiteness is improved.In one embodiment, the fluorescence of the amount in the range of 0.01 weight % to 1 weight % may be present in polyamide
Brightening agent.On the one hand, fluorescent whitening agent can be titanium dioxide.
In addition, antioxidative stabilizer, antibacterial additives etc. can be used to prepare these polyamide polymers.In addition, it can make
Polyamide polymer is prepared with antigassing additive.In one embodiment, 1ppm may be present in polyamide（Weight）Extremely
500ppm（Weight）In the range of amount antigassing additive.
Polyamide polymer disclosed according to the embodiment of the present invention is born acid dyeable, but also can by
The dye of positive ion is copolymerized in polymer to be modified these polymer or copolymer, and converts it into basic dyeing form.These
It is modified that composition is caused especially to receive the dyeing with basic dye.
Turning now to Figure 1A and 1B, which show the cross-sectional views of two illustrative agitated autoclaves.These figures
It is not necessarily drawn to scale, and without each and all details usually existing in display agitated autoclave, but selects selection
Property show and schematically shown with the present invention especially relevant feature.Therefore, in the present embodiment, in respective figure,
Agitated autoclave 10 may include high pressure processing vessels 20 and blender or spiral 22.Although showing blender and spiral,
It is not necessary.The container include chamber wall 24, it typically is electroplating container wall, and set the chamber wall and/or its
His structure is to support the heating component 26a and 26b of one or more types.In the present embodiment, 26a shows that external jacket adds
Hot component, 26b show internal heating component.It should be noted that the heating component in Figure 1A is placed in relatively close blender
Place, this is than more typical；And the heating component in Figure 1B is placed in closer at chamber wall, this for non-stirred type autoclave more
It is typical.But as described, the position of heating element, which can lead to those skilled in the art, is considering that the present invention was determining later.Another
In a embodiment, heating element all may be present two positions, i.e., close to chamber wall and close to blender.
External jacket heating component 26a can be used for the temperature of the polymerizable components or polymer contained in increase container, and
Internal heating component 26b is used especially for the inner surface that polymer is prevented to become attached to chamber wall and/or blender.Such as Figure 1A
It is shown, in addition to showing internal heating component, also there is a pair of of update stick（refresherbars）, with central stirrer or
Spiral 22 is worked together with more novel polymer.Blender work works as stirring so that polymer to be moved up along the central part
During the polymer of fusing, using the pair of update stick by updating the polymer of fusing from sidewall surfaces removing polymer.
This set can be in improvement system heat transfer, and the height being vortexed as caused by blender can be reduced.
It should be noted that although schematically showing internal heating component 26b on sectional view, it is understood that
It is the inside heating component that any shape or structure can be used.It is also to be noted that the heating component can be constructed or set
Into any fluid of the prior art can be carried（Including gas and/or liquid）, for providing heat for autoclave.It also shows
Imported valve 28 and autoclave ventilation hole 30, and the imported valve 28 and autoclave ventilation hole 30 can be used as pressure controller
To be used together or be used alone（Together with heating component 26a and 26b, also controllable pressing pressure）.Do not show pressue device or
Pressure source, it will be appreciated that the pressue device or pressure source may be present when wanting impressed pressure.Alternatively, as this field
It is intelligible, pressure can be increased by adding heat, and reduce pressure by emptying.Further, high pressure processing vessels
Bottom be valve openings 32.This figure does not show extrusion valve, but this be the polymer prepared in autoclave be extruded with
In the position being processed further.It is also to be noted that it is as will be understood by the skilled person in the art, no matter these imports, valve
The position of description and the display of door, ventilation hole etc. compared with shown, can use these or other ports differently,
For any purpose of user design.
It should be noted that provide this is formed in autoclave illustrative high pressure processing vessels of polyamide polymer with
The purpose of being given for example only property of method, as any number of other technical process, autoclave and additive next life can be used
Produce polyamide polymer.No matter how polymer is prepared in autoclave, this point in the method being generally described is
The main object of the present invention casts the polymer from aggregation container.
As described herein, the present invention provides by cutting the polyamide polymer squeezed out and adjusting kinds of processes parameter
To form the device and method of the uniform particle of polyamide polymer.Especially, method of the invention allows in response to above-mentioned
The change of another technological parameter adjusts the first technological parameter, and first technological parameter includes cutting speed, squeezes out
Valve opening and container pressure.In addition, on the one hand, may be in response to third technological parameter to adjust two technological parameters.At one
In embodiment, although any technological parameter or two technological parameters, the technological parameter being conditioned, which is adjusted, can be or can
To include container pressure.On the other hand, the technological parameter being conditioned can be or can include squeezing out valve opening.The opposing party
Face, the technological parameter being conditioned can be or can include cutting speed.
Turning now to Fig. 2, the device for manufacturing uniform polyamide granules may include container 20, such as be similar to Figure 1A and/
Or the autoclave shown in Figure 1B, the container 20 include pressure controller（It can be inlet line/valve 28, discharge pipe/
The form of valve 30 and/or heating component 26）.It, can be with it should be noted that although showing the heating component of external jacket
It replaces with or increases internal heating component.It also shows to squeeze polymer by what Die and mould plate or other extrusion structures squeezed out
Go out valve 34.Described device may also include cutter 36, and the cutter is configured to the polyamide for being suitble to cutting uniform
The cutting speed of grain.For example, the cutter can be revolution cutter, it is configured to when the polymer being extruded passes through it
It cuts very fast.Described device may also include process controller 60, may include pressure control module 70, cutting speed module
80 and squeeze out valve module 90.Described device may also include plate 38, slurry collects equipment 40, slurry pipeline 42 and drier/rotation
Turn device 44.
In the further description about the process controller 60 of described device, multiple module 70,80,90 can be used
To automatically carry out the general utility functions of automation equipment or processing step.For example, can by pressure control unit 70 come control into
Mouth valve 28, autoclave ventilation opening 30 and heating component 26, to allow the adjusting of pressure.It can be controlled by cutting speed module 80
Cutter 36 processed.By squeezing out valve module 90 valve 34 can be squeezed out to control.Other modules that may be present（It does not show）, including
But it is not limited to blender module, drier module, heating component module etc..The module is simultaneously operable, come uniform to cause
The modes of polyamide granules automated system is provided.
Fig. 3 elaborates the figure for illustrating embodiment, in embodiment, these modules work at the same time realize it is according to the present invention
The remarkable homogeneity of embodiment.Specifically, Fig. 3 illustrates the casting of the technological parameter of device according to the embodiment of the present invention
Make figure.Specifically, this figure provides during casting as the autoclave by single batch casting methods of the function of time
Pressure, the yield of polyamide polymer from autoclave, the extrusion valve figure of linearisation and cutting speed.As shown in the figure, it adjusts
Kinds of processes parameter is saved to provide substantially invariable yield under high cutting speed, and thus provide and keep particle homogeneity
The automated method of high throughput rate is also kept simultaneously.
It is also noted that changing rate of cutting, and rate of cutting is substantially proportional to yield in the chart of Fig. 3, that is, work as
Yield rises or falls（As shown in the chart）, cutting speed equally respectively raising and lowering.Since term " substantially " is related to
Yield and cutting speed is proportional or opposite matching, may be defined as any matching degree, under the matching degree, uniform a batch
It is the 10% of the average quality that the average quality of grain, which is a collection of Individual Quality of the particle at least 95% individual particles,
Within.By matching relative movement of the cutting speed to yield substantially, homogeneity can be kept.As a result, pressure controller and extrusion
The use of valve maintains yield in rational range, for realizing effective cut section.For example, passing through suitable pressure
In the efficient system of the high yield provided with linear valve aperture, can cutting speed be subjected to opposite match with yield.
It should be noted that when yield rises, cutting speed also rises.
Back to Fig. 2, as described herein, the pressure of container 20 can be spontaneous or can come from external pressure source
Generation.In addition, heat, pressure source can be used（It does not show）And/or ventilation hole 30 adjusts pressure.Squeeze out 34 general control of valve
Aperture, polyamide polymer are extruded from the opening.In some respects, the line that valve opening is referred to alternatively as squeezing out valve is squeezed out
Property aperture." linear " used herein refers to being equivalent to the opening of the valve（Open region）It is squeezed out than passing through opening
The mathematic(al) manipulation of the percentage of material.For example, 50% " linear " aperture is referred to from 100%（100% refers to opening completely
Maximum capacity during valve）Total amount in from opening squeeze out 50% material, even if valve opening（Open region）May not be
Total obtain aperture 50%.It should be noted that when valve does not set and opened close to 100%, exist much more poly-
The control of the yield of amide polymer.When valve proximity 70% or 80% aperture, the control of yield is significantly reduced.It for example, will
The aperture of valve, which changes from 40% to 50% pair of yield, has relatively significant effect, and valve is reached 90% pair of yield tool from 80%
There is the effect of very little.Therefore, it is desirable that valve is kept as far as possible in the range of about 30% to 70% aperture, and more typically
In the range of 35% to 60% being maintained at during polymer casting process.In order to complete this target, pressure can be changed and/or cut
Speed is cut to keep valve opening in the preferred range.Notwithstanding these, but these are not strictly required.This
There is provided a kind of mechanism, to keep the maximum flexibility of the aperture about squeezing valve.
A variety of adjustings of technological parameter are back to, the variation that may be in response to other technological parameters carries out the kinds of processes ginseng
Several adjusting, it should be noted that the adjusting of technological parameter can be carried out sequentially or simultaneously（Or it is carried out successively within the time of overlapping）.
In one embodiment, the variation of third technological parameter is may be in response to adjust more than one technological parameter.In order to provide reality
Example is applied to illustrate why these technological parameters can benefit from change, it should be noted that once since high pressure processing vessels squeeze
Go out process, the polyamide polymer usually wherein contained is fully completed its polymerization process not yet.Therefore, polyamide polymer exists
It will continue to further be thickened during extrusion.It it has been found that under these conditions cannot be by individually increasing pressure come simple
Ground keeps yield and prior particle homogeneity.Similarly, only further opening extrusion valve 34 will not always fill
Make up the polymer of thickening with dividing.In addition, even if by controlling two in these parameters together, if not based on yield
Change to adjust cutting speed, the homogeneity of polyamide granules can also be damaged.
About the adjusting, method of the invention allows the more effective adjusting to yield, and combine cutting speed with
The matching of yield provides the homogeneity that was not carried out in the past.Specifically, there are the variables of two influence actual productions：i）It squeezes
Go out valve opening, the raising of aperture leads to raising and the ii of yield）Autoclave pressure, the raising of autoclave pressure also cause
The raising of yield.It squeezes out valve opening and is suitable for the measured yield of quick correction.But it is protected using the aperture of four corner
It is typically what is be very limited to hold constant yield.In addition, when reducing autoclave pressure during casting, it may hair in autoclave
The significant bubble of raw polymer.This causes autoclave pressure to be not suitable as the main means of control yield.In order to overcome this
The limitation of two variables controls yield using valve output.Then, each valve opening is more than the target output of restriction
When, just further increase the pressure of autoclave.Using multiple variables come control yield when the traditional technology much more efficiently.Into
One step, embodiments of the present invention allow cutting speed to match to provide the particle homogeneity being not carried out before with yield.
Therefore, apparatus and method of the present invention includes the use of the pressure, the valve opening of variation and cutting for variation of variation
It speed is cut to control yield, and therefore controls particle homogeneity, uniform particle is realized with effective means.Therefore, one
In a specific embodiment, illustrative yield can in the range of 2 to 10 tphs or 5 to 9 tphs or particularly
Ground, 6 to 8 tphs.Illustrative pressure during extrusion can be in 0 to 12 bar, 1 to 10 bar or 5 to 10 bars of range
It is interior.Illustrative valve opening level can be in the range of 30% to 70% or in the range of 45% to 65%.Use helical cutters
Or the illustrative cutting speed of other similar rotary cutters is in the range of 100 to 2000RPM, 400 to 1800RPM,
Or in the range of 600 to 1500RPM.In general, during casting, these technological parameters are maintained in the range of these, and is led to
It crosses in the range of these and adjusts the parameter, it can be achieved that the homogeneity of polyamide granules.Although set forth it is above-mentioned these, can also make
Technological parameter other than these ranges, as long as particle homogeneity as described in the present invention can be kept.
Yield can be controlled at least partially through 34 aperture of valve is squeezed out, can cutting speed be controlled by cutter 36, and
And yield can be controlled come control pressure by one or more pressure controllers 26,28,30.Although more than one technique is adjusted
Parameter maintains the homogeneity of polyamide granules, and in a specific embodiment, pressure and/or cutting speed allow
Operation squeezes out valve in the range of linear aperture is 30% to 70%, 35 to 65% or 40% to 60%.It is in addition, ideal in order to provide
Efficiency, in one embodiment, in big system, yield can be at least 5 ton hours or at least 7 ton hours, and adjust work
Skill parameter changes in the range of can maintaining target output within the 10 mass %.
Process controller 60 generally by computer, other computing devices or other network equipments come with cutter 36 and hold
Device network connection.The device of the invention can be the automatic device using multiple module.In one embodiment, in response to cutting
It cuts speed or squeezes out the change of the aperture of valve 34, pressure control module 70 can adjust pressure controller 26,28,30.On the one hand,
In response to the change of cutting speed and the aperture for squeezing out valve, pressure control module can adjust pressure controller.In another reality
It applies in mode, in response to the change of pressure or the aperture for squeezing out valve, cutting speed module 80 can adjust the cutting of cutter 36
Speed.On the one hand, in response to the change of pressure and the aperture for squeezing out valve, cutting speed module can adjust cutting speed.Another
In one embodiment, in response to the change of cutting speed or pressure, squeeze out valve module and can adjust extrusion valve.On the one hand,
In response to the change of cutting speed and pressure, squeeze out valve module and can adjust extrusion valve.Similarly, module of the invention can be through
Process controller works at the same time, and during casting, work is adjusted in a manner of being enough to provide consistent and uniform polyamide granules
Skill parameter.
As further instruction, in order to aid in determining whether for technological parameter（Such as pressure, valve opening and cutting
Speed）A suitable level of activity, can be based on any amount of technology come forecast production, the technology includes the use of optics and comments
Estimate, assessed using weight and/or volume（In a reservoir and/or after extrusion）, based on the polymer in relation to being extruded around
Cast the assessments such as the assessment of energy transmission of water.With specific reference to energy transmission technology, this casting method may include using casting
Production forecast or the dynamic Distribution value for adjusting technological parameter in the production of polyamide granules.For example, assessment casting yield
It may include measuring the temperature and flow velocity of casting water, so calculate Heat transmission and be then associated with casting yield.
Some as further instruction, in order to more specifically emphasize its independence implemented, described in this specification
Functional unit is referred to as " module ".Such as " module " can be implemented as hardware circuit, the hardware circuit includes customization
Super large-scale integration（Very Large Scale Integration, VLSI）Circuit or grid array, such as logic
The semiconductor that can be purchased off the shelf, transistor or other discrete elements of chip.Module can also be on programmable hardware device
Implement, the programmable hardware device such as field programmable gate array, programmable logic array, programmable logic device
Part etc..Module can also be implemented being performed in software for passing through a plurality of types of processors.The identification of executable code
Module for example may include one or more blocks of computer instructions, can be carried out tissue as object, program or function.However, know
The executable code of other module does not need to be physically located together, but may include being stored in the different instruction of different location, described
Different location includes module, and when being joined logically together, and realizes the above-mentioned purpose for module.
In fact, the module of executable code can be single instruction or many instructions, and can even be distributed across several
In different code segment, between distinct program and cross over several memory devices.Similarly, it can identify and illustrate herein in the module
The operation data, and can embody in any suitable form operation data and with the data structure of suitable type come
Organize the operation data.Can operation data be collected or can be in different position distribution operands with individual data set
According to the different position includes different storage device.The module can be passive or positive, including operable to hold
The medium of row required function.
Embodiment
Embodiment 1- polyamide granules #1
The water of adipic acid and hexamethylene diamine is filled in the commercially available autoclave for the nylon 6,6 each cycle that production capacity is 1200kg
Solution.Temperature is risen to 280 DEG C from 150 DEG C, and implement to polymerize according to circular treatment.As shown in figure 4, control yield and cutting
Speed provides uniform chipping qualities.Target slice quality is 23mgr/ particles.Significantly, the figure of Fig. 4 shows slice weight
The maximum deviation of amount is to be less than about 0.5mgr relative to target slice weight, has obtained about 97.8% during whole service process
Homogeneity.As shown in figure 5, by controlling cutting speed, valve output and autoclave（Autoclave, AC）Pressure is realized
The homogeneity.
Embodiment 2- polyamide granules #2
The water of adipic acid and hexamethylene diamine is filled in the commercially available autoclave for the nylon 6,6 each cycle that production capacity is 1200kg
Solution.Temperature is risen to 280 DEG C from 150 DEG C, and implement to polymerize according to circular treatment.As shown in figure 5, control yield and cutting
Speed provides uniform chipping qualities.Target slice quality is 28mgr/ particles.Significantly, the figure of Fig. 6 shows slice weight
The maximum deviation of amount is to be less than about 0.75mgr relative to target slice weight, has obtained about 97.3% during whole service process
Homogeneity.As shown in figure 5, by controlling cutting speed, valve output and autoclave（Autoclave, AC）Pressure is realized
The homogeneity.
The non-uniform polyamide granules of embodiment 3-
Prepare autoclave by being filled with the aqueous solution of adipic acid and hexamethylene diamine.Temperature is risen to 280 DEG C from 150 DEG C, and
Implement to polymerize according to circular treatment.As shown in figure 8, with the present invention on the contrary, being exported using static cutting speed, pressure and valve
Particle is handled, has obtained sinusoidal curve of the chipping qualities as the function of casting time.Significantly, when target slice quality is
During 23mgr/ particles, maximum deviation is more than 5mg, leads to the homogeneity less than 78%.
Although for structure feature and/or operation specific language description subject of the present invention, should to manage
Solution, the theme being limited by the accompanying claims are not necessarily limited to specific feature as described above and operation.And
It is the exemplary form that above-described specific feature and action are disclosed as implementing claim.Can carry out it is multiple improvement and
Alternative setting is without departing from the spirit and scope of described technology.
Claims (34)
1. a kind of method for the uniform particle for producing polyamide polymer, including：
The polyamide polymer bar of extrusion is cut with the essence cutting speed proportional to the yield of polyamide polymer,
To realize the homogeneity of polymer beads；And
The first technological parameter is adjusted to keep the uniform of polyamide granules in response to the change of alternative second technological parameter
Property, first technological parameter is selected from by cutting speed, squeezes out the group that valve opening and container pressure form, and described second
Technological parameter is selected from the group being made of cutting speed, extrusion valve opening and container pressure；
Wherein, homogeneity is to measure the average quality of a collection of particle, of a batch particle at least 95% individual particles
Weight is within the 10% of the average quality.
2. it according to the method described in claim 1, it is characterized in that, is controlled at least partially through valve opening is squeezed out described
Yield.
3. according to the method described in claim 1, it is characterized in that, described be adjusted in response to third technological parameter, described
Three technological parameters are selected from the group being made of cutting speed, extrusion valve opening and container pressure.
4. according to the method described in claim 1, it is characterized in that, the method further includes in response to joining with the second technique
Several changes adjusts third technological parameter, and the third technological parameter is selected from by cutting speed, squeezes out valve opening and appearance
The group of device stress structure.
5. according to the method described in claim 4, it is characterized in that, the first technique ginseng is carried out in the time range of overlapping
The adjustment of number and the third technological parameter.
6. according to the method described in claim 1, it is characterized in that, the container that pressurizes is so that squeeze out valve with 30% to 70%
Linear aperture operate.
7. according to the method described in claim 6, it is characterized in that, the linear aperture is 45% to 65%.
8. according to the method described in claim 1, it is characterized in that, the yield is the rate of at least 5 ton hours, and squeezes
The adjustment for going out valve opening or container pressure is maintained the yield and is changed by terms of average weight no more than 10%.
9. according to the method described in claim 1, it is characterized in that, the yield is the rate of 2 to 10 ton hours.
10. according to the method described in claim 1, it is characterized in that, first technological parameter is container pressure, in response to cutting
It cuts speed or squeezes out the change of one or two of valve opening to adjust the container pressure.
11. according to the method described in claim 10, it is characterized in that, the container pressure is adjusted in the range of 0 to 12 bar.
12. according to the method described in claim 10, it is characterized in that, the container pressure is adjusted in the range of 5 to 10 bars.
13. according to the method described in claim 1, it is characterized in that, first technological parameter is squeezes out valve opening, response
The extrusion valve opening is adjusted in the change of one or two of container pressure or cutting speed.
14. according to the method described in claim 1, it is characterized in that, first technological parameter is cutting speed, in response to holding
Device pressure squeezes out the change of one or two of valve opening to adjust the cutting speed.
15. according to the method for claim 14, which is characterized in that use range of the rotary cutter 100 to 2000RPM
It is interior to adjust the cutting speed.
16. according to the method described in claim 1, it is characterized in that, calculate heat conduction model and then with cast yield be associated with,
And the cutting speed follows the yield calculated using the heat conduction model.
17. according to the method described in claim 1, it is characterized in that, during batch extrusion, with polyamide polymer
Relative viscosity increase at any time, keep the homogeneity.
18. according to the method described in claim 1, it is characterized in that, the polyamide polymer is nylon 6,6.
It is 19. described according to the method described in claim 1, it is characterized in that, homogeneity is to measure the average quality of a collection of particle
Individual Quality of a collection of particle at least 99% individual particles is within the 5% of the average quality.
20. it is a kind of for manufacturing the device of uniform polyamide granules, including：
High pressure processing vessels, including：
Pressure controller and
Squeeze out valve；
Cutter, suitable for cutting the polyamide polymer squeezed out from high pressure processing vessels to form polyamide granules；And
Process controller, including：
Pressure control module, for control pressure controller,
Cutting speed module, for controlling cutting speed；And
Valve module is squeezed out, valve is squeezed out for controlling,
Wherein, configuration described device is come by with the bar of the polyamide extruded polymer of the extruded valve of certain yield, and will
The bar is cut and is manufactured the uniform polyamide granules of batch with certain cutting speed, wherein, homogeneity is to survey
The average quality of a collection of particle of amount, the Individual Quality of a batch particle at least 95% individual particles are the average matter
Within the 10% of amount；
It calculates heat conduction model and is then associated with, and the cutting speed module is followed using heat conduction model meter with casting yield
The yield of calculating；
The holding of the homogeneity of polyamide granules adjusts the first work by the change in response to alternative second technological parameter
Skill parameter, first technological parameter is selected from the group being made of cutting speed, extrusion valve opening and container pressure, described
Second technological parameter is selected from the group being made of cutting speed, extrusion valve opening and container pressure.
21. device according to claim 20, which is characterized in that the container is non-stirred autoclave.
22. device according to claim 20, which is characterized in that the container is agitated autoclave.
23. device according to claim 20, which is characterized in that the process controller is by computer come network connection
In the cutter and the container.
24. device according to claim 20, which is characterized in that variation in response to cutting speed squeezes out opening for valve
The variation of degree, the pressure control module modulation adjust the pressure controller.
25. device according to claim 20, which is characterized in that variation in response to cutting speed and squeeze out opening for valve
The variation of degree, the pressure control module adjust the pressure controller.
26. device according to claim 20, which is characterized in that the pressure controller includes one or more dump valves
Door, imported valve or heating component.
27. device according to claim 20, which is characterized in that first technological parameter is cutting speed, in response to
The variation of pressure or the variation of the aperture of extrusion valve, the cutting speed module adjust the cutting speed.
28. device according to claim 20, which is characterized in that first technological parameter is cutting speed, in response to
The variation of pressure and the variation of the aperture of extrusion valve, the cutting speed module adjust the cutting speed.
29. device according to claim 20, which is characterized in that first technological parameter is the aperture for squeezing out valve,
It is described to squeeze out the valve module adjustment aperture for squeezing out valve in response to the variation of cutting speed or pressure.
30. device according to claim 20, which is characterized in that first technological parameter is the aperture for squeezing out valve,
It is described to squeeze out the valve module adjustment aperture for squeezing out valve in response to the variation of cutting speed and pressure.
31. device according to claim 20, which is characterized in that the process controller keeps 30% to 70% extrusion valve
The linear aperture of door.
32. device according to claim 20, which is characterized in that the polyamide polymer is nylon 6,6.
33. device according to claim 20, which is characterized in that homogeneity is to measure the average quality of a collection of particle, institute
It is within the 5% of the average quality to state Individual Quality of a collection of particle at least 99% individual particles.
34. device according to claim 20, which is characterized in that described device is suitable for during cutting or in cutting
Before, make polyamide polymer described in water quenching using chill casting.
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|---|---|---|---|
| US201361818192P | 2013-05-01 | 2013-05-01 | |
| US61/818,192 | 2013-05-01 |
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| EP (1) | EP2992042A1 (en) |
| CN (1) | CN104129009B (en) |
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| CN104129010B (en) * | 2013-05-01 | 2018-04-17 | 英威达纺织（英国）有限公司 | The vacuum pre-cast of polyamide polymer |
| CN104877129B (en) * | 2015-06-25 | 2017-03-15 | 安庆市虹泰新材料有限责任公司 | A kind of polyamide production system |
| WO2018031564A1 (en) | 2016-08-08 | 2018-02-15 | Ticona Llc | Thermally conductive polymer composition for a heat sink |
| CN109642048A (en) | 2016-08-30 | 2019-04-16 | 陶氏环球技术有限责任公司 | Reduce the method for acrolein concentrations |
| CN108501247B (en) * | 2017-02-24 | 2022-05-10 | 上海凯赛生物技术股份有限公司 | Polyamide grain cutting method, resin preparation method and prepared resin |
| CN110705118B (en) * | 2019-10-11 | 2023-07-25 | 合肥工业大学 | Network experiment platform of industrial control system and construction method thereof |
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| WO2011019604A1 (en) * | 2009-08-10 | 2011-02-17 | Invista Technologies S.A R.L. | Improved nylon resins and process |
-
2014
- 2014-04-10 CN CN201410143762.7A patent/CN104129009B/en active Active
- 2014-04-10 TW TW103113134A patent/TW201500157A/en unknown
- 2014-04-15 WO PCT/US2014/034231 patent/WO2014179070A1/en active Application Filing
- 2014-04-15 EP EP14724608.6A patent/EP2992042A1/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10037030A1 (en) * | 2000-07-27 | 2002-02-07 | Basf Ag | Production of polyamide with a low dirt content, e.g. for production of mouldings, film or fibres, involves polymerization with a higher water vapor pressure and granulation at higher hydraulic pressure |
| JP2010000654A (en) * | 2008-06-19 | 2010-01-07 | Japan Steel Works Ltd:The | Method and equipment for manufacturing fiber-reinforced resin pellet |
| CN101691445A (en) * | 2009-03-07 | 2010-04-07 | 从化市聚赛龙工程塑料有限公司 | Alcoholysis resistant PA66 composite material used for automobiles and preparation method thereof |
| CN203973820U (en) * | 2013-05-01 | 2014-12-03 | 英威达科技公司 | Device for the manufacture of homogeneous polyamide granules |
Also Published As
| Publication number | Publication date |
|---|---|
| EP2992042A1 (en) | 2016-03-09 |
| WO2014179070A1 (en) | 2014-11-06 |
| CN104129009A (en) | 2014-11-05 |
| TW201500157A (en) | 2015-01-01 |
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