CN109762162A - Functionality polyamide and its continuous producing method - Google Patents
Functionality polyamide and its continuous producing method Download PDFInfo
- Publication number
- CN109762162A CN109762162A CN201811595090.8A CN201811595090A CN109762162A CN 109762162 A CN109762162 A CN 109762162A CN 201811595090 A CN201811595090 A CN 201811595090A CN 109762162 A CN109762162 A CN 109762162A
- Authority
- CN
- China
- Prior art keywords
- function
- melt
- reaction
- polyamide
- caprolactam
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
Disclose a kind of function polyamide and its continuous producing method.Grinding distribution is carried out this method comprises: being continuously conveyed the pre-dispersed material of function powder slurry being deployed by water, caprolactam and function powder to function powder slurry multistage grinding device；Gained function powder slurry, which is uniformly mixed after heat exchanger adjusts temperature with caprolactam melt and catalyst through dynamic mixer, enters hydrolysis reactor progress ring-opening reaction；Gained function hexanolactam oligomer melt enters prepolymerization reactor after oligomer melt dehydrator removes excess water and carries out sudden reaction；Gained function Polvamide prepolymer melt enters post-polymerization device after pre-polymer melt dehydrator sloughs residual moisture and carries out polycondensation reaction；Gained function polyamide melt successively through pelletizing, extraction and drying, obtains function polyamide slice.Function powder disperses in high uniformity in this method quantity-produced function polyamide, suitable for the production products such as high quality fiber and film.
Description
Technical field
The present invention relates to synthesis of polymer material technical fields, in particular to a kind of function polyamide and its continuously
Production method.
Background technique
Currently, the preparation method of function polyamide is mainly masterbatch method.Masterbatch method is first by function powder and vector resin
Melting mixing obtains the functional agglomerate of high function powder content, then again uniformly mixes functional agglomerate melt with polyamide melt
Function polyamide slice is obtained through extruding pelletization.During preparing function polyamide due to masterbatch method, function powder is viscous in height
Dispersion in polyamide melt mainly relies on mechanical shear stress provided by mixing apparatus, exists to be difficult to realize function powder
Height in polyamide melt is evenly dispersed, and the spinning properties and membrane performance for being sliced the function polyamide being prepared are poor.
Therefore, how continuous-stable, which prepares the function polyamide that function powder high uniformity disperses, becomes preparation high-quality functional fibre
The problem of with film urgent need to resolve.
Summary of the invention
The present invention is intended to provide a kind of function polyamide and its continuous producing method, to realize function powder high uniformity point
It is prepared by the continuous-stable of scattered function polyamide.
To achieve the goals above, according to an aspect of the invention, there is provided a kind of function polyamide continuous production side
Method, this method include the following steps:
(1) the pre-dispersed material of function powder slurry being deployed by water, caprolactam and function powder is continuously conveyed to function
Energy powdery pulp multistage grinding device carries out grinding distribution, obtains function powder slurry；
(2) function powder slurry and caprolactam melt and catalyst is prepared in step (1) to mix through dynamic mixer
It closes and uniformly enters hydrolysis reactor progress ring-opening reaction after heat exchanger adjusts temperature, it is molten to obtain function hexanolactam oligomer
Body；
(3) function hexanolactam oligomer melt is prepared in step (2) to remove excessively through oligomer melt dehydrator
Enter prepolymerization reactor after moisture and carry out sudden reaction, obtains function Polvamide prepolymer melt；
(4) function Polvamide prepolymer melt is prepared in step (3) and sloughs residual water through pre-polymer melt dehydrator
Enter post-polymerization device after point and carry out polycondensation reaction, obtains function polyamide melt；
(5) function polyamide melt is prepared successively through pelletizing, extraction and drying in step (4), obtains function polyamides
Amine slice.
Further, in step (1), function powder slurry multistage grinding device is connected in series by 1~5 grinder.
Further, in step (2), hydrolysis reactor is the tower reactor of built-in mixed cell, material bottom in and top out
It is flowed in plug flow
Further, in step (2), catalyst is Bronsted acid.
Further, in step (1), the average grain diameter of function powder is not higher than 1 μm in function powder slurry.
Further, in step (1), water, caprolactam, function powder mass ratio be 1:0.5~1:0.06~3
Further, in step (2), the additive amount of catalyst is 30~1000ppm of caprolactam melt quality into one
Step, in step (2), the temperature of heat exchanger is 130~200 DEG C
Further, in step (2), the reaction temperature of ring-opening reaction is 200~280 DEG C, reaction pressure is 1.6~
6.2MPa, reaction time are 30~90min.
Further, in step (3), the temperature of oligomer melt dehydrator is 220~280 DEG C, and material is molten in oligomer
The residence time is 15~60min in body dehydrator, and pressure is down to 150kPa~1000kPa from 1.6~6.2MPa
Further, in step (3), the reaction temperature of sudden reaction is 220~280 DEG C, reaction pressure be 150kPa~
1000kPa, reaction time are 2~10h
Further, in step (4), the temperature of pre-polymer melt dehydrator is 230~280 DEG C, and material is molten in oligomer
The residence time is 30~90min in body dehydrator, and pressure is down to 10kPa~110kPa from 150kPa~1000kPa.
Further, in step (4), the reaction temperature of polycondensation reaction is 230~280 DEG C, reaction pressure be 10kPa~
110kPa, reaction time are 5~20h
According to a further aspect of the invention, a kind of function polyamide is provided, the function polyamide is by any of the above-described kind
Function polyamide continuous producing method is prepared.
Further, the relative viscosity of function polyamide is that 2.0~5.0, filters pressing value DF is not higher than 0.8kPa.cm2/g。
The invention has the following advantages:
The present invention is directed to the problem of existing capability method for making polyamide, and it is continuous to provide a kind of function polyamide
Production method is, it can be achieved that function powder is in the continuous production of the function polyamide of high uniformity dispersion.And this method is easy to
Industrializing implementation is, it can be achieved that function polyamide heavy industrialization continuous production, so that the production efficiency of function polyamide is substantially
It improves, production cost is greatly reduced.
The present invention is by introducing function polyamide continuous process system for function powder slurry multistage grinding device, by function
The continuous preparation section of powdery pulp is integrated into function polyamide continuous production processes process, on the one hand, the company of can further improve
The quality stability of the function polyamide of continuous production；On the other hand, the production cost of function polyamide can be further decreased.This
Outside, the present invention uses solvent of the caprolactam water solution as function powder slurry, can reduce containing for water in function powder slurry
Amount, adds the content for being introduced into water in reaction system by function powder slurry to effectively reduce, so that production run can be improved
Stability, reduce production energy consumption.
The present invention uses novel tower reactor as hydrolysis reactor, in function polyamide continuous production processes process
The middle hydrolysis process for introducing caprolactam.By adjusting the additive amount of catalyst and the reaction temperature of hydrolysis reaction
The open loop of caprolactam effectively hydrolyzing can be had strong interaction at function powder by degree, reaction pressure and reaction time
Highly polar aminocaproic acid, so that real function powder is in the hexanolactam oligomer that hydrolysis reaction generates in height
It is evenly dispersed.
The present invention also provides a kind of function polyamide, compared with the prior art in similar product have higher function
Powder dispersing uniformity.
Detailed description of the invention
By reading the following detailed description of the preferred embodiment, various other advantages and benefits are common for this field
Technical staff will become clear.The drawings are only for the purpose of illustrating a preferred embodiment, and is not considered as to the present invention
Limitation.And throughout the drawings, the same reference numbers will be used to refer to the same parts.
In the accompanying drawings:
Fig. 1 is function polyamide continuous production processes flow diagram.
Specific embodiment
The present invention in order to solve the problems existing in the prior art, provides a kind of function polyamide and its continuous producing method, with
Realize the continuous-stable preparation of the function polyamide of function powder high uniformity dispersion.
It is of the invention to reach the technical means and efficacy that predetermined goal of the invention is taken further to illustrate, below in conjunction with
Attached drawing and preferred embodiment, to function polyamide proposed according to the present invention and its continuous producing method, specific embodiment,
Structure, feature and its effect, detailed description is as follows.In the following description, different " embodiment " or " embodiment " refers to not
It must be the same embodiment.In addition, the feature, structure or feature in one or more embodiments can be combined by any suitable form.
The terms "and/or", only a kind of incidence relation for describing affiliated partner, indicates that there may be three kinds of passes
System, it is specific to understand for example, A and/or B are as follows: it can simultaneously include A and B, can be with individualism A, it can also be with individualism
B can have above-mentioned three kinds of any case.
As background technique is previously mentioned, in the prior art, there are function powders to be difficult to realize in polyamide melt
The poor technical problem of the spinning properties and membrane performance of function polyamide slice that is evenly dispersed and leading to preparation.In order to improve
The drawbacks described above of the prior art, the present invention provides a kind of function polyamide continuous producing methods, as shown in Figure 1.Of the invention
Embodiment carries out the continuous production of function polyamide according to process shown in FIG. 1: will be deployed by water, caprolactam and function powder
At the pre-dispersed material of function powder slurry be continuously conveyed to function powder slurry multistage grinding device carry out grinding distribution, obtain function
It can powdery pulp；Gained function powder slurry is uniformly mixed through dynamic mixer through heat exchanger with caprolactam melt and catalyst
Enter hydrolysis reactor progress ring-opening reaction after adjusting temperature, obtains function hexanolactam oligomer melt；Gained function is in oneself
Oligoamide melt enters prepolymerization reactor after oligomer melt dehydrator removes excess water and carries out sudden reaction, obtains
To function Polvamide prepolymer melt；Gained function Polvamide prepolymer melt sloughs residual moisture through pre-polymer melt dehydrator
Enter post-polymerization device afterwards and carry out polycondensation reaction, obtains function polyamide melt；Gained function polyamide melt is successively through cutting
Grain, extraction and drying obtain function polyamide slice.
In above-mentioned function polyamide continuous producing method of the invention, by the way that function powder slurry multistage grinding device is drawn
Enter function polyamide continuous process system, the continuous preparation section of function powder slurry is integrated into function polyamide continuous production work
In skill process, on the one hand, can further improve the quality stability of quantity-produced function polyamide；It on the other hand, can be into one
Step reduces the production cost of function polyamide.Using novel tower reactor as hydrolysis reactor, connect in function polyamide
The hydrolysis process of caprolactam is introduced in the continuous technological process of production.By the additive amount and hydrolysis that adjust catalyst
It reaction temperature, reaction pressure and the reaction time of reaction, can be strong at having with function powder by the open loop of caprolactam effectively hydrolyzing
The highly polar aminocaproic acid of interaction force, so that real function powder is low in the caprolactam that hydrolysis reaction generates
Disperse in polymers in high uniformity.It is continuously made in existing polyamide continuous production processes process by what's new powdery pulp
Standby process and hydrolysis process, it can be achieved that function polyamide high efficiency, low cost continuous production, and function produced
Function powder disperses in high uniformity in energy polyamide, suitable for the production products such as high quality fiber and film
In above-mentioned function polyamide continuous producing method of the invention, function powder slurry multistage grinding device is by 1~5
Grinder is connected in series.By in the series connection number of units and grinder of grinder in regulatory function powdery pulp multistage grinding device
The partial size of abrasive media can regulate and control the average grain diameter of function powder in the function powder slurry being continuously prepared.It is continuously conveyed
The pre-dispersed material of function powder slurry to function powder slurry multistage grinding device can through function powder slurry multistage grinding device
Continuously prepare the function powder slurry of function powder high uniformity dispersion.Function powder in the function powder slurry continuously prepared
Average grain diameter is not higher than 1 μm.The average grain diameter of function polyamide continuous polymerization function powder in function powdery pulp is controlled
Within the above range, the average grain diameter of function powder in the function polyamide of subsequent production can be effectively controlled, so that function powder
With the dispersing uniformity of height in function polyamide.
In above-mentioned function polyamide continuous producing method of the invention, realize function powder at oneself in such a way that dynamic mixes
Uniform mixing dispersion in lactams, to reach almost homogeneous physical blending.Suitable dynamic mixer include shear pump,
Planetary gear dynamic mixer, sound gear ring type dynamic mixer, ball-and-socket type dynamic mixer.
In above-mentioned function polyamide continuous producing method of the invention, hydrolysis reactor is the tower anti-of built-in mixed cell
Device is answered, material bottom in and top out is flowed in plug flow.The mixed cell internals being mounted in tower reactor can guarantee material in diameter
To be sufficiently mixed, to ensure that the homogeneity for the function hexanolactam oligomer structure being prepared.
In above-mentioned function polyamide continuous producing method of the invention, the catalyst of hydrolysis reaction is Bronsted acid, matter
The addition of son can promote the cationic open loop of caprolactam, therefore the addition of catalyst Bronsted acid, can effectively improve caprolactam
The reaction rate of hydrolysis reaction.The above-mentioned Bronsted acid as catalyst include but is not limited to phosphoric acid, pyrophosphoric acid, metaphosphoric acid,
Hypophosphorous acid, phosphorous acid, sulfuric acid, sulfurous acid, nitric acid, nitrous acid, hydrochloric acid, hypochlorous acid.The additive amount of catalyst is molten for caprolactam
30~1000ppm of weight.Within the above range by the additive amount control of catalyst, catalyst opens the hydrolysis of caprolactam
Ring reacts catalytic reaction activity with higher.
In above-mentioned function polyamide continuous producing method of the invention, using water, caprolactam and function powder as raw material into
The configuration of the pre-dispersed material of row function powder slurry.Wherein function powder have coloring, antibacterial, anti-radiation and antibacterial, conduction, it is thermally conductive,
The functions such as far infrared, fire-retardant, anion, fluorescence or magnetism, including but not limited to carbon black, Pigment white 6, pigment brown 3, pigment blue 5,
Pigment blue 15, pigment blue 15: 1, pigment blue 15: 3, pigment blue 15: 4, pigment blue 15: 6, pigment blue 16, pigment blue 28, pigment blue
29, pigment blue 60, pigment violet 19, pigment Violet 23, pigment violet 29, paratonere 101, paratonere 102, paratonere 108, paratonere
112, pigment red 122, pigment red 146, pigment red 149, paratonere 170, paratonere 171, paratonere 172, paratonere 175, face
Expect red 176, paratonere 177, paratonere 178, pigment red179, paratonere 185, paratonere 202, Pigment Red 207, paratonere
208, pigment red 21 4, paratonere 241, paratonere 242, paratonere 254, paratonere 255, paratonere 263, paratonere 264, face
Expect red 272, pigment yellow 6, pigment yellow 13, pigment Yellow 14, pigment yellow 17, pigment yellow 21, pigment yellow 37, pigment yellow 77, pigment yellow
74, pigment yellow 81, pigment yellow 97, pigment yellow 107, pigment yellow 110, pigment Yellow 12 0, pigment Yellow 12 9, pigment yellow 13 8, pigment yellow
139, pigment yellow 147, pigment Yellow 14 8, pigment yellow 150, pigment yellow 151, pigment yellow 155, pigment yellow 168, pigment yellow 17 4, face
Material Huang 180, pigment yellow 187, pigment yellow 192, pigment yellow 195, pigment yellow 196, pigment yellow 197, pigment orange 34, pigment orange 36,
Pigment orange 43, pigment orange 61, pigment orange 64, pigment orange 68, pigment orange 70, pigment orange 73, naphthol green 5, pigment Green 7, naphthol green
36, naphthol green 50, yellowish green luminescent powder (ZnS:Cu), long lad phosphor (SrMgAl4O8:Eu2+Dy3+), sky blue luminescent powder
(Sr2MgSi2O7), orange luminescent powder (Y2O2S:Eu.Mg:Ti), green-yellow light luminescent powder (SrAl2O4:Eu.Dy), blue green light night
Light powder (Sr4A14O25:Eu.Dy), orange red luminescent powder (Y2O2S:Eu.Mg:Ti), silver, germanium, silver oxide, cuprous oxide, oxidation
Zinc, aluminium oxide, titanium dioxide, silica, graphene, carbon nanotube, aluminium nitride, boron nitride, silicon carbide, graphite, bamboo charcoal, coffee
Coffee carbon, zirconium carbide, zirconium oxide, titanium carbide, hafnium carbide, tourmaline, Strange ice stone, opal, strange stone, layered double-hydroxide,
Mica, jade, magnesium hydroxide, zinc borate, ferroso-ferric oxide or tin-antiomony oxide, tin indium oxide.In a kind of preferred implementation of the present invention
Example in, stated in the pre-dispersed material of function powder slurry water, caprolactam, function powder mass ratio be 1:0.50~1:0.06~3.
Solvent using caprolactam water solution as function powder slurry can reduce the content of water in function powder slurry, with effective
Reduction the content for being introduced into water in reaction system is added by function powder slurry, thus can be improved the stability of production run,
Reduce production energy consumption.
In above-mentioned function polyamide continuous producing method of the invention, function powder slurry and caprolactam melt and catalysis
Agent is uniformly mixed through dynamic mixer enters hydrolysis reactor after heat exchanger adjusts temperature, wherein the temperature of the heat exchanger of heat exchanger
Degree is 130~200 DEG C.Into before hydrolysis reactor, function powder slurry is blended with what caprolactam melt and catalyst were formed
Object can effectively avoid the caprolactam in blend and occur to thermally decompose and influence because sharply heating after heat exchanger is preheated
The form and aspect of product.
In above-mentioned function polyamide continuous producing method of the invention, function hexanolactam oligomer melt is molten through oligomer
Body dehydrator enters prepolymerization reactor progress sudden reaction after removing excess water；Function Polvamide prepolymer melt is through pre-polymerization
Object melt dehydrator enters the progress polycondensation reaction of post-polymerization device after sloughing residual moisture.In the addition polymerization of polyamide continuous polymerization
Reaction and polycondensation reaction stage, water is more in reaction system, is more unfavorable for the further growth of strand.Therefore anti-in addition polymerization
Should and polycondensation reaction stage, regulate and control reaction system in water content, be improve and stablize molecular weight important measures.Oligomer is molten
Body dehydrator and pre-polymer melt dehydrator are flash vessel, using the principle of flash distillation by the moisture removal in melt.Oligomer
The temperature of melt dehydrator is 220~280 DEG C, and material residence time in oligomer melt dehydrator is 15~60min, pressure
150kPa~1000kPa is down to from 1.6~6.2MPa；The temperature of pre-polymer melt dehydrator is 230~280 DEG C, and material is low
The residence time is 30~90min in polymer melt dehydrator, and pressure is down to 10kPa~110kPa from 150kPa~1000kPa.
In above-mentioned function polyamide continuous producing method of the invention, the reaction temperature of ring-opening reaction is 200~280 DEG C,
Reaction pressure is 1.6~6.2MPa, and the reaction time is 30~90min.Within the above range by the control of ring-opening reaction condition, can make
The hydrolysis conversion ratio for obtaining caprolactam meets the requirement of subsequent sudden reaction.The reaction temperature of sudden reaction is 220~280
DEG C, reaction pressure is 150kPa~1000kPa, and the reaction time is 2~10h.Within the above range by the control of sudden reaction condition,
The relative viscosity that function Polvamide prepolymer is prepared may make to meet the requirement of subsequent polycondensation reaction.The reaction of polycondensation reaction
Temperature is 230~280 DEG C, and reaction pressure is 10kPa~110kPa, and the reaction time is 5~20h.Polycondensation reaction condition is controlled
Within the above range, the function polyamide that relative viscosity is 2.0~5.0 can be prepared, to meet subsequent spinning and membrane
Viscosity requirement.
In another exemplary embodiment of the invention, a kind of function polyamide is additionally provided, by any of the above-described kind of function
Energy polyamide continuous producing method is prepared.The relative viscosity of function polyamide provided by the present invention is 2.0~5.0, presses
Filter value DF is not higher than 0.8kPa.cm2/g；Filters pressing value is the validity feature for characterizing function powder degree of scatter in polymer matrix
Value.Within the above range by the filters pressing value control of function polyamide, it can make function powder in polyamide substrate in high uniformity
Dispersion, so that the function polyamide being prepared can be used conveniently to prepare the products such as high quality thin film and fiber.Filters pressing value DF
Test method: be the melt metering pump of 1.2cc, melt pressure by single screw extrusion machine that draw ratio is Φ 25mm × 25D, volume
Force snesor and screen area S are 3.8cm2Four layers of combination strainer of 60-100-1400-100-20 mesh be sequentially connected composition filters pressing
Ability meter；Filters pressing performance test process conditions: pressure set points are before melt temperature is 270 DEG C, melt metering pump pumps
6.5MPa, melt metering pump metered flow are 38g/min；500g polyamide 6 is squeezed out from filters pressing ability meter first, is recorded
Balance pressure is initial pressure Ps, then squeezes out 3000g function polyamide from filters pressing ability meter, then by 500g polyamides
Amine 6 is squeezed out from filters pressing ability meter, and record balance pressure is termination pressure PT, finally according to formula:Filters pressing value DF is calculated.
Embodiment 1
(1) will be by water, caprolactam and pigment blue 15: the 3 pre-dispersed material of function powder slurry being made into be continuously conveyed to function
Energy powdery pulp multistage grinding device carries out grinding distribution, wherein water, caprolactam and pigment blue 15: 3 mass ratio is 1:
0.8:1.8, function powder slurry multistage grinding device are connected in series by 3 grinders, obtain pigment blue 15: 3 content is
50wt%, the function powder slurry that average grain diameter is 0.28 μm；
(2) function powder slurry and caprolactam melt and catalyst is prepared in step (1) to mix through dynamic mixer
It closes and uniformly enters hydrolysis reactor progress ring-opening reaction after heat exchanger adjusts temperature, wherein catalyst is phosphoric acid, catalyst
Additive amount is the 400ppm of caprolactam melt quality, the additive amount of function powder slurry is caprolactam melt quality 5%,
The temperature of heat exchanger is 160 DEG C, and the reaction temperature of ring-opening reaction is 270 DEG C, reaction pressure 5.5MPa, reaction time are
60min obtains original liquid coloring hexanolactam oligomer；
(3) original liquid coloring hexanolactam oligomer melt is prepared in step (2) to remove through oligomer melt dehydrator
Enter prepolymerization reactor after excess water and carry out sudden reaction, wherein the temperature of oligomer melt drier is 270 DEG C, material
Residence time in oligomer melt dehydrator is that 15min, pressure from 5.5MPa are down to 300kPa, the reaction temperature of sudden reaction
Degree be 260 DEG C, reaction pressure 300kPa, reaction time 3h,
Obtain original liquid coloring Polvamide prepolymer melt；
(4) by step (3) be prepared original liquid coloring Polvamide prepolymer melt slough through pre-polymer melt dehydrator it is residual
Enter post-polymerization device after remaining moisture and carry out polycondensation reaction, wherein the temperature of pre-polymer melt drier is 260 DEG C, material exists
Residence time in oligomer melt dehydrator is that 30min, pressure from 300kPa are down to 110kPa, the reaction temperature of polycondensation reaction
For 240 DEG C, reaction pressure 110kPa, reaction time 10h,
Obtain original liquid coloring polyamide melt；
(5) original liquid coloring polyamide melt is prepared successively through pelletizing, extraction and drying in step (4), obtained opposite
The original liquid coloring blue polyamide that viscosity is 2.4 is sliced, and wherein the filters pressing value DF of original liquid coloring blue polyamide slice is
0.21kPa.cm2/g。
Embodiment 2
(1) the pre-dispersed material of function powder slurry being deployed by water, caprolactam and carbon black is continuously conveyed to function powder
Somaplasm material multistage grinding device carries out grinding distribution, and wherein the mass ratio of water, caprolactam and carbon black is 1:0.8:0.77, function
Powdery pulp multistage grinding device is connected in series by 3 grinders, and the content for obtaining carbon black is 30wt%, average grain diameter 0.11
μm function powder slurry；
(2) function powder slurry and caprolactam melt and catalyst is prepared in step (1) to mix through dynamic mixer
It closes and uniformly enters hydrolysis reactor progress ring-opening reaction after heat exchanger adjusts temperature, wherein catalyst is phosphoric acid, catalyst
Additive amount is the 400ppm of caprolactam melt quality, the additive amount of function powder slurry is caprolactam melt quality
10.7%, the temperature of heat exchanger is 130 DEG C, the reaction temperature of ring-opening reaction is 220 DEG C, reaction pressure 2.3MPa, reaction when
Between be 60min, obtain original liquid coloring hexanolactam oligomer；
(3) original liquid coloring hexanolactam oligomer melt is prepared in step (2) to remove through oligomer melt dehydrator
Enter prepolymerization reactor after excess water and carry out sudden reaction, wherein the temperature of oligomer melt drier is 280 DEG C, material
Residence time in oligomer melt dehydrator is that 30min, pressure from 2.3MPa are down to 300kPa, the reaction temperature of sudden reaction
Degree be 260 DEG C, reaction pressure 300kPa, reaction time 3h,
Obtain original liquid coloring Polvamide prepolymer melt；
(4) by step (3) be prepared original liquid coloring Polvamide prepolymer melt slough through pre-polymer melt dehydrator it is residual
Enter post-polymerization device after remaining moisture and carry out polycondensation reaction, wherein the temperature of pre-polymer melt drier is 260 DEG C, material exists
Residence time in oligomer melt dehydrator is that 30min, pressure from 300kPa are down to 110kPa, the reaction temperature of polycondensation reaction
For 240 DEG C, reaction pressure 110kPa, reaction time 10h,
Obtain original liquid coloring polyamide melt；
(5) original liquid coloring polyamide melt is prepared successively through pelletizing, extraction and drying in step (4), obtained opposite
The original liquid coloring black polyamide that viscosity is 2.4 is sliced, and wherein the filters pressing value DF of original liquid coloring black polyamide slice is
0.11kPa.cm2/g。
Embodiment 3
(1) the pre-dispersed material of function powder slurry being deployed by water, caprolactam and pigment red179 is continuously conveyed to function
Energy powdery pulp multistage grinding device carries out grinding distribution, and wherein the mass ratio of water, caprolactam and pigment red179 is 1:0.5:
0.375, function powder slurry multistage grinding device is connected in series by 2 grinders, and the content for obtaining pigment red179 is
20wt%, the function powder slurry that average grain diameter is 0.28 μm；
(2) function powder slurry and caprolactam melt and catalyst is prepared in step (1) to mix through dynamic mixer
It closes and uniformly enters hydrolysis reactor progress ring-opening reaction after heat exchanger adjusts temperature, wherein catalyst is metaphosphoric acid, catalyst
Additive amount be the 1000ppm of caprolactam melt quality, the additive amount of function powder slurry is caprolactam melt quality
9.4%, the temperature of heat exchanger is 180 DEG C, and the reaction temperature of ring-opening reaction is 250 DEG C, reaction pressure 4.0MPa, reaction time
For 30min, original liquid coloring hexanolactam oligomer is obtained；
(3) original liquid coloring hexanolactam oligomer melt is prepared in step (2) to remove through oligomer melt dehydrator
Enter prepolymerization reactor after excess water and carry out sudden reaction, wherein the temperature of oligomer melt drier is 280 DEG C, material
Residence time in oligomer melt dehydrator is that 30min, pressure from 4.0MPa are down to 1000kPa, the reaction of sudden reaction
Temperature is 220 DEG C, reaction pressure 1000kPa, reaction time 2h,
Obtain original liquid coloring Polvamide prepolymer melt；
(4) by step (3) be prepared original liquid coloring Polvamide prepolymer melt slough through pre-polymer melt dehydrator it is residual
Enter post-polymerization device after remaining moisture and carry out polycondensation reaction, wherein the temperature of pre-polymer melt drier is 230 DEG C, material exists
Residence time in oligomer melt dehydrator is that 30min, pressure from 1000kPa are down to 110kPa, the reaction temperature of polycondensation reaction
Degree be 230 DEG C, reaction pressure 110kPa, reaction time 5h,
Obtain original liquid coloring polyamide melt；
(5) original liquid coloring polyamide melt is prepared successively through pelletizing, extraction and drying in step (4), obtained opposite
The original liquid coloring red polyamide that viscosity is 2.0 is sliced, and wherein the filters pressing value DF of original liquid coloring red polyamide slice is
0.26kPa.cm2/g。
Embodiment 4
(1) the pre-dispersed material of function powder slurry being deployed by water, caprolactam and pigment violet 29 is continuously conveyed to function
Energy powdery pulp multistage grinding device carries out grinding distribution, and wherein the mass ratio of water, caprolactam and pigment violet 29 is 1:1:3,
Function powder slurry multistage grinding device is connected in series by 2 grinders, and the content for obtaining pigment violet 29 is 60wt%, averagely grain
The function powder slurry that diameter is 0.31 μm；
(2) function powder slurry and caprolactam melt and catalyst is prepared in step (1) to mix through dynamic mixer
It closes and uniformly enters hydrolysis reactor progress ring-opening reaction after heat exchanger adjusts temperature, wherein catalyst is hypophosphorous acid, catalyst
Additive amount be the 30ppm of caprolactam melt quality, the additive amount of function powder slurry is caprolactam melt quality
5.2%, the temperature of heat exchanger is 200 DEG C, and the reaction temperature of ring-opening reaction is 280 DEG C, reaction pressure 6.2MPa, reaction time
For 60min, original liquid coloring hexanolactam oligomer is obtained；
(3) original liquid coloring hexanolactam oligomer melt is prepared in step (2) to remove through oligomer melt dehydrator
Enter prepolymerization reactor after excess water and carry out sudden reaction, wherein the temperature of oligomer melt drier is 280 DEG C, material
Residence time in oligomer melt dehydrator is that 15min, pressure from 6.2MPa are down to 600kPa, the reaction temperature of sudden reaction
Degree be 260 DEG C, reaction pressure 600kPa, reaction time 4h,
Obtain original liquid coloring Polvamide prepolymer melt；
(4) by step (3) be prepared original liquid coloring Polvamide prepolymer melt slough through pre-polymer melt dehydrator it is residual
Enter post-polymerization device after remaining moisture and carry out polycondensation reaction, wherein the temperature of pre-polymer melt drier is 260 DEG C, material exists
Residence time in oligomer melt dehydrator is that 30min, pressure from 600kPa are down to 100kPa, the reaction temperature of polycondensation reaction
For 240 DEG C, reaction pressure 100kPa, reaction time 12h,
Obtain original liquid coloring polyamide melt；
(5) original liquid coloring polyamide melt is prepared successively through pelletizing, extraction and drying in step (4), obtained opposite
The 2.8 original liquid coloring purple polyamide slice that viscosity is, the filters pressing value DF that wherein original liquid coloring purple polyamide is sliced are
0.56kPa.cm2/g。
Embodiment 5
(1) the pre-dispersed material of function powder slurry being deployed by water, caprolactam and pigment orange 68 is continuously conveyed to function
Energy powdery pulp multistage grinding device carries out grinding distribution, and wherein the mass ratio of water, caprolactam and pigment orange 68 is 1:0.52:
0.08, function powder slurry multistage grinding device is connected in series by 2 grinders, and the content for obtaining pigment orange 68 is 5wt%, puts down
The function powder slurry that equal partial size is 0.21 μm；
(2) function powder slurry and caprolactam melt and catalyst is prepared in step (1) to mix through dynamic mixer
It closes and uniformly enters hydrolysis reactor progress ring-opening reaction after heat exchanger adjusts temperature, wherein catalyst is phosphoric acid, catalyst
Additive amount is the 30ppm of caprolactam melt quality, the additive amount of function powder slurry is caprolactam melt quality 19%,
The temperature of heat exchanger is 130 DEG C, and the reaction temperature of ring-opening reaction is 200 DEG C, reaction pressure 1.6MPa, reaction time are
90min obtains original liquid coloring hexanolactam oligomer；
(3) original liquid coloring hexanolactam oligomer melt is prepared in step (2) to remove through oligomer melt dehydrator
Enter prepolymerization reactor after excess water and carry out sudden reaction, wherein the temperature of oligomer melt drier is 200 DEG C, material
Residence time in oligomer melt dehydrator is that 60min, pressure from 1.6MPa are down to 1000kPa, the reaction of sudden reaction
Temperature is 220 DEG C, reaction pressure 1000kPa, reaction time 3h,
Obtain original liquid coloring Polvamide prepolymer melt；
(4) by step (3) be prepared original liquid coloring Polvamide prepolymer melt slough through pre-polymer melt dehydrator it is residual
Enter post-polymerization device after remaining moisture and carry out polycondensation reaction, wherein the temperature of pre-polymer melt drier is 230 DEG C, material exists
Residence time in oligomer melt dehydrator is that 90min, pressure from 1000kPa are down to 90kPa, the reaction temperature of polycondensation reaction
For 230 DEG C, reaction pressure 90kPa, reaction time 12h,
Obtain original liquid coloring polyamide melt；
(5) original liquid coloring polyamide melt is prepared successively through pelletizing, extraction and drying in step (4), obtained opposite
The orange polyamide slice of the original liquid coloring that viscosity is 3.2, the filters pressing value DF that wherein the orange polyamide of original liquid coloring is sliced are
0.23kPa.cm2/g。
Embodiment 6
(1) the pre-dispersed material of function powder slurry being deployed by water, caprolactam and naphthol green 50 is continuously conveyed to function
Energy powdery pulp multistage grinding device carries out grinding distribution, and wherein the mass ratio of water, caprolactam and naphthol green 50 is 1:1:
0.86, function powder slurry multistage grinding device is connected in series by 1 grinder, obtain naphthol green 50 content be 30wt%,
The function powder slurry that average grain diameter is 0.42 μm；
(2) function powder slurry and caprolactam melt and catalyst is prepared in step (1) to mix through dynamic mixer
It closes and uniformly enters hydrolysis reactor progress ring-opening reaction after heat exchanger adjusts temperature, wherein catalyst is phosphoric acid, catalyst
Additive amount is the 90ppm of caprolactam melt quality, the additive amount of function powder slurry is caprolactam melt quality
4.1%, the temperature of heat exchanger is 160 DEG C, and the reaction temperature of ring-opening reaction is 260 DEG C, reaction pressure 4.7MPa, reaction time
For 90min, original liquid coloring hexanolactam oligomer is obtained；
(3) original liquid coloring hexanolactam oligomer melt is prepared in step (2) to remove through oligomer melt dehydrator
Enter prepolymerization reactor after excess water and carry out sudden reaction, wherein the temperature of oligomer melt drier is 280 DEG C, material
Residence time in oligomer melt dehydrator is that 30min, pressure from 4.7MPa are down to 150kPa, the reaction temperature of sudden reaction
Degree be 280 DEG C, reaction pressure 150kPa, reaction time 10h,
Obtain original liquid coloring Polvamide prepolymer melt；
(4) by step (3) be prepared original liquid coloring Polvamide prepolymer melt slough through pre-polymer melt dehydrator it is residual
Enter post-polymerization device after remaining moisture and carry out polycondensation reaction, wherein the temperature of pre-polymer melt drier is 280 DEG C, material exists
Residence time in oligomer melt dehydrator is that 60min, pressure from 150kPa are down to 10kPa, the reaction temperature of polycondensation reaction
For 280 DEG C, reaction pressure 10kPa, reaction time 20h,
Obtain original liquid coloring polyamide melt；
(5) original liquid coloring polyamide melt is prepared successively through pelletizing, extraction and drying in step (4), obtained opposite
The original liquid coloring green polyamide that viscosity is 5.0 is sliced, and wherein the filters pressing value DF of original liquid coloring green polyamide slice is
0.62kPa.cm2/g。
Embodiment 7
(1) the pre-dispersed material of function powder slurry being deployed by water, caprolactam and pigment yellow 192 is continuously conveyed to function
Energy powdery pulp multistage grinding device carries out grinding distribution, and wherein the mass ratio of water, caprolactam and pigment yellow 192 is 1:1:
0.35, function powder slurry multistage grinding device is connected in series by 5 grinders, obtain pigment yellow 192 content be 15wt%,
The function powder slurry that average grain diameter is 0.18 μm；
(2) function powder slurry and caprolactam melt and catalyst is prepared in step (1) to mix through dynamic mixer
It closes and uniformly enters hydrolysis reactor progress ring-opening reaction after heat exchanger adjusts temperature, wherein catalyst is phosphoric acid, catalyst
Additive amount is the 90ppm of caprolactam melt quality, the additive amount of function powder slurry is caprolactam melt quality
17.8%, the temperature of heat exchanger is 130 DEG C, the reaction temperature of ring-opening reaction is 230 DEG C, reaction pressure 2.8MPa, reaction when
Between be 60min, obtain original liquid coloring hexanolactam oligomer；
(3) original liquid coloring hexanolactam oligomer melt is prepared in step (2) to remove through oligomer melt dehydrator
Enter prepolymerization reactor after excess water and carry out sudden reaction, wherein the temperature of oligomer melt drier is 260 DEG C, material
Residence time in oligomer melt dehydrator is that 60min, pressure from 2.8MPa are down to 150kPa, the reaction temperature of sudden reaction
Degree be 260 DEG C, reaction pressure 150kPa, reaction time 6h,
Obtain original liquid coloring Polvamide prepolymer melt；
(4) by step (3) be prepared original liquid coloring Polvamide prepolymer melt slough through pre-polymer melt dehydrator it is residual
Enter post-polymerization device after remaining moisture and carry out polycondensation reaction, wherein the temperature of pre-polymer melt drier is 230 DEG C, material exists
Residence time in oligomer melt dehydrator is that 90min, pressure from 150kPa are down to 40kPa, the reaction temperature of polycondensation reaction
For 240 DEG C, reaction pressure 40kPa, reaction time 12h,
Obtain original liquid coloring polyamide melt；
(5) original liquid coloring polyamide melt is prepared successively through pelletizing, extraction and drying in step (4), obtained opposite
The original liquid coloring yellow polyamide that viscosity is 4.0 is sliced, and wherein the filters pressing value DF of original liquid coloring yellow polyamide slice is
0.21kPa.cm2/g。
Embodiment 8
(1) the pre-dispersed material of function powder slurry being deployed by water, caprolactam and antibacterial agent cuprous oxide is continuously defeated
It send to function powder slurry multistage grinding device and carries out grinding distribution, wherein the mass ratio of water, caprolactam and cuprous oxide is
1:1:1.33, function powder slurry multistage grinding device are connected in series by 5 grinders, and the content for obtaining cuprous oxide is
40wt%, the function powder slurry that average grain diameter is 0.09 μm；
(2) function powder slurry and caprolactam melt and catalyst is prepared in step (1) to mix through dynamic mixer
It closes and uniformly enters hydrolysis reactor progress ring-opening reaction after heat exchanger adjusts temperature, wherein catalyst is phosphoric acid, catalyst
Additive amount is the 90ppm of caprolactam melt quality, the additive amount of function powder slurry is caprolactam melt quality
7.9%, the temperature of heat exchanger is 160 DEG C, and the reaction temperature of ring-opening reaction is 250 DEG C, reaction pressure 4.0MPa, reaction time
For 60min, function hexanolactam oligomer is obtained；
(3) function hexanolactam oligomer melt is prepared in step (2) to remove excessively through oligomer melt dehydrator
Enter prepolymerization reactor after moisture and carry out sudden reaction, wherein the temperature of oligomer melt drier is 270 DEG C, material is low
Residence time in polymer melt dehydrator is that 30min, pressure from 4.0MPa are down to 600kPa, and the reaction temperature of sudden reaction is
270 DEG C, reaction pressure 600kPa, reaction time 3h,
Obtain function Polvamide prepolymer melt；
(4) function Polvamide prepolymer melt is prepared in step (3) and sloughs residual water through pre-polymer melt dehydrator
Enter post-polymerization device after point and carry out polycondensation reaction, wherein the temperature of pre-polymer melt drier is 260 DEG C, material is oligomeric
Residence time in object melt dehydrator is that 30min, pressure from 600kPa are down to 110kPa, and the reaction temperature of polycondensation reaction is
230 DEG C, reaction pressure 110kPa, reaction time 10h,
Obtain function polyamide melt；
(5) function polyamide melt is prepared successively through pelletizing, extraction and drying in step (4), obtains relative viscosity
It is sliced for 2.4 antibacterial polyamide, wherein the filters pressing value DF of antibacterial polyamide slice is 0.16kPa.cm2/g。
Embodiment 9
(1) the function powder slurry being deployed by water, caprolactam and the yellowish green luminescent powder of fluorescer (ZnS:Cu) is divided in advance
Bulk cargo is continuously conveyed to function powder slurry multistage grinding device and carries out grinding distribution, wherein water, caprolactam and yellowish green noctilucence
The mass ratio of powder (ZnS:Cu) is 1:1:0.22, and function powder slurry multistage grinding device is connected in series by 1 grinder, is obtained
The function powder slurry that the content of yellowish green luminescent powder (ZnS:Cu) is 10wt%, average grain diameter is 0.50 μm；
(2) function powder slurry and caprolactam melt and catalyst is prepared in step (1) to mix through dynamic mixer
It closes and uniformly enters hydrolysis reactor progress ring-opening reaction after heat exchanger adjusts temperature, wherein catalyst is phosphoric acid, catalyst
Additive amount is the 30ppm of caprolactam melt quality, the additive amount of function powder slurry is caprolactam melt quality
36.3%, the temperature of heat exchanger is 130 DEG C, the reaction temperature of ring-opening reaction is 200 DEG C, reaction pressure 1.6MPa, reaction when
Between be 30min, obtain function hexanolactam oligomer；
(3) function hexanolactam oligomer melt is prepared in step (2) to remove excessively through oligomer melt dehydrator
Enter prepolymerization reactor after moisture and carry out sudden reaction, wherein the temperature of oligomer melt drier is 220 DEG C, material is low
Residence time in polymer melt dehydrator is that 15min, pressure from 1.6MPa are down to 1000kPa, the reaction temperature of sudden reaction
For 220 DEG C, reaction pressure 1000kPa, reaction time 2h,
Obtain function Polvamide prepolymer melt；
(4) function Polvamide prepolymer melt is prepared in step (3) and sloughs residual water through pre-polymer melt dehydrator
Enter post-polymerization device after point and carry out polycondensation reaction, wherein the temperature of pre-polymer melt drier is 230 DEG C, material is oligomeric
Residence time in object melt dehydrator is that 30min, pressure from 1000kPa are down to 80kPa, and the reaction temperature of polycondensation reaction is
230 DEG C, reaction pressure 80kPa, reaction time 5h,
Obtain function polyamide melt；
(5) function polyamide melt is prepared successively through pelletizing, extraction and drying in step (4), obtains relative viscosity
It is sliced for 2.0 fluorescent polyamide, wherein the filters pressing value DF of fluorescent polyamide slice is 0.71kPa.cm2/g。
Embodiment 10
(1) the pre-dispersed material of function powder slurry that will be deployed by water, caprolactam and far-infrared functional powder zirconium carbide
It is continuously conveyed to function powder slurry multistage grinding device and carries out grinding distribution, wherein the quality of water, caprolactam and zirconium carbide
Than for 1:0.52:0.08, function powder slurry multistage grinding device is connected in series by 2 grinders, the content of zirconium carbide is obtained
The function powder slurry for being 0.14 μm for 5wt%, average grain diameter；
(2) function powder slurry and caprolactam melt and catalyst is prepared in step (1) to mix through dynamic mixer
It closes and uniformly enters hydrolysis reactor progress ring-opening reaction after heat exchanger adjusts temperature, wherein catalyst is metaphosphoric acid, catalyst
Additive amount be the 1000ppm of caprolactam melt quality, the additive amount of function powder slurry is caprolactam melt quality
19.3%, the temperature of heat exchanger is 130 DEG C, the reaction temperature of ring-opening reaction is 220 DEG C, reaction pressure 2.3MPa, reaction when
Between be 30min, obtain function hexanolactam oligomer；
(3) function hexanolactam oligomer melt is prepared in step (2) to remove excessively through oligomer melt dehydrator
Enter prepolymerization reactor after moisture and carry out sudden reaction, wherein the temperature of oligomer melt drier is 260 DEG C, material is low
Residence time in polymer melt dehydrator is that 60min, pressure from 2.3MPa are down to 300kPa, and the reaction temperature of sudden reaction is
260 DEG C, reaction pressure 300kPa, reaction time 4h,
Obtain function Polvamide prepolymer melt；
(4) function Polvamide prepolymer melt is prepared in step (3) and sloughs residual water through pre-polymer melt dehydrator
Enter post-polymerization device after point and carry out polycondensation reaction, wherein the temperature of pre-polymer melt drier is 260 DEG C, material is oligomeric
Residence time in object melt dehydrator is that 60min, pressure from 300kPa are down to 100kPa, and the reaction temperature of polycondensation reaction is
240 DEG C, reaction pressure 100kPa, reaction time 12h,
Obtain function polyamide melt；
(5) function polyamide melt is prepared successively through pelletizing, extraction and drying in step (4), obtains relative viscosity
It is sliced for 2.8 far infrared polyamide, the filters pressing value DF of mid and far infrared polyamide slice is 0.19kPa.cm2/g。
Embodiment 11
(1) the pre-dispersed material of function powder slurry being deployed by water, caprolactam and thermal conducting agent aluminium nitride is continuously conveyed
Grinding distribution is carried out to function powder slurry multistage grinding device, wherein the mass ratio of water, caprolactam and aluminium nitride is 1:1:
3, function powder slurry multistage grinding device is connected in series by 3 grinders, and the content for obtaining aluminium nitride is 60wt%, averagely grain
The function powder slurry that diameter is 0.18 μm；
(2) function powder slurry and caprolactam melt and catalyst is prepared in step (1) to mix through dynamic mixer
It closes and uniformly enters hydrolysis reactor progress ring-opening reaction after heat exchanger adjusts temperature, wherein catalyst is phosphoric acid, catalyst
Additive amount is the 400ppm of caprolactam melt quality, the additive amount of function powder slurry is caprolactam melt quality
5.2%, the temperature of heat exchanger is 200 DEG C, and the reaction temperature of ring-opening reaction is 280 DEG C, reaction pressure 6.2MPa, reaction time
For 30min, function hexanolactam oligomer is obtained；
(3) function hexanolactam oligomer melt is prepared in step (2) to remove excessively through oligomer melt dehydrator
Enter prepolymerization reactor after moisture and carry out sudden reaction, wherein the temperature of oligomer melt drier is 280 DEG C, material is low
Residence time in polymer melt dehydrator is that 15min, pressure from 6.2MPa are down to 150kPa, and the reaction temperature of sudden reaction is
280 DEG C, reaction pressure 150kPa, reaction time 10h,
Obtain function Polvamide prepolymer melt；
(4) function Polvamide prepolymer melt is prepared in step (3) and sloughs residual water through pre-polymer melt dehydrator
Enter post-polymerization device after point and carry out polycondensation reaction, wherein the temperature of pre-polymer melt drier is 280 DEG C, material is oligomeric
Residence time in object melt dehydrator is 30min, pressure from 150kPa is down to 40kPa, and the reaction temperature of polycondensation reaction is 280
DEG C, reaction pressure 40kPa, reaction time 20h,
Obtain function polyamide melt；
(5) function polyamide melt is prepared successively through pelletizing, extraction and drying in step (4), obtains relative viscosity
It is sliced for 5.0 thermally conductive polyamide, wherein the filters pressing value DF of thermally conductive polyamide slice is 0.31kPa.cm2/g。
Embodiment 12
(1) the pre-dispersed material of function powder slurry being deployed by water, caprolactam and uvioresistant zinc oxide is continuously conveyed
Grinding distribution is carried out to function powder slurry multistage grinding device, wherein the mass ratio of water, caprolactam and zinc oxide is 1:1:
0.86, function powder slurry multistage grinding device is connected in series by 3 grinders, and the content for obtaining zinc oxide is 30wt%, puts down
The function powder slurry that equal partial size is 0.33 μm；
(2) function powder slurry and caprolactam melt and catalyst is prepared in step (1) to mix through dynamic mixer
It closes and uniformly enters hydrolysis reactor progress ring-opening reaction after heat exchanger adjusts temperature, wherein catalyst is phosphoric acid, catalyst
Additive amount is the 100ppm of caprolactam melt quality, the additive amount of function powder slurry is caprolactam melt quality
6.2%, the temperature of heat exchanger is 160 DEG C, and the reaction temperature of ring-opening reaction is 260 DEG C, reaction pressure 4.7MPa, reaction time
For 90min, function hexanolactam oligomer is obtained；
(3) function hexanolactam oligomer melt is prepared in step (2) to remove excessively through oligomer melt dehydrator
Enter prepolymerization reactor after moisture and carry out sudden reaction, wherein the temperature of oligomer melt drier is 270 DEG C, material is low
Residence time in polymer melt dehydrator is that 60min, pressure from 4.7MPa are down to 300kPa, and the reaction temperature of sudden reaction is
270 DEG C, reaction pressure 300kPa, reaction time 5h,
Obtain function Polvamide prepolymer melt；
(4) function Polvamide prepolymer melt is prepared in step (3) and sloughs residual water through pre-polymer melt dehydrator
Enter post-polymerization device after point and carry out polycondensation reaction, wherein the temperature of pre-polymer melt drier is 270 DEG C, material is oligomeric
Residence time in object melt dehydrator is 90min, pressure from 300kPa is down to 10kPa, and the reaction temperature of polycondensation reaction is 240
DEG C, reaction pressure 10kPa, reaction time 10h,
Obtain function polyamide melt；
(5) function polyamide melt is prepared successively through pelletizing, extraction and drying in step (4), obtains relative viscosity
It is sliced for 3.8 uvioresistant poly amide, wherein the filters pressing value DF of uvioresistant poly amide slice is 0.26kPa.cm2/g。
Embodiment 13
(1) the pre-dispersed material of function powder slurry being deployed by water, caprolactam and antimicrobial powder graphene is continuously defeated
It send to function powder slurry multistage grinding device and carries out grinding distribution, wherein the mass ratio of water, caprolactam and graphene is 1:
0.94:0.06, function powder slurry multistage grinding device are connected in series by 3 grinders, and the content for obtaining graphene is
3wt%, the function powder slurry that average grain diameter is 1.00 μm；
(2) function powder slurry and caprolactam melt and catalyst is prepared in step (1) to mix through dynamic mixer
It closes and uniformly enters hydrolysis reactor progress ring-opening reaction after heat exchanger adjusts temperature, wherein catalyst is metaphosphoric acid, catalyst
Additive amount be the 1000ppm of caprolactam melt quality, the additive amount of function powder slurry is caprolactam melt quality
22.1%, the temperature of heat exchanger is 130 DEG C, the reaction temperature of ring-opening reaction is 220 DEG C, reaction pressure 2.3MPa, reaction when
Between be 30min, obtain function hexanolactam oligomer；
(3) function hexanolactam oligomer melt is prepared in step (2) to remove excessively through oligomer melt dehydrator
Enter prepolymerization reactor after moisture and carry out sudden reaction, wherein the temperature of oligomer melt drier is 260 DEG C, material is low
Residence time in polymer melt dehydrator is that 60min, pressure from 2.3MPa are down to 300kPa, and the reaction temperature of sudden reaction is
260 DEG C, reaction pressure 300kPa, reaction time 4h,
Obtain function Polvamide prepolymer melt；
(4) function Polvamide prepolymer melt is prepared in step (3) and sloughs residual water through pre-polymer melt dehydrator
Enter post-polymerization device after point and carry out polycondensation reaction, wherein the temperature of pre-polymer melt drier is 260 DEG C, material is oligomeric
Residence time in object melt dehydrator is that 60min, pressure from 300kPa are down to 100kPa, and the reaction temperature of polycondensation reaction is
240 DEG C, reaction pressure 100kPa, reaction time 10h,
Obtain function polyamide melt；
(5) function polyamide melt is prepared successively through pelletizing, extraction and drying in step (4), obtains relative viscosity
It is sliced for 2.4 antibacterial polyamide, wherein the filters pressing value DF of antibacterial polyamide slice is 0.80kPa.cm2/g。
Embodiment 14
(1) the pre-dispersed material of function powder slurry being deployed by water, caprolactam and conductive agent tin-antiomony oxide is continuously defeated
It send to function powder slurry multistage grinding device and carries out grinding distribution, wherein the mass ratio of water, caprolactam and tin-antiomony oxide is
1:0.86:0.8, function powder slurry multistage grinding device are connected in series by 5 grinders, and the content for obtaining tin-antiomony oxide is
30wt%, the function powder slurry that average grain diameter is 0.08 μm；
(2) function powder slurry and caprolactam melt and catalyst is prepared in step (1) to mix through dynamic mixer
It closes and uniformly enters hydrolysis reactor progress ring-opening reaction after heat exchanger adjusts temperature, wherein catalyst is hypophosphorous acid, catalyst
Additive amount be the 30ppm of caprolactam melt quality, the additive amount of function powder slurry is caprolactam melt quality
10.3%, the temperature of heat exchanger is 200 DEG C, the reaction temperature of ring-opening reaction is 260 DEG C, reaction pressure 4.7MPa, reaction when
Between be 60min, obtain original liquid coloring hexanolactam oligomer；
(3) original liquid coloring hexanolactam oligomer melt is prepared in step (2) to remove through oligomer melt dehydrator
Enter prepolymerization reactor after excess water and carry out sudden reaction, wherein the temperature of oligomer melt drier is 280 DEG C, material
Residence time in oligomer melt dehydrator is that 15min, pressure from 4.7MPa are down to 600kPa, the reaction temperature of sudden reaction
Degree be 260 DEG C, reaction pressure 600kPa, reaction time 4h,
Obtain original liquid coloring Polvamide prepolymer melt；
(4) by step (3) be prepared original liquid coloring Polvamide prepolymer melt slough through pre-polymer melt dehydrator it is residual
Enter post-polymerization device after remaining moisture and carry out polycondensation reaction, wherein the temperature of pre-polymer melt drier is 260 DEG C, material exists
Residence time in oligomer melt dehydrator is that 30min, pressure from 600kPa are down to 100kPa, the reaction temperature of polycondensation reaction
For 240 DEG C, reaction pressure 100kPa, reaction time 12h,
Obtain original liquid coloring polyamide melt；
(5) original liquid coloring polyamide melt is prepared successively through pelletizing, extraction and drying in step (4), obtained opposite
The static resistant polyamide that viscosity is 2.8 is sliced, and wherein the filters pressing value DF of static resistant polyamide slice is 0.18kPa.cm2/g。
Embodiment 15
(1) the pre-dispersed material of the function powder slurry being deployed by water, caprolactam and anion propellant tourmaline is connected
The continuous function powder slurry multistage grinding device that is delivered to carries out grinding distribution, wherein the mass ratio of water, caprolactam and tourmaline
For 1:0.84:0.46, function powder slurry multistage grinding device is connected in series by 3 grinders, and the content for obtaining tourmaline is
20wt%, the function powder slurry that average grain diameter is 0.21 μm；
(2) function powder slurry and caprolactam melt and catalyst is prepared in step (1) to mix through dynamic mixer
It closes and uniformly enters hydrolysis reactor progress ring-opening reaction after heat exchanger adjusts temperature, wherein catalyst is metaphosphoric acid, catalyst
Additive amount be the 1000ppm of caprolactam melt quality, the additive amount of function powder slurry is caprolactam melt quality
10.4%, the temperature of heat exchanger is 180 DEG C, the reaction temperature of ring-opening reaction is 250 DEG C, reaction pressure 4.0MPa, reaction when
Between be 30min, obtain original liquid coloring hexanolactam oligomer；
(3) original liquid coloring hexanolactam oligomer melt is prepared in step (2) to remove through oligomer melt dehydrator
Enter prepolymerization reactor after excess water and carry out sudden reaction, wherein the temperature of oligomer melt drier is 280 DEG C, material
Residence time in oligomer melt dehydrator is that 30min, pressure from 4.0MPa are down to 1000kPa, the reaction of sudden reaction
Temperature is 220 DEG C, reaction pressure 1000kPa, reaction time 2h,
Obtain original liquid coloring Polvamide prepolymer melt；
(4) by step (3) be prepared original liquid coloring Polvamide prepolymer melt slough through pre-polymer melt dehydrator it is residual
Enter post-polymerization device after remaining moisture and carry out polycondensation reaction, wherein the temperature of pre-polymer melt drier is 230 DEG C, material exists
Residence time in oligomer melt dehydrator is that 30min, pressure from 1000kPa are down to 110kPa, the reaction temperature of polycondensation reaction
Degree be 230 DEG C, reaction pressure 110kPa, reaction time 10h,
Obtain original liquid coloring polyamide melt；
(5) original liquid coloring polyamide melt is prepared successively through pelletizing, extraction and drying in step (4), obtained opposite
The negative ion polyamide that viscosity is 2.4 is sliced, and wherein the filters pressing value DF of negative ion polyamide slice is 0.56kPa.cm2/g。
Comparative example 1
By polyamide slice and pigment blue 15: 3 concentration are that the functional agglomerate of 25wt% mixes according to mass ratio 1:0.106
Enter screw extruder after even, extruding pelletization obtains function after melt blending under the conditions of 260 DEG C of temperature through screw extruder
Polyamide slice, the inherent viscosity of function polyamide slice is 2.4, filters pressing value DF is 1.14kPa.cm2/g。
The slice of function polyamide prepared by embodiment 1~15 as above and comparative example 1 is tested for the property, test item
Mesh is as follows: function powder average grain diameter (μm) in function powder slurry, test method: being tested using dynamic light scattering particle size instrument；
Function polyamide is sliced relative viscosity, test method: referring to FZ/T 51004-2011；Function polyamide filters pressing value DF
(kPa.cm2/ g), test method: by single screw extrusion machine that draw ratio is Φ 25mm × 25D, the melt meter that volume is 1.2cc
Amount pump, melt force sensor and screen area S are 3.8cm2Four layers of combination strainer of 60-100-1400-100-20 mesh successively
Connection composition filters pressing ability meter；Filters pressing performance test process conditions: melt temperature is 270 DEG C, presses before melt metering pump pump
Power setting value is 6.5MPa, melt metering pump metered flow is 38g/min；First polyamide 6 is squeezed from filters pressing ability meter
Out, record balance pressure is initial pressure Ps, then squeezes out 3000g function polyamide from filters pressing ability meter, then will
500g polyamide 6 is squeezed out from filters pressing ability meter, and record balance pressure is termination pressure PT, finally according to formula:Filters pressing value DF is calculated.Test result is shown in Table 1.
As the data in table 1 it is found that using function polyamides prepared by function polyamide continuous producing method of the invention
The filters pressing value DF of amine is not higher than 0.8kPa.cm2/ g, and there is lower pressure compared to the function polyamide of masterbatch method preparation
Filter value shows function polyamide prepared by function polyamide continuous producing method of the invention with higher function powder point
Dissipate the uniformity.
The embodiment of the present invention 1 and comparative example 1 prepare function polyamide and use identical pigment blue 15: 3 additive amounts, but real
Apply pigment blue 15 in example 1: 3 are added in caprolactam melt using open loop in the form of the function powder slurry continuously prepared
Reaction, sudden reaction and polycondensation reaction obtain function polyamide；Pigment blue 15 in comparative example 1: 3 are added in the form of functional agglomerate
Function polyamide melt is prepared through screw extruder melt blending again into polyamide slice.Since masterbatch method prepares function
During polyamide, dispersion of the function powder in high bondable polyamide melt mainly relies on machinery provided by mixing apparatus
Shearing force keeps the function being prepared poly- so that it is evenly dispersed to be difficult to realize height of the function powder particle in polyamide melt
The spinning of amide slice and drawing-die performance are poor.The preparation of function powder slurry uses grinder, in the height of grinder disperser
Under speed operating, grinder abrasive media will generate strong collision, friction, shear action between the colorant particles of solid,
To realize function powder in the aqueous solution of caprolactam with the dispersion of small scale efficient uniform.Function powder slurry and acyl in oneself
Function powder is prepared using ring-opening reaction, sudden reaction and polycondensation reaction after dynamic mixer efficiently mixes in amine melt
The function polyamide of particle high uniformity dispersion, effectively reduces pigment blue 15 in function polyamide preparation process: the group of 3 particles
It is poly-.The filters pressing value DF of function polyamide is 0.21kPa.cm in embodiment 12The filters pressing value DF of function polyamide in/g, comparative example 1
For 1.14kPa.cm2/g。
Although preferred embodiments of the present invention have been described, it is created once a person skilled in the art knows basic
Property concept, then additional changes and modifications may be made to these embodiments.So it includes excellent that the following claims are intended to be interpreted as
It selects embodiment and falls into all change and modification of the scope of the invention.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
Mind and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to include these modifications and variations.
Claims (10)
1. function polyamide continuous producing method, which is characterized in that the method includes following steps:
(1) the pre-dispersed material of function powder slurry being deployed by water, caprolactam and function powder is continuously conveyed to function powder
Somaplasm material multistage grinding device carries out grinding distribution, obtains function powder slurry；
(2) function powder slurry is prepared in step (1) to mix with caprolactam melt and catalyst through dynamic mixer
It is even to enter hydrolysis reactor progress ring-opening reaction after heat exchanger adjusts temperature, obtain function hexanolactam oligomer melt；
(3) function hexanolactam oligomer melt is prepared in step (2) and removes excess water through oligomer melt dehydrator
Enter prepolymerization reactor afterwards and carry out sudden reaction, obtains function Polvamide prepolymer melt；
(4) function Polvamide prepolymer melt is prepared after pre-polymer melt dehydrator sloughs residual moisture in step (3)
Polycondensation reaction is carried out into post-polymerization device, obtains function polyamide melt；
(5) function polyamide melt is prepared successively through pelletizing, extraction and drying in step (4), obtains function polyamide and cuts
Piece.
2. function polyamide continuous producing method according to claim 1, which is characterized in that in step (1), the function powder
Somaplasm material multistage grinding device is connected in series by 1~5 grinder.
3. function polyamide continuous producing method according to claim 1, which is characterized in that in step (2), the hydrolysis is anti-
Answering device is the tower reactor of built-in mixed cell, and material bottom in and top out is flowed in plug flow.
4. function polyamide continuous producing method according to claim 1, which is characterized in that in step (2), the catalyst
For Bronsted acid.
5. function polyamide continuous producing method according to claim 1, which is characterized in that in step (1), the function powder
The average grain diameter of function powder is not higher than 1 μm in somaplasm material.
6. function polyamide continuous producing method according to claim 1, which is characterized in that in step (1), the water,
Caprolactam, function powder mass ratio be 1:(0.5~1): (0.06~3).
7. function polyamide continuous producing method according to claim 1, which is characterized in that in step (2), the catalysis
The additive amount of agent is 30~1000ppm of caprolactam melt quality.
8. function polyamide continuous producing method according to claim 1, which is characterized in that in step (2), heat exchanger
Temperature is 130~200 DEG C；
Preferably, in step (2), the reaction temperature of the ring-opening reaction is 200~280 DEG C, reaction pressure is 1.6~
6.2MPa, reaction time are 30~90min；
Preferably, the temperature of the oligomer melt dehydrator is 220~280 DEG C, and material is molten in oligomer in step (3)
The residence time is 15~60min in body dehydrator, and pressure is down to 150kPa~1000kPa from 1.6~6.2MPa；
Preferably, in step (3), the reaction temperature of the sudden reaction is 220~280 DEG C, reaction pressure be 150kPa~
1000kPa, reaction time are 2~10h；
Preferably, the temperature of the pre-polymer melt dehydrator is 230~280 DEG C, and material is molten in oligomer in step (4)
The residence time is 30~90min in body dehydrator, and pressure is down to 10kPa~110kPa from 150kPa~1000kPa；
Preferably, in step (4), the reaction temperature of the polycondensation reaction is 230~280 DEG C, reaction pressure be 10kPa~
110kPa, reaction time are 5~20h.
9. function polyamide, which is characterized in that by function polyamide described in any item of the claim 1 to 8 continuous production side
Method is prepared.
10. function polyamide according to claim 9, which is characterized in that the relative viscosity of the function polyamide is 2.0
~5.0, filters pressing value DF is not higher than 0.8kPa.cm2/g。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811595090.8A CN109762162B (en) | 2018-12-25 | 2018-12-25 | Functional polyamide and continuous production method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811595090.8A CN109762162B (en) | 2018-12-25 | 2018-12-25 | Functional polyamide and continuous production method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109762162A true CN109762162A (en) | 2019-05-17 |
| CN109762162B CN109762162B (en) | 2021-07-06 |
Family
ID=66450289
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811595090.8A Active CN109762162B (en) | 2018-12-25 | 2018-12-25 | Functional polyamide and continuous production method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109762162B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112724398A (en) * | 2021-01-28 | 2021-04-30 | 海阳科技股份有限公司 | Production device and process for in-situ polymerization coloring graphene modified polyamide-6 slice |
| CN113336937A (en) * | 2021-07-02 | 2021-09-03 | 中国纺织科学研究院有限公司 | Preparation method of polyamide 6 and polyamide 6 |
| CN114835893A (en) * | 2022-06-10 | 2022-08-02 | 盐城工学院 | Preparation method of polyamide with ultraviolet absorption and fluorescence functions, product and application thereof |
| CN114875521A (en) * | 2022-06-02 | 2022-08-09 | 浙江理工大学 | Preparation method of efficient antibacterial and antiviral fiber |
| CN114875513A (en) * | 2022-06-02 | 2022-08-09 | 浙江理工大学 | Preparation method of nano-copper antibacterial and antiviral black fiber |
| CN114892300A (en) * | 2022-06-02 | 2022-08-12 | 浙江理工大学 | Preparation method of antibacterial antiviral thermal fiber |
| CN115536837A (en) * | 2022-10-14 | 2022-12-30 | 杭州明日新材料科技有限公司 | Polyamide material and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4172161A (en) * | 1977-07-13 | 1979-10-23 | Chemische Werke Huls Ag | Pulverulent copolyamides for the coating of glass bottles |
| CN101928457A (en) * | 2010-05-18 | 2010-12-29 | 赵明久 | Carbon-based nano cast nylon composite material and in-situ polymerization preparation method thereof |
| CN102653591A (en) * | 2012-05-23 | 2012-09-05 | 浙江华建尼龙有限公司 | Process for producing caprolactam and nylon 66 salt copolymer slice |
| CN104387580A (en) * | 2014-11-05 | 2015-03-04 | 湖南金帛化纤有限公司 | Nylon-6 slice production method capable of improving polymerization conversion rate |
| CN107022076A (en) * | 2017-04-14 | 2017-08-08 | 长乐力恒锦纶科技有限公司 | A kind of preparation method of the deep dye section of polyamide fibre 6 |
-
2018
- 2018-12-25 CN CN201811595090.8A patent/CN109762162B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4172161A (en) * | 1977-07-13 | 1979-10-23 | Chemische Werke Huls Ag | Pulverulent copolyamides for the coating of glass bottles |
| CN101928457A (en) * | 2010-05-18 | 2010-12-29 | 赵明久 | Carbon-based nano cast nylon composite material and in-situ polymerization preparation method thereof |
| CN102653591A (en) * | 2012-05-23 | 2012-09-05 | 浙江华建尼龙有限公司 | Process for producing caprolactam and nylon 66 salt copolymer slice |
| CN104387580A (en) * | 2014-11-05 | 2015-03-04 | 湖南金帛化纤有限公司 | Nylon-6 slice production method capable of improving polymerization conversion rate |
| CN107022076A (en) * | 2017-04-14 | 2017-08-08 | 长乐力恒锦纶科技有限公司 | A kind of preparation method of the deep dye section of polyamide fibre 6 |
Non-Patent Citations (3)
| Title |
|---|
| BERND ROTHE ET AL.: "Masterbatch Production of Polyamide 6-Clay Compounds via Continuous In Situ Polymerization from Caprolactam and Layered Silicates", 《JOURNAL OF APPLIED POLYMER SCIENCE》 * |
| 梁霄 等: "功能化二硫化钼／聚酰胺复合材料的制备及性能研究", 《安徽大学学报（自然科学版）》 * |
| 赵亚奇: "《高分子自由基合成技术研究》", 31 December 2017, 中央名族大学出版社 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112724398A (en) * | 2021-01-28 | 2021-04-30 | 海阳科技股份有限公司 | Production device and process for in-situ polymerization coloring graphene modified polyamide-6 slice |
| CN113336937A (en) * | 2021-07-02 | 2021-09-03 | 中国纺织科学研究院有限公司 | Preparation method of polyamide 6 and polyamide 6 |
| CN114875521A (en) * | 2022-06-02 | 2022-08-09 | 浙江理工大学 | Preparation method of efficient antibacterial and antiviral fiber |
| CN114875513A (en) * | 2022-06-02 | 2022-08-09 | 浙江理工大学 | Preparation method of nano-copper antibacterial and antiviral black fiber |
| CN114892300A (en) * | 2022-06-02 | 2022-08-12 | 浙江理工大学 | Preparation method of antibacterial antiviral thermal fiber |
| CN114835893A (en) * | 2022-06-10 | 2022-08-02 | 盐城工学院 | Preparation method of polyamide with ultraviolet absorption and fluorescence functions, product and application thereof |
| CN114835893B (en) * | 2022-06-10 | 2023-12-19 | 盐城工学院 | Preparation method of polyamide with ultraviolet absorption fluorescence function, product and application thereof |
| CN115536837A (en) * | 2022-10-14 | 2022-12-30 | 杭州明日新材料科技有限公司 | Polyamide material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109762162B (en) | 2021-07-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109762162A (en) | Functionality polyamide and its continuous producing method | |
| CN109811423B (en) | Production method of continuous polymerization melt direct spinning functional polyamide fiber and functional polyamide fiber | |
| CN109679076B (en) | Functional polyester product and preparation method thereof | |
| CN109705319B (en) | Functional polyester production method and system and functional polyester fiber | |
| CN101215404B (en) | Special-purpose material for spinning-stage polyetheretherketone resin and preparation method thereof | |
| CN109705320B (en) | Method for continuously producing polyester functional master batch and polyester functional master batch | |
| CN105254870B (en) | A kind of high-performance monomer moulding casting nylon/graphene nanocomposite material and its in-situ polymerization method for preparing | |
| CN107513162A (en) | A kind of preparation method of graphene/nylon 6 nano-composite | |
| CN109750385B (en) | Continuous production system and preparation method of functional polyester | |
| CN100999413A (en) | Nanometer ceramic powder sizing agent composition and its preparation method | |
| CN102400234B (en) | Method for preparing polyacrylonitrile-based carbon fiber protofilament spinning stock solution | |
| CN112694610A (en) | Modified para-aramid polymer liquid, coating slurry, lithium battery diaphragm and preparation method thereof | |
| CN111101217A (en) | High-thermal-conductivity ultra-high molecular weight polyethylene fiber and preparation method thereof | |
| CN103031006A (en) | Surface treatment method of inorganic nano-microparticle and preparation method of composite material | |
| CN102732032B (en) | Corona-resistant polyimide film and process for preparing same | |
| CN112844280A (en) | Horizontal reaction kettle, functional polyester production system applying same and production method | |
| CN102400239B (en) | Method for manufacturing polyacrylonitrile base carbon fiber precursor | |
| CN106752384B (en) | Elastic nanofiber conductive ink and preparation method and application thereof | |
| CN109852047B (en) | Functional polyamide production system, production method and functional polyamide | |
| US20160122479A1 (en) | Process for dispersing particles in filled resin compositions | |
| JP6746443B2 (en) | Hexagonal boron nitride powder | |
| CN102964815A (en) | Microscopically well-dispersed high performance nano reinforced nylon composite and preparation method thereof | |
| CN109851824B (en) | Method for continuously producing polyamide functional master batch and polyamide functional master batch | |
| CN101871138A (en) | Method for manufacturing nylon6/nanometer SiO2 composite fiber material | |
| CN103012933A (en) | Polyethylene/nano silica hybrid material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |