CN107325279A - A kind of method of continuous production semi-aromatic nylon - Google Patents
A kind of method of continuous production semi-aromatic nylon Download PDFInfo
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- CN107325279A CN107325279A CN201710675222.7A CN201710675222A CN107325279A CN 107325279 A CN107325279 A CN 107325279A CN 201710675222 A CN201710675222 A CN 201710675222A CN 107325279 A CN107325279 A CN 107325279A
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- aromatic nylon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/28—Preparatory processes
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- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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Abstract
The present invention relates to a kind of method of continuous production semi-aromatic nylon, belong to preparation and the production field of nylon.Semi-aromatic nylon salt and water and other auxiliary agents are added dissolution kettle and melted by it, pass sequentially through evaporator, reactor, flash vessel and polymerizer, and reaction obtains semi-aromatic nylon.Production efficiency of the present invention is high, and product quality is stable, it is easy to mass produce, the semi-aromatic nylon of production can be used in terms of automobile, electronic apparatus.
Description
Technical field
The present invention relates to a kind of method of continuous production semi-aromatic nylon, belong to preparation and the production field of nylon.
Background technology
The end of last century because electronics, motor part, auto parts plastic, its performance is had the further requirement that,
The particularly development of surface mounting technology (Surface Mount Technology, abbreviation SMT), connector, switch, after
The various electric elements such as electrical equipment, capacitor are installed, connected in the circuit board simultaneously, promote electronic component miniaturization, densification.
But, using SMT technologies, each electric elements and circuit base plate will be heated in infrared heating device simultaneously, each to being made
The resistance to reflow and dimensional stability of the material of individual element and wiring board proposes higher requirement.Traditional PA66, PA6 etc.
The heat resistance of material can not meet requirement.
Semi-aromatic nylon is that diamines or dicarboxylic acids with aromatic ring are prepared with aliphatic dicarboxylic acid or diamines polycondensation reaction
Polyamide.Due to having imported aromatic ring in polyamide molecule main chain, semiaromatic polyamide composition is than conventional polyamide（Such as nylon 6,
Nylon66 fiber）There are higher heat resistance and more low water absorption.With developing rapidly for technology, electronics industry and car industry are to being used
The performance such as the heat resistance of polyamide have higher requirement, this cause semiaromatic polyamide composition have in these areas it is wide should
Use prospect.
Current most patent is all to produce semi-aromatic nylon with the method for interval.With semi-aromatic nylon
Extensive using increasingly coming, urgent need is a kind of semi-aromatic nylon is met with high yield, the production method of steady quality increasingly
The demand of growth.
The content of the invention
The purpose of the present invention is to overcome above-mentioned weak point there is provided a kind of method of continuous production semi-aromatic nylon,
The semi-aromatic nylon yield that this method is produced is high, steady quality.
Technical scheme, a kind of method of continuous production semi-aromatic nylon, mainly by 5 main reactor
（Dissolution kettle, evaporator, reactor, flash vessel, polymerizer）Realize composition.
Semi-aromatic nylon come from the % of 70 moles of more than %, preferably 80 moles of the construction unit of Long carbon chain diamine component with
Upper, more preferably 90 moles more than % come from Long carbon chain diamines, 70 moles of more than % of the construction unit of dicarboxylic acid component, preferably
80 moles of more than % of more than %, more preferably 90 moles come from aromatic diacid.
Long carbon chain diamine is made up of bioanalysis or chemical method, and it, which is originated, to be oil, its biological spin-off.Long carbon chain
Diamine include but is not limited to decamethylene diamine, 11 carbon diamines, 12 carbon diamines, 13 carbon diamines, 14 carbon diamines,
15 carbon diamines, 16 carbon diamines, 17 carbon diamines, preferably DC18, decamethylene diamine.
As the raw material diamine component beyond Long carbon chain diamines, Putriscine, 1,6- hexamethylene diamines, 1 can be exemplified,
8- octamethylenediamines, 2- methyl isophthalic acids, 5- pentanediamines, 2,2,4- trimethyl -1,6- hexamethylene diamines, 2,4,4- trimethyl -1,6- hexamethylene diamines,
2- methyl isophthalic acids, 8- octamethylenediamines, 5- methyl isophthalic acids, the aliphatic diamine such as 9- nonane diamines, 1,3- double (aminomethyl) hexamethylene, Isosorbide-5-Nitraes-bis-
The ester ring type diamines such as (aminomethyl) hexamethylene, cyclohexanediamine, methyl cyclohexane diamines, IPD, the virtue such as m-xylene diamine
Fragrant race's diamines or their mixture, but it is not limited to this.
Aromatic dicarboxylic acid and its derivative include but is not limited to terephthalic acid (TPA), M-phthalic acid.Preferably to benzene two
Formic acid.
As the raw material diacid beyond aromatic dicarboxylic acid, succinic acid, glutaric acid, adipic acid, heptan can be exemplified
Diacid, suberic acid, azelaic acid, decanedioic acid, DC11, SL-AH, tridecanyldicarboxylic acid, 14 carbon binary
Acid, 15 carbon dicarboxylic acids, 16-dicarboxylic acid, DC17, DC18 or their mixture, but not
It is defined in this.
When preparing nylon resin, in order to adjust the molecular weight of nylon resin or improve its hot water resistance, nylon resin
End-capping reagent can be further added in raw materials for production.End-capping reagent is monocarboxylic acid, monoamine, acid anhydrides, monoisocyanates, single acyl
Any one or a few combination in halogen, monoesters class and monohydric alcohol.Wherein, acid anhydrides includes but is not limited to phthalic acid
Acid anhydride.From the viewpoint of production stability, preferably monocarboxylic acid or monoamine is used as end-capping reagent.
As the monocarboxylic acid that can act as end-capping reagent, as long as there is the monocarboxylic acid of reactivity then without spy with amino
Do not limit.Monocarboxylic acid includes but is not limited to aliphatic monocarboxylic acid, alicyclic monocarboxylic acid and aromatic series monocarboxylic acid etc..Its
In, aliphatic monocarboxylic acid includes but is not limited to acetic acid, propionic acid, butyric acid, valeric acid, caproic acid, octanoic acid, laurate, tridecanoic acid, meat
Myristic acid, palmitic acid, stearic acid, trimethylace tonitric and isobutyric acid.Alicyclic monocarboxylic acid includes but is not limited to hexane formic acid.
Aromatic series monocarboxylic acid includes but is not limited to benzoic acid, toluic acid, α-naphthoicacid, β-naphthoic acid, methyl naphthoic acid and benzene
The aromatic series monocarboxylic acid such as guanidine-acetic acid.
As the monoamine that can act as end-capping reagent, as long as the monoamine for having reactivity with carboxyl is not limited especially then
System.Monoamine includes but is not limited to aliphatic mono, cycloaliphatic monoamines and aromatic monoamines etc..Wherein, aliphatic one
First amine includes but is not limited to methylamine, ethamine, propylamine, butylamine, hexylamine, octylame, decyl amine, stearylamine, dimethylamine, diethylamine, dipropyl
Amine and dibutyl amine.Cycloaliphatic monoamines include but is not limited to cyclohexylamine and dicyclohexyl amine.Aromatic monoamines include but is not limited to
Aniline, toluidines, diphenylamines and naphthylamines.
When preparing nylon resin, catalyst can also be added to improve reaction speed, such as compound containing phosphorus atoms, such as
Phosphoric acid, phosphorous acid, hypophosphorous acid etc., preferably phosphoric acid.
The semi-aromatic nylon manufacturing process of this method is as follows：
（1）Dissolution kettle：Semi-aromatic nylon salt and water are conveyed into dissolution kettle and mixed.Semi-aromatic nylon salt can be with often
Rule method is produced, and such as will carry out crystallization and purification after salt-forming reaction in diamines and aromatic diacid addition organic solvent such as ethanol obtains
Arrive.Semi-aromatic nylon salt can be added in the way of solid or slurry.Dissolution kettle is band stirring vertical response kettle, whipped form
It can be push type, anchor formula etc., outside carries chuck, and inside carries coil pipe, conduction oil or steam can be walked to provide reaction institute
The heat needed.Residence time of material 30-60 minutes, 160-180 DEG C of operation temperature.Concentration of salt solution is 30%-40%.
（2）Evaporator：Salting liquid after dissolving is pumped into evaporator further to be concentrated.Evaporator is that band stirring is vertical
Exhaust outlet is arranged at reactor, top, for discharging vapor, and whipped form can be push type, anchor formula etc., and outside carries chuck,
Inside carries coil pipe, can walk conduction oil to provide the heat needed for reaction.Residence time of material 30-60 minutes, operation temperature
200-230℃.Operating pressure 1.5-3.0MPa.The concentration of salt solution for leaving evaporator is 70%-80%.
（3）Reactor：Salting liquid after concentration enters reactor and carries out preliminary polymerization.Reactor is horizontal tubular reactor
Device, top has exhaust outlet to be used to discharge the pressure that vapor controls reactor, and there is chuck outside, and it is anti-to provide to walk conduction oil
Answer required heat.Reactor is equipped with liquid level gauge, the liquid level to control reactor.In reactor, salting liquid further steams
Shampoo point, while carrying out preliminary polymerization.230-260 DEG C of the operation temperature of reactor, operating pressure 3.0-5.0MPa, during stop
Between 1-2 hours.
（4）Flash vessel：The material that reactor comes out, which enters flash vessel, to be continued to react.Flash vessel is that a caliber constantly becomes big
Horizontal tubular reactor device.There is chuck outside.In flash vessel, with the flowing of material, pressure is gradually reduced, and temperature gradually rises
It is high.During Flow of Goods and Materials, material is separated with the water evaporated, forms two phase flow, has a gas-liquid point in flash vessel afterbody
From device, the operation temperature of gas-liquid separator is higher than 10-20 DEG C of the fusing point of semi-aromatic nylon, operating pressure 0.2-0.5MPa, to prevent
Only material solidifies.Enter polymerizer after having an atomizer, semi-aromatic nylon formation molten melt drop after gas-liquid separator.Material stops
Stay time 20-40 minute.
（5）Polymerizer：Semi-aromatic nylon melt liquid enters after polymerizer.It is cooled into solid particle, Ran Hou
Further viscosified at 230-260 DEG C.Polymerizer is vertical vessel, and operating pressure 0-1MPa, top is cooling section, and bottom is thickening
Section, similar to fixed bed reactors, there is hot nitrogen bottom toward blowing in container, and the moisture for reacting generation is taken away.There is chuck outside.
Residence time 5-24 hour of the material in polymerizer.
Beneficial effects of the present invention：Production efficiency of the present invention is high, and product quality is stable, it is easy to mass produce, production
Semi-aromatic nylon can be used in terms of automobile, electronic apparatus.
Brief description of the drawings
Fig. 1 is reaction structure schematic diagram of the present invention.
Description of reference numerals：1st, dissolution kettle；2nd, evaporator；3rd, reactor；4th, flash vessel；5th, polymerizer.
Embodiment
Relative viscosity
Accurate weighing 0.2g samples, stirring and dissolving is in the sulfuric acid of 25mL 96% at 20 ~ 30 DEG C.After being completely dissolved, solution is put into
In dark type viscometer, lowering time (t) is determined at 25 DEG C.Same method determines the lowering time (t0) of 96% sulfuric acid.Relatively
Viscosity can be obtained by following formula：
Relative viscosity=t/t0
The device of reaction is in series by dissolution kettle 1, evaporator 2, reactor 3, flash vessel 4, polymerizer 5.
Dissolution kettle 1 is vertical stirred autoclave, is stirred as push type, reactor volume 40L.Charging is arranged at reactor top
Mouth, exhaust outlet, bottom connection Melt Pump.Reactor carries admittance deep fat inside chuck, chuck, with the temperature needed for maintenance reaction
Degree.
Evaporator 2 is to carry vertical stirred autoclave, and charging aperture, exhaust are arranged at reactor volume 40L, reactor top
Mouthful, bottom connection Melt Pump.Reactor carries admittance deep fat inside chuck, chuck, with the temperature needed for maintenance reaction.
Reactor 3 is tubular reactor, and caliber 50mm, length 1m, top have exhaust outlet to be used for control pressure, with folder
Set, behind have Melt Pump.Reactor is equipped with radiation liquid level gauge to control liquid level.
Flash vessel 4 is tubular reactor, head caliber 50mm, afterbody caliber caliber 100mm, length 1m, jacketed.Flash distillation
Device afterbody is 20L gas-liquid separator, and jacketed, top is exhaust outlet, and bottom is discharging opening, connects Melt Pump and atomizer.
Polymerizer 5 is 1m3Vertical vessel, bottom leads to hot nitrogen, with chuck.
Embodiment 1
Paraphenylene terephthalamide's decamethylene diamine salt 10kg/hr, deionized water 15kg/hr are continuously added to dissolution kettle 1.The temperature 160 of dissolution kettle 1
℃.200 DEG C of 2 temperature of evaporator, pressure 1.5MPa.240 DEG C of 3 temperature of reactor, pressure 3.2MPa.The afterbody pressure of flash vessel 4
0.2MPa, 320 DEG C of temperature.The pressure 0.02MPa of polymerizer 5,240 DEG C of nitrogen temperature.From the bottom collection PA10T particles of polymerizer 5,
Relative viscosity 2.10.
Embodiment 2
The carbon diamine salts 10kg/hr of paraphenylene terephthalamide 12, deionized water 18kg/hr are continuously added to dissolution kettle 1.The temperature of dissolution kettle 1
170 DEG C of degree.205 DEG C of 2 temperature of evaporator, pressure 1.6MPa.250 DEG C of 3 temperature of reactor, pressure 4.0MPa.The afterbody pressure of flash vessel 4
Power 0.3MPa, 310 DEG C of temperature.The pressure 0.02MPa of polymerizer 5,250 DEG C of nitrogen temperature.From 5 bottom collection of polymerizer PA12T
Son, relative viscosity 2.20.
Embodiment 3
The carbon diamine salts 10kg/hr of paraphenylene terephthalamide 12, deionized water 20kg/hr are continuously added to dissolution kettle 1.The temperature of dissolution kettle 1
170 DEG C of degree.205 DEG C of 2 temperature of evaporator, pressure 1.6MPa.250 DEG C of 3 temperature of reactor, pressure 4.0MPa.The afterbody pressure of flash vessel 4
Power 0.3MPa, 310 DEG C of temperature.The pressure 0.02MPa of polymerizer 5,250 DEG C of nitrogen temperature.From 5 bottom collection of polymerizer PA12T
Son, relative viscosity 2.20.
The above-mentioned description to embodiment is that this hair is understood that and used for ease of those skilled in the art
It is bright.Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein
General Principle is applied in other embodiment without passing through performing creative labour.Therefore, the invention is not restricted to above-mentioned implementation
Example, those skilled in the art do not depart from improvement that scope made and change all should be according to the announcement of the present invention
Within protection scope of the present invention.
Claims (6)
1. a kind of method of continuous production semi-aromatic nylon, it is characterized in that step is as follows：
（1）Dissolution kettle：Semi-aromatic nylon salt and water are conveyed into dissolution kettle（1）It is interior to be mixed so that gained salting liquid matter
Amount concentration is 30%-40%；Wherein dissolution kettle is the vertical response kettle with stirring, and outside is provided with chuck, and inside is provided with coil pipe；Material
Residence time 30-60min, operation temperature is 160-180 DEG C；
（2）Evaporator：Step（1）Gained salting liquid is conveyed into evaporator（2）In be evaporated, residence time of material is 30-
60min, operation temperature is 200-230 DEG C, and operating pressure is 1.5-3.0MPa；The evaporator is band stirring vertical response kettle,
Exhaust outlet is arranged at top, for discharging vapor, and outside carries chuck, and inside carries coil pipe；
（3）Reactor：Step（2）Resulting material is conveyed into reactor（3）, preliminary polymerization is carried out in reactor, reactor
230-260 DEG C of operation temperature, operating pressure is 3.0-5.0MPa, and the residence time is 1-2 hours；The reactor is horizontal pipe
Reactor, top has exhaust outlet to be used to discharge the pressure that vapor controls reactor, and there is chuck outside, and inside is provided with liquid level gauge,
Liquid level to control reactor；
（4）Flash vessel：Step（3）Resulting material is conveyed into flash vessel（4）, in flash vessel, with the flowing of material, pressure by
Gradually reduce, temperature gradually rises；Flash vessel afterbody connects gas-liquid separator, and the operation temperature of gas-liquid separator is molten higher than material
10-20 DEG C of point, operating pressure 0.2-0.5MPa；Gas-liquid separator is connected with atomizer, and material forms fused solution in atomizer
Drop, atomizer operating temperature is 1.0-5.0MPa higher than 20-30 DEG C of material fusing point, operating pressure;
（5）Polymerizer：Step（4）Resulting material is conveyed into polymerizer（5）, top is cooling section, and bottom is thickening section, and bottom leads to
Enter and chuck is provided with outside 200-260 DEG C of nitrogen, polymerizer, polymerization temperature is 230-260 DEG C, and polymerization pressure is 0-1MPa, instead
It is 5-24h between seasonable, produces semi-aromatic nylon.
2. the method for continuous production semi-aromatic nylon as claimed in claim 1, it is characterized in that：The semi-aromatic nylon salt
By raw material diamines of effective functional group mole accounting more than 70% of Long carbon chain diamines and the effective functional group mole of aromatic dicarboxylic acid
Raw material dicarboxyl acid reaction of the accounting more than 70% is formed.
3. the method for continuous production semi-aromatic nylon as claimed in claim 1, it is characterized in that：The Long carbon chain diamine tool
Body be decamethylene diamine, 11 carbon diamines, 12 carbon diamines, 13 carbon diamines, 14 carbon diamines, 15 carbon diamines,
16 carbon diamines, 17 carbon diamines, preferably DC18, decamethylene diamine；
Raw material diamine component beyond Long carbon chain diamines, specially Putriscine, 1,6- hexamethylene diamines, 1,8- octamethylenediamines, 2- first
Base -1,5- pentanediamines, 2,2,4- trimethyl -1,6- hexamethylene diamines, 2,4,4- trimethyl -1,6- hexamethylene diamines, 2- methyl isophthalic acids, 8- are pungent
Diamines, 5- methyl isophthalic acids, the aliphatic diamine such as 9- nonane diamines, 1,3- double (aminomethyl) hexamethylene, Isosorbide-5-Nitrae-bis- (aminomethyl) hexamethylenes
The ester ring type diamines such as alkane, cyclohexanediamine, methyl cyclohexane diamines, IPD, the aromatic diamine such as m-xylene diamine or it
Mixture.
4. the method for continuous production semi-aromatic nylon as claimed in claim 1, it is characterized in that：The aromatic dicarboxylic acid is
Terephthalic acid (TPA) and/or M-phthalic acid and its derivative；
Raw material diacid beyond the aromatic dicarboxylic acid, can exemplify succinic acid, glutaric acid, adipic acid, pimelic acid,
Suberic acid, azelaic acid, decanedioic acid, DC11, SL-AH, tridecanyldicarboxylic acid, DC14,15
Carbon dicarboxylic acid, 16-dicarboxylic acid, DC17, DC18 or their mixture.
5. the method for continuous production semi-aromatic nylon as claimed in claim 1, it is characterized in that：Also include envelope in reaction raw materials
Hold agent, end-capping reagent is any in monocarboxylic acid, monoamine, acid anhydrides, monoisocyanates, single carboxylic acid halides, monoesters class and monohydric alcohol
One or more of combinations；Addition semi-aromatic nylon salt：End-capping reagent mass ratio is 100：0.05-0.5.
6. the method for continuous production semi-aromatic nylon as claimed in claim 1, it is characterized in that：Also include urging in reaction raw materials
Compound of the agent containing phosphorus atoms；Semi-aromatic nylon salt：Catalyst quality ratio is 100:0.01-0.05.
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| CN201710675222.7A CN107325279A (en) | 2017-08-09 | 2017-08-09 | A kind of method of continuous production semi-aromatic nylon |
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| CN201710675222.7A CN107325279A (en) | 2017-08-09 | 2017-08-09 | A kind of method of continuous production semi-aromatic nylon |
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Cited By (5)
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| CN108559075A (en) * | 2018-04-08 | 2018-09-21 | 金发科技股份有限公司 | A kind of Semi-aromatic polyamide resin and preparation method thereof and the polyamide moulding composition being made from it |
| CN108586733A (en) * | 2018-04-08 | 2018-09-28 | 金发科技股份有限公司 | A kind of Semi-aromatic polyamide resin and the polyamide moulding composition being made from it |
| WO2021129045A1 (en) * | 2019-12-24 | 2021-07-01 | 浙江新和成特种材料有限公司 | Semi-aromatic polyamide thermoplastic elastomer and continuous production method therefor |
| WO2021217997A1 (en) * | 2020-04-27 | 2021-11-04 | 扬州惠通化工科技股份有限公司 | High-capacity nylon polymerization system |
| WO2023036265A1 (en) * | 2021-09-13 | 2023-03-16 | 成都肆零壹科技有限公司 | Semi-aromatic nylon continuous polymerization process |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108559075A (en) * | 2018-04-08 | 2018-09-21 | 金发科技股份有限公司 | A kind of Semi-aromatic polyamide resin and preparation method thereof and the polyamide moulding composition being made from it |
| CN108586733A (en) * | 2018-04-08 | 2018-09-28 | 金发科技股份有限公司 | A kind of Semi-aromatic polyamide resin and the polyamide moulding composition being made from it |
| WO2021129045A1 (en) * | 2019-12-24 | 2021-07-01 | 浙江新和成特种材料有限公司 | Semi-aromatic polyamide thermoplastic elastomer and continuous production method therefor |
| WO2021217997A1 (en) * | 2020-04-27 | 2021-11-04 | 扬州惠通化工科技股份有限公司 | High-capacity nylon polymerization system |
| WO2023036265A1 (en) * | 2021-09-13 | 2023-03-16 | 成都肆零壹科技有限公司 | Semi-aromatic nylon continuous polymerization process |
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