CN103910878B - A kind of lysine synthesis semi-aromatic nylon and preparation method thereof - Google Patents
A kind of lysine synthesis semi-aromatic nylon and preparation method thereof Download PDFInfo
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- CN103910878B CN103910878B CN201310007272.XA CN201310007272A CN103910878B CN 103910878 B CN103910878 B CN 103910878B CN 201310007272 A CN201310007272 A CN 201310007272A CN 103910878 B CN103910878 B CN 103910878B
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Abstract
The present invention relates to high polymer material nylon to synthesize field, is related to a kind of method for synthesizing semi-aromatic nylon.The semi-aromatic nylon, it is made up of the component comprising following molal quantity：The 15.05mol of aromatic acid 10.65；The 14.60mol of aliphatic diamine 10.55；The 4.90mol of lysine 1.49；The 0.03mol of catalyst 0.015；The 300mol of solvent 220.The reactions steps of the present invention are simple, and the equipment cost for reacting used is cheap, and simultaneous reactions condition is more gently without HTHP, therefore the requirement to equipment is not very high, and its energy consumption is also smaller.The melt index of the semi-aromatic nylon of synthesis is higher, and mobility is preferable, and discharging is convenient, and granulation can be directly drawn through cooling, is easy to encapsulation transport and storage, processing and forming is can be directly used for after drying, dimensionally stable product is without cumbersome last handling process.Meanwhile its mechanical property is also ideal.
Description
Technical field
The invention belongs to high polymer material nylon to synthesize field, is related to a kind of semi-aromatic nylon and preparation method thereof.
Technical background
Nylon（Polyamide）It is a kind of current domestic and international application most widely thermoplastic engineering plastic, it has tough resistance to
The excellent specific property such as mill, impact resistance, endurance, corrosion-resistant, oil resistant, is widely used in auto-parts, electronic apparatus, machinery etc.
Industry, over 60 years, the steady-state growth in the keen competition of engineering plastics, its demand occupy five large-engineering plastics always so far
First place.
Semi-aromatic nylon is with aromatic diacid or diamines, being made through polycondensation by aliphatic diamine or diacid.
Due to importing aliphatic chain in fully aromatic polyamide molecular backbone, so as to improve molding processibility and dissolubility etc..With fat
Fat race nylon is compared, and semi-aromatic nylon maximum feature is fine heat-resisting performance, glass transition temperature generally 100 DEG C with
On, fusing point is generally more than 250 DEG C, mostly all near 300 DEG C.Heat aging property is excellent, mechanical property to temperature according to
Lai Xing little, stable performance can be kept within the scope of wider temperature.Water absorption rate is low, and after moisture absorption product size and mechanics
Performance change is small.The chemicals such as organic solvent-resistant and various vehicle fuels, oil plant, anti-icing fluid are good, and some have good
Barrier properties for gases.Electrical insulation capability is excellent, also outstanding arc resistance agent tracking.Shrinkage, morphotropism, creep properties
Very little, rigidity and intensity are generally better than in general amorphous nylon.
Found through the literature search to prior art, Chinese patent 200910227658.5 discloses a kind of semi-aromatic Buddhist nun
The preparation method of dragon, but the technological reaction time is longer, and technique is relatively complicated（Synthetic nylon salt is first obtained, then arrives reactor again
It is polymerize）, and solvent for use is alcohols or ketone solution, dangerous environmental protection.Chinese patent 200580023100.5 is related to
The defects of by lysine synthesis of caprolactam, solvent for use is alcohol solution, equally there is dangerous environmental protection, and reactions steps are cumbersome.
The content of the invention
It is an object of the invention to provide a kind of semi-aromatic nylon and preparation method thereof in view of the shortcomings of the prior art.
The semi-aromatic nylon is particular plastics, and performance is ideal, is adapted to industrialized production.
The method of synthesis semi-aromatic nylon provided by the invention, is gathered in polymeric kettle again in the absence of first synthetic nylon salt
The cumbersome technique such as close, but raw material added reactor and directly polymerize, therefore its synthesis technique is simple, generated time compared with
It is short；In addition, the present invention can use deionized water as solvent, therefore safer environmental protection, while also save many costs.
To achieve the above object, the present invention uses following technical scheme：
A kind of semi-aromatic nylon, it is made up of the component comprising following molal quantity：
Aromatic acid 10.65-15.05mol；
Aliphatic diamine 10.55-14.60mol；
Lysine 1.49-4.90mol；
Catalyst 0.015-0.03mol；
Solvent 220-300mol；
Described aromatic acid is selected from terephthalic acid (TPA), M-phthalic acid, phthalic acid, 4,4'- biphenyl diformazans
One or more in acid or naphthalenedicarboxylic acid, preferably terephthalic acid (TPA)；
Described aliphatic diamine is one in the aliphatic diamine containing 4-13 carbon atom in strand main chain
Kind or more than one, preferred decamethylene diamine；
Described catalyst be ortho phosphorous acid potassium, sodium phosphite, phosphorous acid magnesium, Arizona bacilli, zinc phosphite, potassium phosphate,
Magnesium phosphate, calcium phosphate, trbasic zinc phosphate, ortho phosphorous acid potassium, sodium hypophosphite, ortho phosphorous acid magnesium, Lime Hypophosphate or ortho phosphorous acid zinc
In one or more, preferred sodium hypophosphite；
Described solvent is deionized water, organic alcohol solvent, organic ketone solvent, and wherein Organic Alcohol is selected from methanol or ethanol；
Organic ketone solvent is selected from acetone, the preferred deionized water of the present invention.
A kind of method of above-mentioned lysine synthesis semi-aromatic nylon, comprises the following steps：
（1）Aromatic acid 10-15mol, aliphatic diamine 10-14mol are weighed according to above-mentioned molal quantity proportioning, are relied
Propylhomoserin 1.0-5.0mol, catalyst 0.015-0.03mol and solvent 220-300mol；
Aromatic acid, aliphatic diamine, lysine and catalyst are well mixed, has been then added into and has stirred
In the polymerization reaction kettle for mixing device, solvent is added, above-mentioned reactant mixture is stirred and inert gas is filled with into reactor, is taken out very
It is empty to exclude to be reserved in the air in reactor；
（2）Heating response kettle is simultaneously incubated, and 120 DEG C -130 DEG C of heat-preserving range, polymerized monomer is dissolved completely in solvent；
Insulation terminates, and reactor is continued to heat up, and the temperature range of heating is 130 DEG C -335 DEG C, now reactor internal pressure
Power rises, until when pressure reaches 2.5MPa in kettle, carries out pressurize to reactor, and reactor is continued to be heated to 260-270
DEG C when, agitator speed is doubled（Agitator speed rises to 120r/min）, pass through circulating heat conduction oil（Equivalent to flowing oil bath）
Continue to raise temperature of reaction kettle to 315-320 DEG C, reactor is carried out under the precondition for keeping temperature of reaction kettle not decline
Release；
Until the pressure in reactor is unloaded to normal pressure, agitator speed is reduced（Agitator speed be down to 12r/min with
Under）, inert gas is filled with to reactor to the pressure in the range of 0.3-1.2MPa in reactor, discharging, cooling and dicing, to obtain
With semi-aromatic nylon pellet.
Described step（1）In power of agitator be 60r/min.
Described step（1）Or step（2）Middle inert gas is nitrogen, carbon dioxide, argon gas or helium, preferably nitrogen.
Described step（2）In, the temperature of heating response is 120-130 DEG C,
Described step（2）Middle semi-aromatic nylon material dries 24h in 110 DEG C of -135 DEG C of baking ovens, then on injection machine
Injection molding, injection silicon carbide is 290 DEG C, 295 DEG C, 295 DEG C, obtains being used for correlated performance testing standard nylon batten.
Described step（2）In, before discharging, the size of material viscosity in kettle is determined according to the watt level of stirring display,
Further determine whether to carry out vacuumizing thickening step：When power of agitator is less than 1100w, vacuumize process；Work as power of agitator
For 1100w-1250w when, without vacuumizing.
The method of synthesis semi-aromatic nylon provided by the invention, is gathered in polymeric kettle again in the absence of first synthetic nylon salt
The cumbersome technique such as close, but raw material added reactor and directly polymerize, therefore its synthesis technique is simple, generated time compared with
It is short；In addition, the present invention can use deionized water as solvent, therefore safer environmental protection, while also save many costs.
The present invention compared with the existing technology, has advantages below：
（1）Reactions steps are simple, and the equipment cost for reacting used is cheap, and simultaneous reactions condition is more gently without high temperature height
Pressure, therefore the requirement to equipment is not very high, and its energy consumption is also smaller.
（2）Solvent used is deionized water, and without toxicity, wide material sources are green, for mitigating environmental pressure,
It is extremely important in terms of environmental protection.
（3）The melt index of the semi-aromatic nylon of synthesis is higher, and mobility is preferable, and discharging is convenient, can be direct through cooling
Traction is granulated, and is easy to encapsulation to transport and storage, be can be directly used for processing and forming after drying, and dimensionally stable product is without after cumbersome
Processing procedure.Meanwhile its mechanical property is also ideal.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.These embodiments are merely to illustrate the present invention, and do not have to
In restriction protection scope of the present invention.The modifications and adaptations that technical staff makes according to the present invention in actual applications, still fall within
Protection scope of the present invention.
Below in an example, using following detection method：
The melt index of nylon presses GB/T3682-2000, at 300 DEG C, is tested under the conditions of 2.16kg.
Tensile property is tested by GB/T1040.1-20O6, rate of extension 5mm/min, is surveyed under constant temperature and humidity experiment condition
Examination.
Simply supported beam notch impact strength is tested by GB/T1043, is tested under constant temperature and humidity experiment condition.
Bending strength GB/T9341-2008 is tested, and is pushed speed 1.25mm/min, is surveyed under constant temperature and humidity experiment condition
Examination.
Embodiment 1
Terephthalic acid (TPA) is weighed in proportion（Purity 100%）2460.8118g（It is roughly equal to 14.8126mol）, decamethylene diamine（Purity
99%）2320.4560g（It is roughly equal to 13.3313mol）, lysine（Purity 99%）217.9631g（It is roughly equal to 1.4813mol）, secondary phosphorous
Sour sodium 1.2894g（It is roughly equal to 0.015mol）, it is well mixed and is poured into 25L reactors, injects 3.96kg deionized waters（About
Close 220mol）In reactor.It is 60r/min to open agitating device rotating speed, is filled with nitrogen and is vacuumized, is repeated 3 times, and is excluded
The air being reserved in kettle；
Insulation terminates, and reactor is continued to heat up, and reactor temperature is risen to 120 DEG C by circulating heat conduction oil and is incubated
2 hours, polymerized monomer is set to be dissolved completely in solvent, insulation end continues to raise reactor temperature to 235 DEG C, now reacts
Pressure increases to 2.5MPa in kettle, pressurize is carried out to reactor, and side pressurize edge height temperature of reaction kettle is until temperature reaches 260 DEG C
When, speed of agitator is increased to 120r/min, continues to raise temperature of reaction kettle until temperature is 315 DEG C, holding temperature of reaction kettle is not
Under the premise of decline, release is carried out until pressure is unloaded to normal pressure, now power of agitator is 1189w, without vacuumizing.Stirring is reduced to turn
For speed to 12r/min, being filled with nitrogen makes reacting kettle inner pressure be 0.3MPa, discharging, can directly be cut after obtaining continuity preferably cooling
The semi-aromatic nylon material of grain.
Embodiment 2
Terephthalic acid (TPA) is weighed in proportion（Purity 100%）2499.9065g（It is roughly equal to 15.0479mol）, decamethylene diamine（Purity
99%）1833.4718g（It is roughly equal to 10.5335mol）, lysine（Purity 99%）666.6216g（It is roughly equal to 4.5144mol）, secondary phosphorous
Sour sodium 2.0g（It is roughly equal to 0.02326mol）, it is well mixed and is poured into 25L reactors, injects 4.3kg deionized waters（It is roughly equal to
238.89mol）In reactor.It is 60r/min to open agitating device rotating speed, is filled with nitrogen and is vacuumized, is repeated 3 times, and is arranged
Except the air being reserved in kettle；
Insulation terminates, and reactor is continued to heat up, and reactor temperature is risen to 122 DEG C by circulating heat conduction oil and is incubated
2 hours, polymerized monomer is set to be dissolved completely in solvent；Insulation end continues to raise reactor temperature to 237 DEG C, now reacts
Pressure increases to 2.5MPa in kettle, pressurize is carried out to reactor, and side pressurize edge height temperature of reaction kettle is until temperature reaches 262 DEG C
When, speed of agitator is increased to 120r/min, continues to raise temperature of reaction kettle until temperature is 315 DEG C, holding temperature of reaction kettle is not
Under the premise of decline, release is carried out until pressure is unloaded to normal pressure, now power of agitator is 1212w, without vacuumizing.Stirring is reduced to turn
For speed to 12r/min, being filled with nitrogen makes reacting kettle inner pressure be 0.5MPa, discharging, can directly be cut after obtaining continuity preferably cooling
The semi-aromatic nylon material of grain.
Embodiment 3
Terephthalic acid (TPA) 2429.1803g is weighed in proportion（It is roughly equal to 14.6222mol）, decamethylene diamine 2349.3627g（It is roughly equal to
13.4974mol）, lysine 221.4571g（It is roughly equal to 1.4997mol）, catalyst sodium hypophosphite 2.2g（It is roughly equal to
0.02559mol）, it is well mixed and is poured into 25L reactors, injects 4.5kg deionized waters（It is roughly equal to 250mol）In reaction
In kettle.It is 60r/min to open agitating device rotating speed, is filled with nitrogen and is vacuumized, is repeated 3 times, and excludes the sky being reserved in kettle
Gas；
Insulation terminates, and reactor is continued to heat up, and reactor temperature is risen to 125 DEG C by circulating heat conduction oil and is incubated
2 hours, polymerized monomer is set to be dissolved completely in solvent, insulation end continues to raise reactor temperature to 237 DEG C, now reacts
Pressure increases to 2.5MPa in kettle, pressurize is carried out to reactor, and side pressurize edge height temperature of reaction kettle is until temperature reaches 265 DEG C
When, speed of agitator is increased to 120r/min, continues to raise temperature of reaction kettle until temperature is 315 DEG C, holding temperature of reaction kettle is not
Under the premise of decline, release is carried out until pressure is unloaded to normal pressure, now power of agitator is 1021w, and vacuumize process extremely stirs for 5 minutes
Power is 1160w.Speed of agitator is reduced to 12r/min, being filled with nitrogen makes reacting kettle inner pressure be 0.9MPa, discharging, is connected
After the preferably cooling of continuous property can direct pelletizing semi-aromatic nylon material.
Embodiment 4
Terephthalic acid (TPA) 1766.2614g is weighed in proportion（It is roughly equal to 10.6318mol）, decamethylene diamine 2535.9773g（It is roughly equal to
14.5695mol）, lysine 697.7613g（It is roughly equal to 4.7252mol）, sodium hypophosphite 2.4g（It is roughly equal to 0.02792mol）, mix
Close uniformly and be poured into 25L reactors, inject 4.8kg（It is roughly equal to 266.66mol）Deionized water is in reactor.Unlatching is stirred
It is 60r/min to mix device rotary speed, is filled with nitrogen and is vacuumized, is repeated 3 times, and excludes the air being reserved in kettle；
Insulation terminates, and reactor is continued to heat up, and reactor temperature is risen to 125 DEG C by circulating heat conduction oil and is incubated
2 hours, polymerized monomer is set to be dissolved completely in solvent, insulation end continues to raise reactor temperature to 234 DEG C, now reacts
Pressure increases to 2.5MPa in kettle, pressurize is carried out to reactor, and side pressurize edge height temperature of reaction kettle is until temperature reaches 265 DEG C
When, speed of agitator is increased to 120r/min, continues to raise temperature of reaction kettle until temperature is 315 DEG C, holding temperature of reaction kettle is not
Under the premise of decline, release is carried out until pressure is unloaded to normal pressure, now power of agitator is 1141w, without vacuumizing.Stirring is reduced to turn
For speed to 12r/min, being filled with nitrogen makes reacting kettle inner pressure be 0.7MPa, discharging, can directly be cut after obtaining continuity preferably cooling
The semi-aromatic nylon material of grain.
Embodiment 5
Terephthalic acid (TPA) 2396.7507g is weighed in proportion（It is roughly equal to 14.4270mol）, decamethylene diamine 2378.9987g（It is roughly equal to
13.6676mol）, lysine 224.2506g（It is roughly equal to 1.5186mol）, sodium hypophosphite 2.5g（It is roughly equal to 0.02908mol）, mix
Close uniformly and be poured into 25L reactors, inject 5.0kg（It is roughly equal to 277.77mol）Deionized water is in reactor.Unlatching is stirred
It is 60r/min to mix device rotary speed, is filled with nitrogen and is vacuumized, is repeated 3 times, and excludes the air being reserved in kettle；
Insulation terminates, and reactor is continued to heat up, and reactor temperature is risen to 125 DEG C by circulating heat conduction oil and is incubated
2 hours, polymerized monomer is set to be dissolved completely in solvent, insulation end continues to raise reactor temperature to 236 DEG C, now reacts
Pressure increases to 2.5MPa in kettle, pressurize is carried out to reactor, and side pressurize edge height temperature of reaction kettle is until temperature reaches 265 DEG C
When, speed of agitator is increased to 120r/min, continues to raise temperature of reaction kettle until temperature is 315 DEG C, holding temperature of reaction kettle is not
Under the premise of decline, release is carried out until pressure is unloaded to normal pressure, now power of agitator is 1201w, without vacuumizing.Stirring is reduced to turn
For speed to 12r/min, being filled with nitrogen makes reacting kettle inner pressure be 1.0MPa, discharging, can directly be cut after obtaining continuity preferably cooling
The semi-aromatic nylon material of grain.
Embodiment 6
Terephthalic acid (TPA) 2297.2044g is weighed in proportion（It is roughly equal to 13.8277mol）, decamethylene diamine 1982.1257g（It is roughly equal to
11.3875mol）, lysine 720.6699g（It is roughly equal to 4.8804mol）, sodium hypophosphite 2.5788g（It is roughly equal to 0.03mol）, mix
Close uniformly and be poured into 25L reactors, inject 5.4kg（It is roughly equal to 300mol）Deionized water is in reactor.Open stirring
Device rotary speed is 60r/min, is filled with nitrogen and is vacuumized, is repeated 3 times, and excludes the air being reserved in kettle；
Insulation terminates, and reactor is continued to heat up, and reactor temperature is risen to 130 DEG C by circulating heat conduction oil and is incubated
2 hours, polymerized monomer is set to be dissolved completely in solvent, insulation end continues to raise reactor temperature to 239 DEG C, now instead
Answer pressure in kettle to increase to 2.5MPa, pressurize is carried out to reactor, and side pressurize edge height temperature of reaction kettle is until temperature reaches 270
DEG C when, increase speed of agitator to 120r/min, continue to raise temperature of reaction kettle until temperature is 320 DEG C, keep temperature of reaction kettle
Under the premise of not declining, release is carried out until pressure is unloaded to normal pressure, and now power of agitator is 980w, and vacuumize process 11 minutes is to stirring
It is 1145w to mix power.Speed of agitator is reduced to 12r/min, being filled with nitrogen makes reacting kettle inner pressure be 1.2MPa, discharging, obtains
After continuity preferably cooling can direct pelletizing semi-aromatic nylon material.
Embodiment 1-6 the performance test results such as table 1.
Table 1
| Melt index（g/10min） | Tensile strength（MPa） | Impact strength（KJ/m2） | Bending strength（MPa） | |
| Embodiment 1 | 172.3 | 54.87 | 8.35 | 120.30 |
| Embodiment 2 | 174.5 | 50.90 | 7.81 | 118.28 |
| Embodiment 3 | 172.2 | 48.79 | 8.48 | 111.09 |
| Embodiment 4 | 172.8 | 56.86 | 7.79 | 114.30 |
| Embodiment 5 | 177.3 | 60.04 | 8.75 | 119.94 |
| Embodiment 6 | 173.6 | 49.98 | 7.17 | 122.86 |
Pass through the implementation process and the performance test results of the various embodiments described above, it is known that can be facilitated by preparation method of the present invention
Aliphatic diamine and the molar ratio of aromatic acid and lysine are adjusted, so as to be to obtain required good mechanical performance
A kind of semi-aromatic nylon provide an extremely easy method, and directly synthesized after the completion of present invention charging, technique
Simple and easy while used solvent is deionized water, without toxicity, safety and environmental protection.
The above-mentioned description to embodiment is understood that for ease of those skilled in the art and using this hair
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 by performing creative labour.Therefore, the invention is not restricted to implementation here
Example, for those skilled in the art according to the announcement of the present invention, not departing from improvement that scope made and modification all should be
Within protection scope of the present invention.
Claims (16)
- A kind of 1. semi-aromatic nylon, it is characterised in that：It is made up of the component comprising following molal quantity：The method for synthesizing above-mentioned semi-aromatic nylon, comprises the following steps：(1) each component material of following parts by weight is weighed：Aromatic acid 10.65-15.05mol, aliphatic diamine 10.55-14.60mol, lysine 1.49-4.90mol, catalyst 0.015-0.03mol and solvent 220-300mol；Aromatic acid, aliphatic diamine, lysine and catalyst are well mixed, have been then added into stirring dress In the polymerization reaction kettle put, add solvent, stir above-mentioned reactant mixture and be filled with into reactor inert gas, vacuumize with Exclude the air being reserved in reactor；(2) heating response kettle to 120 DEG C -130 DEG C and is incubated, and polymerized monomer is dissolved completely in solvent；Insulation terminates, to anti- Kettle is answered to continue to heat up, the temperature range of heating is 130 DEG C -335 DEG C, and now reacting kettle inner pressure rises, until pressure reaches in kettle During to 2.5MPa, when carrying out pressurize to reactor, and continuing to be heated to 260-270 DEG C to reactor, agitating device rotating speed liter To 120r/min, continue to raise temperature of reaction kettle to 315-320 DEG C by circulating heat conduction oil, do not decline keeping temperature of reaction kettle Precondition under to reactor carry out release；Until the pressure in reactor is unloaded to normal pressure, agitating device rotating speed is reduced to below 12r/min, is filled with to reactor lazy Property gas so as to the pressure in the range of 0.3-1.2MPa in reactor, discharging, obtains semi-aromatic nylon pellet at cooling and dicing；In described step (2), before discharging, when power of agitator is less than 1100w, vacuumize process is carried out.
- 2. semi-aromatic nylon according to claim 1, it is characterised in that：Described aromatic acid is selected to benzene two One or more in formic acid, M-phthalic acid, phthalic acid, 4,4'- biphenyl dicarboxylic acids or naphthalenedicarboxylic acid.
- 3. semi-aromatic nylon according to claim 2, it is characterised in that：Described aromatic acid is terephthaldehyde Acid.
- 4. semi-aromatic nylon according to claim 1, it is characterised in that：Described aliphatic diamine is strand master The one or more in aliphatic diamine containing 4-13 carbon atom in chain.
- 5. semi-aromatic nylon according to claim 4, it is characterised in that：Described aliphatic diamine is decamethylene diamine.
- 6. semi-aromatic nylon according to claim 1, it is characterised in that：Described catalyst is ortho phosphorous acid potassium, Asia Sodium phosphate, phosphorous acid magnesium, Arizona bacilli, zinc phosphite, potassium phosphate, magnesium phosphate, calcium phosphate, trbasic zinc phosphate, sodium hypophosphite, secondary Asia One or more in magnesium phosphate, Lime Hypophosphate or ortho phosphorous acid zinc.
- 7. semi-aromatic nylon according to claim 6, it is characterised in that：Described catalyst is sodium hypophosphite.
- 8. semi-aromatic nylon according to claim 1, it is characterised in that：Described solvent is deionized water, Organic Alcohol Solvent, organic ketone solvent.
- 9. semi-aromatic nylon according to claim 8, it is characterised in that：Described solvent is deionized water.
- 10. semi-aromatic nylon according to claim 8, it is characterised in that：Described Organic Alcohol is selected from methanol or ethanol.
- 11. semi-aromatic nylon according to claim 8, it is characterised in that：The organic ketone solvent is selected from acetone.
- 12. a kind of method of any described synthesis semi-aromatic nylon in the claims 1-11, it is characterised in that：Including Following steps：(1) each component material of following parts by weight is weighed according to the molal quantity proportioning described in claim 1：Aromatic acid 10.65-15.05mol, aliphatic diamine 10.55-14.60mol, lysine 1.49-4.90mol, catalyst 0.015- 0.03mol and solvent 220-300mol；Aromatic acid, aliphatic diamine, lysine and catalyst are well mixed, have been then added into stirring dress In the polymerization reaction kettle put, add solvent, stir above-mentioned reactant mixture and be filled with into reactor inert gas, vacuumize with Exclude the air being reserved in reactor；(2) heating response kettle to 120 DEG C -130 DEG C and is incubated, and polymerized monomer is dissolved completely in solvent；Insulation terminates, to anti- Kettle is answered to continue to heat up, the temperature range of heating is 130 DEG C -335 DEG C, and now reacting kettle inner pressure rises, until pressure reaches in kettle During to 2.5MPa, when carrying out pressurize to reactor, and continuing to be heated to 260-270 DEG C to reactor, agitating device rotating speed liter To 120r/min, continue to raise temperature of reaction kettle to 315-320 DEG C by circulating heat conduction oil, do not decline keeping temperature of reaction kettle Precondition under to reactor carry out release；Until the pressure in reactor is unloaded to normal pressure, agitating device rotating speed is reduced to below 12r/min, is filled with to reactor lazy Property gas so as to the pressure in the range of 0.3-1.2MPa in reactor, discharging, obtains semi-aromatic nylon pellet at cooling and dicing.
- 13. the method for synthesis semi-aromatic nylon according to claim 12, it is characterised in that：In described step (1) Agitating device rotating speed be 60r/min.
- 14. the method for synthesis semi-aromatic nylon according to claim 12, it is characterised in that：Described step (1) or Inert gas is nitrogen, carbon dioxide, argon gas or helium in step (2).
- 15. the method for synthesis semi-aromatic nylon according to claim 14, it is characterised in that：Described step (1) or Inert gas is nitrogen in step (2).
- 16. the method for synthesis semi-aromatic nylon according to claim 12, it is characterised in that：In described step (2) Semi-aromatic nylon pellet dries 24h in 110 DEG C of -135 DEG C of baking ovens, the then injection molding on injection machine, is molded silicon carbide For 290 DEG C, 295 DEG C, 295 DEG C, obtain being used for correlated performance testing standard nylon batten.
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| CN104817693B (en) * | 2015-05-21 | 2017-05-24 | 郑州大学 | Semi-aromatic polyamide PA11T and preparation method thereof |
| CN106916298A (en) * | 2015-12-25 | 2017-07-04 | 上海杰事杰新材料(集团)股份有限公司 | A kind of environment friendly biological base semi-aromatic PA10T/11 copolymeric materials and preparation method thereof |
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| EP1266930B1 (en) * | 2001-06-05 | 2006-12-20 | Kuraray Co., Ltd. | Polyamide composition |
| FR2858626B1 (en) * | 2003-08-05 | 2005-10-07 | Atofina | SOFT SEMI AROMATIC POLYAMIDES WITH LOW HUMIDITY RESUME |
| EP2325260B1 (en) * | 2009-11-23 | 2016-04-27 | Ems-Patent Ag | Semi-aromatic moulding masses and their applications |
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Denomination of invention: Lysine-synthesized semi-aromatic nylon and its synthesizing method Effective date of registration: 20191223 Granted publication date: 20180102 Pledgee: Chuzhou economic and Technological Development Corporation Pledgor: Shanghai Jieshijie New Materials (Group) Co., Ltd. Registration number: Y2019980001220 |
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