CN106589351A - Semi-aromatic transparent nylon material PA6I and preparing method thereof - Google Patents
Semi-aromatic transparent nylon material PA6I and preparing method thereof Download PDFInfo
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- CN106589351A CN106589351A CN201510660451.2A CN201510660451A CN106589351A CN 106589351 A CN106589351 A CN 106589351A CN 201510660451 A CN201510660451 A CN 201510660451A CN 106589351 A CN106589351 A CN 106589351A
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- 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
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Abstract
The invention provides a semi-aromatic transparent nylon material PA6I and a preparing method thereof. PA6I is prepared from 58-60 parts of isophthalic acid, 40-42 parts of hexanediamine and 0.0002-0.0007 parts of catalyst. The preparing method comprises the steps of mixing the raw materials in the ratio and adding the raw materials into a high-pressure reaction kettle, and adding 40-80 parts of deionized water; using inert gases to replace air in the high-pressure reaction kettle, and preserving 0.05-1.0MPa inert gases; heating the high-pressure reaction kettle, when the temperature of the high-pressure reaction kettle reaches 100-150 DEG C, keeping the temperature for 1.0-3.0 hours, keeping the temperature for 1.0-3.0 hours when the temperature reaches 200-230 DEG c, continuing increasing the temperature, when the pressure of high-pressure reaction kettle reaches 2.3-2.70MPa, keeping the pressure constant for 1.0-2.0 hours, and continuing heating the high-pressure reaction kettle when the pressure is constant; unloading the pressure when the temperature of the high-pressure reaction kettle reaches 275-290MPa, and keeping the temperature at 255-275 DEG C when unloading the temperature; when the pressure of the high-pressure reaction kettle reaches normal pressure, continuing stirring at the velocity of 7-12 rpm for 3-10 min, cooling and pelletizing to obtain PA6I. The semi-aromatic transparent nylon material PA6I is high in transparency, excellent in mechanical performance, simple in synthetic steps, small in energy consumption, and suitable for industrialized production.
Description
Technical field
The invention belongs to macromolecular material nylon synthesis field, is related to a kind of semi-aromatic transparent nylon material PA6I and its preparation side
Method.
Background technology
In recent years, nylon is at home and abroad widely used as a kind of thermoplastic engineering plastic.Because its have it is wear-resisting,
The excellent specific property such as impact resistance, endurance, corrosion-resistant, oil resistant, thus be widely used in auto-parts, electronic apparatus,
The industries such as machinery.Over nearly 60 years, demand steady-state growth in the keen competition of engineering plastics of nylon is still occupied always so far
In the first place of five large-engineering plastics.
In general, nylon is semi-crystalline material, the transparency is poor.It is translucent to the exigent occasion of transparent material
Nylon material cannot meet the requirement of people.Transparent nylon is generally amorphous polymer, compared with other transparent materials, no
But it is with the good transparency, and with preferable mechanical property therefore noticeable always to the research of transparent nylon.
Understand that patent 201110419298.6 discloses a kind of preparation method of transparent nylon through the retrieval to existing document, its
Although transparent nylon has been obtained, the technology is that processing is blended by the later stage to carry out, and adds composition to occur not with nylon matrix
Easily compatible problem is still difficult to effectively solving；Patent 201310549652.6 discloses a kind of synthesis technique of copolymerization transparent nylon,
But the technology also needs further to extrude tackified finish after completion of polymerization, and technique is complex.
The content of the invention
Present invention is primarily targeted at a kind of semi-aromatic transparent nylon material PA6I is provided, the semi-aromatic transparent nylon material
PA6I is not only transparent good, and with good mechanical performance.
Further object is that providing a kind of preparation method of semi-aromatic transparent nylon material PA6I, the preparation method
Step is simple, shortens polymerization time, reduces polymerization cost.
To reach above-mentioned purpose, the solution of the present invention is：
A kind of semi-aromatic transparent nylon material PA6I, containing following components and every kind of component weight portion it is as follows：
The gross weight number of M-phthalic acid and hexamethylene diamine is 100 parts.
Above-mentioned catalyst be sodium hypophosphite, phosphorous acid magnesium, Arizona bacilli, zinc phosphite, potassium phosphate in any one or
Several combinations.Catalyst is preferably sodium hypophosphite.
A kind of method for preparing above-mentioned semi-aromatic transparent nylon material PA6I, comprises the steps：
(1), the M-phthalic acid of 58-60 weight portions, the hexamethylene diamine of 40-42 weight portions, 0.0002-0.0007 weight portions are urged
It is added in autoclave after agent mixing, adds the deionized water of 40-80 weight portions；
(2), with the air in inert gas replacement autoclave at least three times, the indifferent gas of 0.05-1.0MPa is then reserved
Body is used as reaction shielding gas；
(3) autoclave, is heated and is stirred continuously, is incubated when the internal temperature of autoclave reaches 100-150 DEG C
1.0-3.0 hours, continue to heat up afterwards, 1.0-3.0 hours are incubated when the temperature of autoclave reaches 200-230 DEG C, afterwards
Continue to heat up, when the pressure of autoclave reaches 2.3-2.70MPa constant pressure 1.0-2.0 hours, continue during constant pressure plus thermal high is anti-
Answer kettle；
(4), release is carried out to autoclave when the temperature of autoclave reaches 275-290 DEG C, heating is stopped during release high
Pressure reactor and maintain autoclave temperature be 255-275 DEG C；
(5), stirring 3-10min is continued with the speed of 7-12rpm when the pressure of autoclave is equal to atmospheric pressure, and cooling is cut
Grain, obtains semi-aromatic transparent nylon material PA6I.
Wherein, the inert gas in step (2) is any one in nitrogen, carbon dioxide, argon gas and helium, preferably nitrogen
Gas.
Stir speed (S.S.) in step (3) is 60-120rpm, and heating rate is 2-5 DEG C/min.
Due to adopting such scheme, the invention has the beneficial effects as follows：
First, the transparency of semi-aromatic transparent nylon material PA6I of the invention is high, good toughness, excellent in mechanical performance, pelletizing
Convenient, particle outward appearance is beautiful.
Secondly, the semi-aromatic transparent nylon material PA6I of the present invention is straight in the presence of catalyst by M-phthalic acid and hexamethylene diamine
Connect and be polymerized, eliminate nylon salt of the prior art after its formation and also need before polymerization through cooling, crystallization, suction filtration
Etc. step and the modified thickening step in later stage, polymerization time is substantially reduced, saved polymerization cost, energy consumption is also less, fitted
In industrialized production.In addition, PA6I in building-up process using deionized water as solvent, it is nontoxic, beneficial to environmental protection.
Specific embodiment
The invention provides a kind of semi-aromatic transparent nylon material PA6I and preparation method thereof.
<Semi-aromatic transparent nylon material PA6I>
Semi-aromatic transparent nylon material PA6I contains following components and the weight portion of every kind of component is as follows：
The gross weight number of M-phthalic acid and hexamethylene diamine is 100 parts.
Catalyst is any one or a few in sodium hypophosphite, phosphorous acid magnesium, Arizona bacilli, zinc phosphite, potassium phosphate
Combination, preferably sodium hypophosphite.
<The preparation method of semi-aromatic transparent nylon material PA6I>
The preparation method of above-mentioned semi-aromatic transparent nylon material PA6I comprises the steps：
(1), the M-phthalic acid of 58-60 weight portions, the hexamethylene diamine of 40-42 weight portions, 0.0002-0.0007 weight portions are urged
Agent is well mixed, and is added in the autoclave with agitating device, and 40-80 weight portions are added toward in the autoclave
Deionized water, open agitating device autoclave is stirred.
(2), with the air in inert gas replacement autoclave at least three times, the indifferent gas of 0.05-1.0MPa is then reserved
Body is used as reaction shielding gas.
(3), heat autoclave by circulating heat conduction oil to be allowed to heat up, the temperature inside autoclave is reached
1.0-3.0 hours are incubated when 100-150 DEG C, so that the reaction monomers for adding are completely into salt, continue to heat up afterwards, when high pressure it is anti-
Answer the temperature inside kettle to be incubated 1.0-3.0 hours again when reaching 200-230 DEG C, be beneficial to the formation of oligomer in reaction system,
The pressure for being continuously heating to autoclave afterwards reaches 2.3-2.70MPa, by discharging the vapor in autoclave (by anti-
Should produce) vapor maintain autoclave constant pressure, constant voltage time be 1.0-2.0 hours, during constant pressure continue plus thermal high it is anti-
Kettle is answered, is beneficial to the further polycondensation of the oligomer high polymer larger so as to obtain molecular weight
(4) release is carried out to autoclave when, the temperature inside autoclave reaches 275-290 DEG C so that reaction system
In vapor be completely exhausted out so that polycondensation process carry out it is more abundant.Stop heating autoclave during release and maintain high pressure
The temperature of reactor is 255-275 DEG C.
(5), stir speed (S.S.) is reduced when the pressure of autoclave is equal to atmospheric pressure, continues to stir with the speed of 7-12rpm
3-10min, and cooling and dicing, obtain semi-aromatic transparent nylon material PA6I.
Wherein, the inert gas in step (2) is any one in nitrogen, carbon dioxide, argon gas and helium, preferably nitrogen
Gas.
Step (1) to (4) is required to unlatching agitating device and autoclave is stirred, and stir speed (S.S.) is 60-120rpm.
Autoclave is heated in step (3) by circulating heat conduction oil to be allowed to heat up, heating rate is 2-5 DEG C/min.In nylon
In polymerization process, because different to temperature requirement into salt, precondensation, polycondensation, it is therefore desirable to temperature programming (first heat up,
It is incubated again, heat up again, is incubated again and heats up again), can so make the properties of nylons outward appearance of polymerization more preferable.
Gained semi-aromatic transparent nylon material PA6I of the invention is poly- by reaction monomers M-phthalic acid and hexamethylene diamine direct polycondensation
Conjunction is formed, and not there is a problem of that the later stage is modified, therefore is not related to the inconsistent problem for adding composition to occur with nylon matrix.Separately
Outward, the viscosity needed for being directly obtained by the adjustment to reaction monomers formula rate in the course of the polymerization process, is not present in polymerization
After the completion of also need further to extrude the subsequent steps such as tackified finish, therefore process is simple is feasible, also shortens polymerization time.
With reference to embodiments the present invention is further illustrated.
The method of testing that the present invention is adopted is as follows：
(1) degree of crystallinity test：Carried out using density gradient method.
(2) tensile property test：Carry out by GB/T1040.1-2006, rate of extension is 5mm/min, in constant temperature and humidity experiment
Under the conditions of test.
(3) simply supported beam notch impact strength test：Carry out by GB/T1043, test under constant temperature and humidity experiment condition.
(4) bending strength test：Carry out by GB/T9341-2008, it is 1.25mm/min to push speed, in constant temperature and humidity reality
Test under the conditions of testing.
Embodiment 1
The preparation method of semi-aromatic transparent nylon material PA6I is as follows in the present embodiment：
(1), the weight portion of M-phthalic acid 58 is weighed according to proportioning, the weight portion of hexamethylene diamine 42 (the two weight portion sum is 100),
The weight portion of catalyst sodium hypophosphite 0.0002, it is ensured that the weight portion sum of M-phthalic acid and hexamethylene diamine is 100 parts.
(2) add after, above-mentioned three kinds of raw materials is well mixed in the autoclave that capacity is 25L, toward in the autoclave
The deionized water of 80 weight portions is injected, agitating device is opened, is stirred with the speed of 120r/min (rpm).
(3) air three times, being reserved in nitrogen displacement in autoclave, and reserved 0.05MPa nitrogen is used as shielding gas.
(4), autoclave is heated using circulating heat conduction oil, is allowed to heat up, when the internal temperature of autoclave is arrived
2 hours are incubated up to when 100 DEG C.
(5) continue heating autoclave after, insulation terminates to be allowed to heat up, when the temperature of autoclave reaches 200 DEG C again
Secondary insulation 2 hours.
(6) continue heating autoclave after, insulation terminates to be allowed to heat up, now, the pressure in autoclave is with temperature
Rising and increase, approximately passing through pressure after 15min reaches 2.3MPa, and the vapor that produces during by release reaction maintains high pressure
Reacting kettle inner pressure it is constant, constant voltage time be 1.5 hours, in constant voltage process continue heat autoclave, be allowed to persistently rise
Temperature.
(7) release is carried out to autoclave when, the temperature inside autoclave reaches 290 DEG C, heating is stopped during release
Autoclave and maintain autoclave temperature be 275 DEG C.
(8) when, the pressure inside autoclave is unloaded to normal pressure, the stir speed (S.S.) of agitating device is reduced, with the speed of 10rpm
Rate continues to stir 3min, in 275 DEG C of drop temperature bottom discharge, water-carrying groove cooling and dicing, obtains semi-aromatic transparent nylon PA6I
Material.
Embodiment 2
The preparation method of semi-aromatic transparent nylon material PA6I is as follows in the present embodiment：
(1), the weight portion of M-phthalic acid 59 is weighed according to proportioning, the weight portion of hexamethylene diamine 41 (the two weight portion sum is 100),
The weight portion of catalyst magnesium phosphate 0.0005, it is ensured that the weight portion sum of M-phthalic acid and hexamethylene diamine is 100 parts.
(2) add after, above-mentioned three kinds of raw materials is well mixed in the autoclave that capacity is 25L, toward in the autoclave
The deionized water of 60 weight portions is injected, agitating device is opened, is stirred with the speed of 60r/min (rpm).
(3) air four times, being reserved in nitrogen displacement in autoclave, and reserved 0.07MPa nitrogen is used as shielding gas.
(4), autoclave is heated using circulating heat conduction oil, is allowed to heat up, when the internal temperature of autoclave is arrived
1.5 hours are incubated up to when 120 DEG C.
(5), insulation terminate after continue heat autoclave be allowed to heat up, when autoclave temperature reach 215 DEG C when after
Continuation of insurance temperature 1 hour.
(6) continue heating autoclave after, insulation terminates to be allowed to heat up, now, the pressure in autoclave is with temperature
Rising and increase, approximately passing through pressure after 23min reaches 2.7MPa, and the vapor that produces during by release reaction maintains high pressure
Reacting kettle inner pressure it is constant, constant voltage time be 1 hour, in constant voltage process continue heat autoclave, be allowed to persistently overheating.
(7) release is carried out to autoclave when, the temperature inside autoclave reaches 285 DEG C, heating is stopped during release
Autoclave and maintain autoclave temperature be 265 DEG C.
(8) when, the pressure inside autoclave is unloaded to normal pressure, the stir speed (S.S.) of agitating device is reduced, with the speed of 7rpm
Rate continues to stir 5min, in 265 DEG C of drop temperature bottom discharge, water-carrying groove cooling and dicing, obtains semi-aromatic transparent nylon PA6I
Material.
Embodiment 3
The preparation method of semi-aromatic transparent nylon material PA6I is as follows in the present embodiment：
(1), the weight portion of M-phthalic acid 60 is weighed according to proportioning, the weight portion of hexamethylene diamine 40 (the two weight portion sum is 100),
The weight portion of catalyst calcium phosphate 0.007, it is ensured that the weight portion sum of M-phthalic acid and hexamethylene diamine is 100 parts.
(2) add after, above-mentioned three kinds of raw materials is well mixed in the autoclave that capacity is 25L, toward in the autoclave
The deionized water of 40 weight portions is injected, agitating device is opened, is stirred with the speed of 80r/min (rpm).
(3) air five times, being reserved in nitrogen displacement in autoclave, and the nitrogen of reserved 1.0MPa is used as shielding gas.
(4), autoclave is heated using circulating heat conduction oil, is allowed to heat up, when the internal temperature of autoclave is arrived
1.0 hours are incubated up to when 150 DEG C.
(5), insulation terminate after continue heat autoclave be allowed to heat up, when autoclave temperature reach 230 DEG C when after
Continuation of insurance temperature 1.5 hours.
(6) continue heating autoclave after, insulation terminates to be allowed to heat up, now, the pressure in autoclave is with temperature
Rising and increase, approximately passing through pressure after 10min reaches 2.5MPa, and the vapor that produces during by release reaction maintains high pressure
Reacting kettle inner pressure it is constant, constant voltage time be 1 hour, in constant voltage process continue heat autoclave, be allowed to persistently overheating.
(7) release is carried out to autoclave when, the temperature inside autoclave reaches 275 DEG C, heating is stopped during release
Autoclave and maintain autoclave temperature be 255 DEG C.
(8) when, the pressure inside autoclave is unloaded to normal pressure, the stir speed (S.S.) of agitating device is reduced, with the speed of 12rpm
Rate continues to stir 4min, in 255 DEG C of drop temperature bottom discharge, water-carrying groove cooling and dicing, obtains semi-aromatic transparent nylon PA6I
Material.
The addition of each component is as shown in table 1 in embodiment 1 to 3.
The component ratio table of table 1
The performance test results of the semi-aromatic transparent nylon material PA6I that above-mentioned section Example is obtained are as shown in table 2：
The test result table of table 2
Learn from the test data of table 2, the transparent semi-aromatic nylon material crystalline degree synthesized in embodiment is less, transparent
Shape, preferably, comprehensive mechanical property is excellent for toughness.
Gained transparent nylon material of the invention has the notable features such as tough and tensile, high transparency, solvent resistant, can be applicable to engineering plastics
High optics lens, industrial safety protective cover in the structural timbers such as blending and modifying, auto parts and components, electrical equipment,
Instrument instrument window and packaging material for food etc..
The above-mentioned description to embodiment is that the present invention is understood that and used for ease of those skilled in the art.It is familiar with
The personnel of art technology obviously easily can make various modifications to these embodiments, and should General Principle described herein
Use in other embodiment without through performing creative labour.Therefore, the invention is not restricted to above-described embodiment, art technology
Personnel's announcement of the invention, the improvement made without departing from scope and modification all should be in protection scope of the present invention
Within.
Claims (8)
1. a kind of semi-aromatic transparent nylon material PA6I, it is characterised in that：Containing following components and every kind of component weight portion such as
Under：
The gross weight number of the M-phthalic acid and the hexamethylene diamine is 100 parts.
2. semi-aromatic transparent nylon material PA6I according to claim 1, it is characterised in that：The catalyst is time phosphorous
Any one or a few combination in sour sodium, phosphorous acid magnesium, Arizona bacilli, zinc phosphite, potassium phosphate.
3. semi-aromatic transparent nylon material PA6I according to claim 2, it is characterised in that：The catalyst is time phosphorous
Sour sodium.
4. a kind of method of the semi-aromatic transparent nylon material PA6I prepared as described in arbitrary in claims 1 to 3, its feature exists
In comprising the steps：
(1), the M-phthalic acid of 58-60 weight portions, the hexamethylene diamine of 40-42 weight portions, 0.0002-0.0007 weight portions are urged
It is added in autoclave after agent mixing, adds the deionized water of 40-80 weight portions；
(2), with the air in inert gas replacement autoclave at least three times, the indifferent gas of 0.05-1.0MPa is then reserved
Body is used as reaction shielding gas；
(3) autoclave, is heated and is stirred continuously, is incubated when the internal temperature of autoclave reaches 100-150 DEG C
1.0-3.0 hours, continue to heat up afterwards, 1.0-3.0 hours are incubated when the temperature of autoclave reaches 200-230 DEG C, afterwards
Continue to heat up, when the pressure of autoclave reaches 2.3-2.70MPa constant pressure 1.0-2.0 hours, continue during constant pressure plus thermal high is anti-
Answer kettle；
(4), release is carried out to autoclave when the temperature of autoclave reaches 275-290 DEG C, heating is stopped during release high
Pressure reactor and maintain autoclave temperature be 255-275 DEG C；
(5), stirring 3-10min is continued with the speed of 7-12rpm when the pressure of autoclave is equal to atmospheric pressure, and cooling is cut
Grain, obtains semi-aromatic transparent nylon material PA6I.
5. method according to claim 4, it is characterised in that：Inert gas in step (2) be nitrogen, carbon dioxide,
Any one in argon gas and helium.
6. method according to claim 4, it is characterised in that：Inert gas in step (2) is nitrogen.
7. method according to claim 4, it is characterised in that：Stir speed (S.S.) in step (3) is 60-120rpm.
8. method according to claim 4, it is characterised in that：Heating rate in step (3) is 2-5 DEG C/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114957652A (en) * | 2022-04-12 | 2022-08-30 | 宿迁联盛亚克力有限公司 | Photo-thermal stable nylon 66 and preparation method thereof |
| CN115894900A (en) * | 2021-08-05 | 2023-04-04 | 上海凯赛生物技术股份有限公司 | Polyamide copolymer PA6IT and preparation method thereof |
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| CN103965466A (en) * | 2013-01-25 | 2014-08-06 | 上海杰事杰新材料(集团)股份有限公司 | Semi-aromatic biological nylon and preparation method thereof |
| CN104031264A (en) * | 2014-06-25 | 2014-09-10 | 东莞市意普万尼龙科技股份有限公司 | Transparent copolymer nylon and preparation method thereof |
| CN104250377A (en) * | 2013-06-25 | 2014-12-31 | 上海杰事杰新材料(集团)股份有限公司 | Low-water absorption biological nylon material PA610T and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115894900A (en) * | 2021-08-05 | 2023-04-04 | 上海凯赛生物技术股份有限公司 | Polyamide copolymer PA6IT and preparation method thereof |
| CN114957652A (en) * | 2022-04-12 | 2022-08-30 | 宿迁联盛亚克力有限公司 | Photo-thermal stable nylon 66 and preparation method thereof |
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Application publication date: 20170426 |