CN105348519A - Transparent polyamide-based nanocomposite and synthetic method thereof - Google Patents
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Abstract
The invention discloses a transparent polyamide-based nanocomposite and a synthetic method thereof. The synthetic method of the nanocomposite comprises the following preparation steps: 1, placing nanoparticles and deionized water into a reaction kettle, conducting stirring for 1-3 hours, and obtaining nanoparticle dispersion liquid; 2, sequentially adding aromatic diacid monomer, aliphatic diacid monomer, cycloaliphatic diamine monomer, polyamine monomer and an auxiliary agent to the nanoparticle dispersion liquid, raising the temperature to 200-220 DEG C in a staged mode under gas protection, maintaining the constant temperature and constant pressure for 0.5-3 hours, then continuing conducting heating, raising the temperature to 250-300 DEG C, controlling the pressure to be 1.5-3 MPa, conducting a reaction for 1-5 hours at the constant temperature with the pressure maintained, then releasing gas slowly, releasing the gas till the normal pressure is reached within 1-3 hours, then conducting vacuumizing for 0.5-3 hours, and conducting pressuring and discharging. The melt index of the transparent polyamide-based nanocomposite prepared through the synthetic method is 10-30 g/10 min, the light transmittance is 80-90%, the water absorption rate is low, and the nanocomposite is resistant to alcohols solvent and excellent in performance.
Description
Technical field
The invention belongs to polymeric material field, be specifically related to a kind of transparent polyamide based nano composite material and synthetic method thereof.
Background technology
Polymeric amide (PA) is the general name of resin containing recurring amide radical group (-CONH-) on molecular chain, is commonly called as nylon, be the kind that kind is maximum, output maximum and purposes is the widest in five large general engineering plastic in the world.Transparent nylon is one indispensable in nylon family, and it is a kind of nylon of amorphous or crystallite, and compared with other transparent plasticss, its transparency is better than polycarbonate (PC), close to polymethylmethacrylate (PMMA).In addition, it also has the performances such as good thermostability, impact property, electrical insulating property, dimensional stability, ageing resistance and linear expansivity are little, finished product shrinking percentage is low, nontoxic, odorless, is widely used in the fields such as automobile, electric, mechanical, optics, physical culture.
Transparent nylon is succeeded in developing early than Dynamit Nobel AG (DynamitNobel) by Germany in 1966 and realizes industrialization, the country such as Japan, the U.S., Switzerland, France has also carried out research and production in succession subsequently, and the transparent nylon of existing multiple kind is researched and developed successfully and achieves industrialization at present.Patent DE4310970, US20120142810A1, CN103589151A and CN103483581A etc. all describe the synthetic method of transparent polyamide.Known by the technology of the synthesis transparent polyamide announced, often in transparent polyamide molecular chain, alicyclic ring is introduced in order to improve its transparency, the introducing of alicyclic ring reduces the regularity of polyamide segment greatly, thus slackened crystallizing power, material is made to form crystallite or in amorphous state, but this is the unavoidable mechanical property sacrificing transparent polyamide just, causes its application to limit to some extent.By adding cheap filler in polyamide substrate, to be enhanced polymeric amide through blending extrusion.Transparent polyamide be its transparency in characteristic, and conventional packing material significantly can reduce its transparency when being used on transparent polyamide, the nanoparticle that the present invention selects belongs to bedded substance, in water after fully emulsified, when carrying out home position polymerization reaction with transparent polyamide monomer, can not affect the transparency of polymerization process and product, but mechanical strength improves a lot than single transparent polyamide.Therefore by changing the relative content of stratiform nanoparticle and transparent polyamide monomer, the object of optimized product performance can just be realized within the specific limits.
Transparent polyamide is a kind of nylon of amorphous or crystallite, its intensity is lower but shock resistance is better, adding of laminar nano particle serves enhancement to transparent polyamide, the mechanical strength of material is increased, add the crystallization behavior that can not change transparent polyamide in essence simultaneously due to layered silicate material, make product have transparent, refractive index and the regulatable feature of mechanical property.Patent CN104250376A adopts layered silicate material successfully to improve the mechanical property of transparent polyamide, the transmittance of transparent polyamide can reach 80% simultaneously, but does not comprise any one nanoparticle that the present invention relates in its mineral filler of selecting.
In order to improve its transparency in the technology of existing synthesis transparent polyamide, often in transparent polyamide molecular chain, introduce alicyclic ring, the introducing of alicyclic ring reduces the regularity of polyamide segment greatly, thus slackened crystallizing power, material is made to form crystallite or in amorphous state, but this is the unavoidable mechanical property sacrificing transparent polyamide just, causes its application to limit to some extent.As everyone knows, packing material can reinforced polyamide, improves its mechanical property.And conventional packing material significantly can reduce its transparency when being used on transparent polyamide, the nanoparticle that the present invention selects belongs to bedded substance, in water after fully emulsified, when carrying out home position polymerization reaction with transparent polyamide monomer, can not affect the transparency of polymerization process and product, but mechanical strength improves a lot than single transparent polyamide.Therefore by changing the relative content of stratiform nanoparticle and transparent polyamide monomer, the object of optimized product performance can just be realized within the specific limits.
Summary of the invention
The present invention aims to provide the transparent polyamide based nano composite material and synthetic method thereof that a kind of mechanical property is good, transparency is high.
A kind of transparent polyamide based nano composite material and synthetic method thereof, is characterized in that, comprise the following steps:
(1) take nanoparticle, dispersion agent and deionized water as in reactor by design proportion, open and stir, strong stirring can obtain nanoparticle dispersion liquid after 1 ~ 3 hour; (2) aromatic dicarboxylic acid mono, binary aliphatic acid mono, cycloalphatic diamine monomer, polyamine monomers and required auxiliary agent are added in nanoparticle dispersion liquid by a certain percentage successively; under the protection of shielding gas, 200 ~ 220 DEG C are warming up to stage by stage after substitution gas; constant temperature and pressure 0.5 ~ 3 hour; then continue to be heated to 250 ~ 300 DEG C; control pressure is at 1.5 ~ 3MPa; pressurize isothermal reaction 1 ~ 5 hour; slowly exit afterwards; exitted in 1 ~ 3 hour to normal pressure; then vacuumize 0.5 ~ 3 hour, reaction terminate, suppress, discharging.
Described nanoparticle is one or more in lithium algae soil, polynite, Feldspar Powder, talcum powder, mica powder and vermiculite, and add-on is 1wt% ~ 30wt%.
Described aromatic monomer is one or more in m-phthalic acid, terephthalic acid and naphthalene diacid, preferred m-phthalic acid and terephthalic acid.
Described binary aliphatic acid mono is one or more in pentanedioic acid, hexanodioic acid, pimelic acid, suberic acid, nonane diacid, sebacic acid, undecane diacid, dodecanedioic acid, undecane dicarboxylic acid, tetradecane diacid, pentadecane diacid, Thapsic acid, pentadecane dicarboxylic acid, octadecane diacid, nonadecen diacid, octadecane dicarboxylic acid, nonadecane dicarboxylic acid, preferred sebacic acid and dodecanedioic acid.
Described aromatic acid and the mol ratio of aliphatic dibasic acid are 1: 9 ~ 9: 1.
Described cycloalphatic diamine is 4, 4 '-diamino cyclohexyl-methane (PACM), 4, 4 '-diamino cyclohexyl propane (PACP), 3, 3 '-dimethyl-4, 4'-diamino cyclohexyl propane (MACM), 3, 3 '-diethyl-4, 4'-diamino cyclohexyl propane (EACM), 3, 3 ', 5, 5 '-tetramethyl--4, one or more in your ketone diamines (IPD) of 4'-diamino cyclohexyl propane (TMACM) and different fluorine, the add-on of cycloalphatic diamine monomer and polyamine monomers summation are 1.0 ~ 1.1 times of diprotic acid molar weight.
Described polyamine monomers is triaminotriphenyl methylmethane, polymine, diethylenetriamine, triethylene tetramine, polyamide-amide and polyetheramine T403, preferably polyethylene imines and polyetheramine T403, content is the 0.1mol% ~ 15mol% of total monomer of polyamide amount.
Auxiliary agent of the present invention comprises end-capping reagent, oxidation inhibitor, catalyzer, whitening agent, thermo-stabilizer, softening agent, releasing agent and fire retardant etc., wherein end-capping reagent is phenylformic acid, acetic acid, propionic acid or Tetra hydro Phthalic anhydride, preferred phenylformic acid, preferred phenylformic acid, addition is 0.01 ~ 1wt% of diacid and diamine monomer total mass, preferably 0.02 ~ 0.5wt%; Oxidation inhibitor is one or more mixing in stannous octoate, dibutyl tin laurate or tin protochloride, preferred tin protochloride, and addition is 0.01 ~ 1wt% of diacid and diamine monomer total mass, preferably 0.02 ~ 0.5wt%; Catalyzer is sodium phosphate, phosphoric acid, calcium phosphate, sodium phosphite, phosphorous acid magnesium, Arizona bacilli, one or more in zinc phosphite, inferior sodium phosphate, ortho phosphorous acid magnesium, Lime Hypophosphate or ortho phosphorous acid zinc, preferred inferior sodium phosphate, addition is 0.01 ~ 0.5wt% of diacid and diamine monomer total mass, preferably 0.02 ~ 0.2wt%; The content of other each auxiliary agents is 0.01 ~ 0.5wt%, preferably equal 0.01 ~ 0.1wt%.
Shielding gas of the present invention is the one in nitrogen, argon gas, helium and carbonic acid gas, preferred nitrogen and carbonic acid gas.
A kind of transparent polyamide based nano composite material, is characterized in that, synthesized by nanoparticle, aromatic dicarboxylic acid mono, binary aliphatic acid mono, cycloalphatic diamine monomer, polyamine monomers and auxiliary agent; Wherein, nanoparticle add-on is 1wt% ~ 30wt%; The mol ratio of aromatic dicarboxylic acid mono and binary aliphatic acid mono is 1: 9 ~ 9: 1; The content of polyamine monomers is the 0.1mol% ~ 15mol% of total monomer of polyamide amount; The add-on of cycloalphatic diamine monomer and polyamine monomers summation are 1.0 ~ 1.1 times of diprotic acid molar weight.
The transmittance of semiaromatic transparent nylon of the present invention is 80 ~ 90%.
The present invention compared with prior art, has following beneficial effect:
(1) outward appearance of transparent polyamide nano composite material that prepared by the present invention has the good transparency, and its mechanical strength is greatly improved simultaneously.
(2) with production formula and controlling of production process molecular size range and distribution, functional polyamines structural unit is introduced, the thermostable transparent nylon resin of synthesis high workability, low processing temperature.
(3) the present invention adopts " single stage method " to prepare transparent polyamide nano composite material, namely adds raw material directly in reactor.This method synthesis technique is simple, decrease due to salification process and extrude Blending Processes, effectively shorten synthesis cycle, improve working efficiency, the use to ethanol in salification process can be reduced simultaneously, reduce cost, decrease and use alcohol solvent and the dangerous fire etc. that brings is unfavorable for the production safety factor of production.
Embodiment
Further illustrate the present invention below by embodiment, following examples are the concrete embodiment of the present invention, but embodiments of the present invention are by the restriction of following embodiment.
Embodiment 1
Take lithium algae soil, dispersion agent and deionized water as in reactor by design proportion, open and stir, strong stirring can obtain lithium algae soil dispersion liquid after 3 hours; By terephthalic acid, dodecanedioic acid, 4,4 '-diamino cyclohexyl-methane (PACM), triethylene tetramine and required auxiliary agent by a certain percentage (see table 1) join in lithium algae soil dispersion liquid successively, and wherein the content of triethylene tetramine is the 5mol% of raw material monomer.With nitrogen replacement gas 6 times, then inflated with nitrogen to pressure is 0.2MPa, sealed reactor.Heat temperature raising, controls temperature rise rate, makes temperature rise to 210 DEG C stage by stage, constant temperature and pressure 1 hour, and wherein open 90 DEG C time and stir, stir speed (S.S.) is 60r/min, starts slow venting when pressure is at 1.8MPa; Then continue to be heated to 275 DEG C, control pressure at 2.2MPa, pressurize isothermal reaction 2 hours, slowly exit afterwards, exitted in 2 hours to normal pressure, then vacuumize 1 hour, reaction terminates, suppresses, discharging, can obtain the native nano composite material of transparent polyamide/lithium algae.
Embodiment 2
Take polynite, dispersion agent and deionized water as in reactor by design proportion, open and stir, strong stirring can obtain lithium algae soil dispersion liquid after 3 hours; By terephthalic acid, dodecanedioic acid, 4,4 '-diamino cyclohexyl-methane (PACM), triethylene tetramine and required auxiliary agent amine by a certain percentage (see table 1) join in lithium algae soil dispersion liquid successively, and wherein the content of triethylene tetramine is the 5mol% of raw material monomer.With nitrogen replacement gas 6 times, then inflated with nitrogen to pressure is 0.2MPa, sealed reactor.Heat temperature raising, controls temperature rise rate, makes temperature rise to 210 DEG C stage by stage, constant temperature and pressure 1 hour, and wherein open 90 DEG C time and stir, stir speed (S.S.) is 60r/min, starts slow venting when pressure is at 1.8MPa; Then continue to be heated to 275 DEG C, control pressure at 2.2MPa, pressurize isothermal reaction 2 hours, slowly exit afterwards, exitted in 2 hours to normal pressure, then vacuumize 1 hour, reaction terminates, suppresses, discharging, can obtain transparent polyamide/Nano composite material of montmorillonite.
Embodiment 3
Take Feldspar Powder, dispersion agent and deionized water as in reactor by design proportion, open and stir, strong stirring can obtain lithium algae soil dispersion liquid after 3 hours; By terephthalic acid, dodecanedioic acid, 4,4 '-diamino cyclohexyl-methane (PACM), polyetheramine T403 and required auxiliary agent by a certain percentage (see table 1) join in lithium algae soil dispersion liquid successively, and wherein the content of polyetheramine T403 is the 5mol% of raw material monomer.With nitrogen replacement gas 6 times, then nitrogen to pressure is 0.2MPa, sealed reactor.Heat temperature raising, controls temperature rise rate, makes temperature rise to 210 DEG C stage by stage, constant temperature and pressure 1 hour, and wherein open 90 DEG C time and stir, stir speed (S.S.) is 60r/min, starts slow venting when pressure is at 1.8MPa; Then continue to be heated to 275 DEG C, control pressure at 2.2MPa, pressurize isothermal reaction 2 hours, slowly exit afterwards, exitted in 2 hours to normal pressure, then vacuumize 1 hour, reaction terminates, suppresses, discharging, can obtain transparent polyamide/Feldspar Powder nano composite material.
Embodiment 4
Take talcum powder, dispersion agent and deionized water as in reactor by design proportion, open and stir, strong stirring can obtain lithium algae soil dispersion liquid after 3 hours; By terephthalic acid, dodecanedioic acid, 4,4 '-diamino cyclohexyl-methane (PACM), polyetheramine T403 and required auxiliary agent by a certain percentage (see table 1) join in lithium algae soil dispersion liquid successively, and wherein the content of polyetheramine T403 is the 5mol% of raw material monomer.With nitrogen replacement gas 6 times, then inflated with nitrogen to pressure is 0.2MPa, sealed reactor.Heat temperature raising, controls temperature rise rate, makes temperature rise to 210 DEG C stage by stage, constant temperature and pressure 1 hour, and wherein open 90 DEG C time and stir, stir speed (S.S.) is 60r/min, starts slow venting when pressure is at 1.8MPa; Then continue to be heated to 275 DEG C, control pressure at 2.2MPa, pressurize isothermal reaction 2 hours, slowly exit afterwards, exitted in 2 hours to normal pressure, then vacuumize 1 hour, reaction terminates, suppresses, discharging, can obtain transparent polyamide/talcum powder nano composite material.
Embodiment 5
Take mica powder, dispersion agent and deionized water as in reactor by design proportion, open and stir, strong stirring can obtain lithium algae soil dispersion liquid after 3 hours; By terephthalic acid, dodecanedioic acid, 4,4 '-diamino cyclohexyl-methane (PACM), diethylenetriamine and required auxiliary agent by a certain percentage (see table 1) join in lithium algae soil dispersion liquid successively, and wherein the content of diethylenetriamine is the 5mol% of raw material monomer.With nitrogen replacement gas 6 times, then inflated with nitrogen to pressure is 0.2MPa, sealed reactor.Heat temperature raising, controls temperature rise rate, makes temperature rise to 210 DEG C stage by stage, constant temperature and pressure 1 hour, and wherein open 90 DEG C time and stir, stir speed (S.S.) is 60r/min, starts slow venting when pressure is at 1.8MPa; Then continue to be heated to 275 DEG C, control pressure at 2.2MPa, pressurize isothermal reaction 2 hours, slowly exit afterwards, exitted in 2 hours to normal pressure, then vacuumize 1 hour, reaction terminates, suppresses, discharging, can obtain transparent polyamide/mica powder nano composite material.
Embodiment 6
Take vermiculite power, dispersion agent and deionized water as in reactor by design proportion, open and stir, strong stirring can obtain lithium algae soil dispersion liquid after 3 hours; By terephthalic acid, dodecanedioic acid, 4,4 '-diamino cyclohexyl-methane (PACM), diethylenetriamine and required auxiliary agent by a certain percentage (see table 1) join in lithium algae soil dispersion liquid successively, and wherein the content of diethylenetriamine is the 5mol% of raw material monomer.With nitrogen replacement gas 6 times, then inflated with nitrogen to pressure is 0.2MPa, sealed reactor.Heat temperature raising, controls temperature rise rate, makes temperature rise to 210 DEG C stage by stage, constant temperature and pressure 1 hour, and wherein open 90 DEG C time and stir, stir speed (S.S.) is 60r/min, starts slow venting when pressure is at 1.8MPa; Then continue to be heated to 275 DEG C, control pressure at 2.2MPa, pressurize isothermal reaction 2 hours, slowly exit afterwards, exitted in 2 hours to normal pressure, then vacuumize 1 hour, reaction terminates, suppresses, discharging, can obtain transparent polyamide/vermiculite power nano composite material.
Comparative example
By terephthalic acid, dodecanedioic acid, 4,4 '-diamino cyclohexyl-methane (PACM) and required auxiliary agent join in autoclave by a certain percentage successively, with nitrogen replacement gas 6 times, then inflated with nitrogen to pressure is 0.2MPa, sealed reactor.Heat temperature raising, controls temperature rise rate, makes temperature rise to 210 DEG C stage by stage, constant temperature and pressure 1 hour, and wherein open 90 DEG C time and stir, stir speed (S.S.) is 60r/min, starts slow venting when pressure is at 1.8MPa; Then continue to be heated to 275 DEG C, control pressure at 2.2MPa, pressurize isothermal reaction 2 hours, slowly exit afterwards, exitted in 2 hours to normal pressure, then vacuumize 1 hour, reaction terminates, suppresses, discharging, can obtain transparent polyamide PACPT/PACP12.
To the transparent polyamide performance test that embodiment 1 ~ 6 and comparative example obtain, the results are shown in Table 2.
The formula table of table 1 embodiment 1 ~ 6 and comparative example
The properties of transparent polyamide prepared by table 2 embodiment 1 ~ 6 and comparative example
Can be found by contrast, after adding nanoparticle, the mechanical property of transparent polyamide is improved, and transparency still remains on more than 85%.
Claims (10)
1. a synthetic method for transparent polyamide based nano composite material, is characterized in that, comprises the following steps:
(1) take nanoparticle and deionized water as in reactor, open and stir, stir and can obtain nanoparticle dispersion liquid after 1 ~ 3 hour; (2) aromatic dicarboxylic acid mono, binary aliphatic acid mono, cycloalphatic diamine monomer, polyamine monomers and auxiliary agent are added in nanoparticle dispersion liquid successively; under the protection of shielding gas, 200 ~ 220 DEG C are warming up to stage by stage after substitution gas; constant temperature and pressure reaction 0.5 ~ 3 hour; then continue to be heated to 250 ~ 300 DEG C; control pressure is at 1.5 ~ 3MPa; pressurize isothermal reaction 1 ~ 5 hour; slowly exit afterwards; exitted in 1 ~ 3 hour to normal pressure; then vacuumize reaction 0.5 ~ 3 hour, reaction terminate, suppress, discharging.
2. the synthetic method of a kind of transparent polyamide based nano composite material according to claim 1, it is characterized in that, described nanoparticle is one or more in lithium algae soil, polynite, Feldspar Powder, talcum powder, mica powder and vermiculite, and add-on is 1wt% ~ 30wt%; Described aromatic dicarboxylic acid mono is one or more in m-phthalic acid, terephthalic acid and naphthalene diacid; Described binary aliphatic acid mono is one or more in pentanedioic acid, hexanodioic acid, pimelic acid, suberic acid, nonane diacid, sebacic acid, undecane diacid, dodecanedioic acid, undecane dicarboxylic acid, tetradecane diacid, pentadecane diacid, Thapsic acid, pentadecane dicarboxylic acid, octadecane diacid, nonadecen diacid, octadecane dicarboxylic acid, nonadecane dicarboxylic acid; Described aromatic dicarboxylic acid mono and the mol ratio of binary aliphatic acid mono are 1: 9 ~ 9: 1.
3. the synthetic method of a kind of transparent polyamide based nano composite material according to claim 1, it is characterized in that, described cycloalphatic diamine monomer is 4, 4 '-diamino cyclohexyl-methane (PACM), 4, 4 '-diamino cyclohexyl propane (PACP), 3, 3 '-dimethyl-4, 4 '-diamino cyclohexyl propane (MACM), 3, 3 '-diethyl-4, 4 '-diamino cyclohexyl propane (EACM), 3, 3 ', 5, 5 '-tetramethyl--4, one or more in your ketone diamines (IPD) of 4 '-diamino cyclohexyl propane (TMACM) and different fluorine, the add-on of cycloalphatic diamine monomer and polyamine monomers summation are 1.0 ~ 1.1 times of diprotic acid molar weight, described polyamine monomers is triaminotriphenyl methylmethane, polymine, diethylenetriamine, triethylene tetramine, polyamide-amide and polyetheramine T403, the amount of described polyamine monomers is the 0.1mol% ~ 15mol% of total monomer of polyamide amount.
4. the synthetic method of a kind of transparent polyamide based nano composite material according to claim 1, it is characterized in that, described auxiliary agent comprises end-capping reagent, end-capping reagent is phenylformic acid, acetic acid, propionic acid or Tetra hydro Phthalic anhydride, and addition is 0.01 ~ 1wt% of diprotic acid and diamine monomer total mass.
5. the synthetic method of a kind of transparent polyamide based nano composite material according to claim 1, it is characterized in that, described auxiliary agent comprises oxidation inhibitor, oxidation inhibitor is one or more mixing in stannous octoate, dibutyl tin laurate and tin protochloride, and addition is 0.01 ~ 1wt% of diprotic acid and diamine monomer total mass.
6. the synthetic method of a kind of transparent polyamide based nano composite material according to claim 1, it is characterized in that, described auxiliary agent comprises catalyzer, catalyzer is sodium phosphate, phosphoric acid, calcium phosphate, sodium phosphite, phosphorous acid magnesium, Arizona bacilli, one or more in zinc phosphite, inferior sodium phosphate, ortho phosphorous acid magnesium, Lime Hypophosphate and ortho phosphorous acid zinc, addition is 0.01 ~ 0.5wt% of diprotic acid and diamine monomer total mass.
7. the synthetic method of a kind of transparent polyamide based nano composite material according to claim 1, is characterized in that, also comprise dispersion agent, whitening agent, thermo-stabilizer, softening agent, releasing agent and fire retardant in described auxiliary agent; The content of described each auxiliary agent is 0.01 ~ 0.5wt%.
8. the synthetic method of a kind of transparent polyamide based nano composite material according to claim 1, is characterized in that, described shielding gas is the one in nitrogen, argon gas, helium and carbonic acid gas, preferred nitrogen and carbonic acid gas.
9. a transparent polyamide based nano composite material, is characterized in that, is synthesized by nanoparticle, aromatic dicarboxylic acid mono, binary aliphatic acid mono, cycloalphatic diamine monomer, polyamine monomers and auxiliary agent; Wherein, nanoparticle add-on is 1wt% ~ 30wt%; The mol ratio of aromatic dicarboxylic acid mono and binary aliphatic acid mono is 1: 9 ~ 9: 1; The content of polyamine monomers is the 0.1mol% ~ 15mol% of total monomer of polyamide amount; The add-on of cycloalphatic diamine monomer and polyamine monomers summation are 1.0 ~ 1.1 times of diprotic acid molar weight.
10. a kind of transparent polyamide based nano composite material according to claim 9, is characterized in that, the melting index of described semiaromatic transparent nylon is 10 ~ 30g/10min; The transmittance of described semiaromatic transparent nylon is 80 ~ 90%.
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