CN110498918A - A kind of preparation method of high-strength wearable damage property nylon resin - Google Patents
A kind of preparation method of high-strength wearable damage property nylon resin Download PDFInfo
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- CN110498918A CN110498918A CN201910745655.4A CN201910745655A CN110498918A CN 110498918 A CN110498918 A CN 110498918A CN 201910745655 A CN201910745655 A CN 201910745655A CN 110498918 A CN110498918 A CN 110498918A
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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
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
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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
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
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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
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
- C08G69/16—Preparatory processes
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyamides (AREA)
Abstract
The invention discloses a kind of preparation methods of high-strength wearable damage property nylon resin, specifically includes the following steps: S1, selection are in right amount than the diluted acid salt, organic acid and organic base of part, diluted acid salt, organic acid and the organic base of selection are put into blender, starting blender is stirred, then it is added in right amount than the polyhydroxy-alcohol of part, organic stabilizer and lactams, mixing time is 20-30 minutes, is mixed them thoroughly uniformly, the present invention relates to nylon resin processing technique fields.The preparation method of high-strength wearable damage property nylon resin, it is modified by olefin(e) acid salt by the organic acid with amino, the water solubility of olefin(e) acid salt and the compatibility of itself and nylon matrix can be improved, modified olefin(e) acid salt can be uniformly dispersed in nylon matrix, stable chemical action can be also produced between nylon molecules chain, the nylon resin being prepared has both excellent toughness and the splendid transparency, while organic stabilizer and lactams is added.
Description
Technical field
The present invention relates to nylon resin processing technique field, specially a kind of preparation side of high-strength wearable damage property nylon resin
Method.
Background technique
Nylon resin materials can manufacture relevant auto parts and components, and the two kinds of automobiles manufactured by nylon resin materials
Components are won a prize due to having used novel nylon resin material, and nylon resin materials related article can be checked by washing in a pan modeling net, polyamides
Amine is commonly called as nylon (Nylon), English name Polyamide (abbreviation PA), density 1.15g/cm3, is on molecular backbone containing weight
The thermoplastic resin general name of multiple amide group-[NHCO]-, including aliphatic PA, fat-aromatic series PA and aromatic series PA,
Middle aliphatic PA is wide in variety, and yield is big, is widely used, and depending on name is by the specific carbon atom number of synthon, nylon is poly-
A kind of saying of nylon (polyamide fibre) can be made into long fine or short fibre, and polyamide fibre is the product name of Fypro, also known as nylon
(Nylon), English name Polyamide (abbreviation PA), basic component are connected by amido bond-[NHCO]-
The fatty polyamide come, resin typically refer to it is heated after be softened or melted range, there is flowing in when softening under external force
It is inclined to, is solid-state, semisolid under room temperature, is also possible to the organic polymer of liquid sometimes, broadly upper definition can be used as modeling
Any high-molecular compound that material products process raw material is referred to as resin.
The wearability of existing nylon resin is bad, so that the product service life of nylon resin production is shorter, Er Qieni
The intensity of imperial resin is bad, reduces the using effect of nylon resin, while also just reducing using nylon resin production product
Quality.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of preparation method of high-strength wearable damage property nylon resin, solutions
Wearability of having determined is bad, so that the product service life of nylon resin production is shorter, and the intensity of nylon resin is bad, reduces
The using effect of nylon resin, while the problem of also just reduce the quality using nylon resin production product.
In order to achieve the above object, the present invention is achieved by the following technical programs: a kind of high-strength wearable damage property nylon tree
The preparation method of rouge, specifically includes the following steps:
S1, it chooses in right amount than the diluted acid salt, organic acid and organic base of part, by diluted acid salt, organic acid and the organic base of selection
It puts into blender, starting blender is stirred, and is then added in right amount than the polyhydroxy-alcohol of part, organic stabilizer and interior acyl
Amine, mixing time are 20-30 minutes, are mixed them thoroughly uniformly;
S2, the mixture then by mixing completion are put into polymerization reaction kettle, are reacted under the protection of nitrogen, will
The temperature of polymerization reaction kettle is controlled at 210-220 degrees Celsius, and pressure is controlled pressure maintaining 1-4 under conditions of 1.8-2.0MPa
Hour;
S3, the mixture in S2 is taken out, pours into blender, the catalyst in right amount than part is then added, is carried out
Stirring is stirred 30-40 minutes, and suitable poly- nitrile rubber solution is then added, and is stirred 20-25 minutes, and whipping temp control exists
20-30℃;
S4, suitable silane coupling agent and deionized water will be added in the mixture in step S3, stir 40-50 minutes,
It mixes them thoroughly, again puts into mixture into polymerization reaction kettle, reacted under the protection of nitrogen, 210~220
1~4h of pressure maintaining under DEG C with 1.8~2.0MPa, then being vented makes pressure in kettle be gradually decrease to normal pressure, and rises temperature in the kettle gradually
Up to 300~350 DEG C, the reaction was continued under the conditions of finally pressure is -0.1~-0.04MPa in kettle, temperature is 300~350 DEG C
10~30min;
S5, the mixture in S4 pour into dryer, the temperature of dryer is adjusted to 60-70 degrees Celsius, it will
Time controlled at 30-50 minutes, and after drying is completed, condensation product carries out pelletizing, obtained finished product, the diameter of finished particle is less than
1CM。
Preferably, raw material components specifically include in the step S1: 14-18 parts of diluted acid salt, 10-15 parts of organic acid, organic
5-12 parts of alkali, 11-15 parts of polyhydroxy-alcohol, 15-20 parts of organic stabilizer and 12-20 parts of lactams.
Preferably, raw material components specifically include in the step S3: 2-6 parts of catalyst and poly- nitrile rubber solution 7-12
Part.
Preferably, raw material components specifically include in the step S3: 5-10 parts and deionized water 7-12 parts of silane coupling agent.
Preferably, the olefin(e) acid salt is Magnesium Acrylate Prepared, calcium acrylate, zinc acrylate resin, acrylic acid copper and zinc methacrylate
One or more of, the organic acid is one or more of alanine, aminocaproic acid and aminoundecanoic acid, described to have
Machine alkali is one or more of triethylamine, pyridine and tetramethylethylenediamine.
Preferably, the catalyst is phosphoric acid, phosphorous acid, hypophosphorous acid and one of its salt and the derivative of ester, institute
The mass ratio for stating catalyst and organic stabilizer is 1:0.5~1:2.
Preferably, the organic stabilizer is one of phenolic group, amido, phosphorus base and thioether based stabilizer, the polyhydroxy
Base alcohol is one or more of ethylene-vinyl alcohol copolymer, polyvinyl alcohol and dipentaerythritol, and the silane coupling agent is silicon
Alkane coupling agent KH550.
Beneficial effect
The present invention provides a kind of preparation methods of high-strength wearable damage property nylon resin.Have compared with prior art following
The utility model has the advantages that the preparation method of high-strength wearable damage property nylon resin, specifically includes the following steps: S1, selection are in right amount than part
Diluted acid salt, organic acid and organic base put into diluted acid salt, organic acid and the organic base of selection into blender, start blender
It is stirred, is then added in right amount than the polyhydroxy-alcohol of part, organic stabilizer and lactams, mixing time is 20-30 minutes, is made
It is sufficiently mixed uniformly;S2, then by mixing complete mixture put into polymerization reaction kettle, under the protection of nitrogen into
Row reaction, the temperature of polymerization reaction kettle is controlled at 210-220 degrees Celsius, and pressure is controlled the condition in 1.8-2.0MPa
Lower pressure maintaining 1-4 hours;S3, the mixture in S2 is taken out, pours into blender, the catalyst in right amount than part is then added, it will
It is stirred, and stirs 30-40 minutes, and suitable poly- nitrile rubber solution is then added, and stirs 20-25 minutes, whipping temp
Control is at 20-30 DEG C;S4, suitable silane coupling agent and deionized water will be added in the mixture in step S3, stirs 40-
It 50 minutes, mixes them thoroughly, again puts into mixture into polymerization reaction kettle, reacted under the protection of nitrogen, In
1~4h of pressure maintaining under 210~220 DEG C and 1.8~2.0MPa, then being vented makes pressure in kettle be gradually decrease to normal pressure, and makes warm in kettle
Degree gradually rises to 300~350 DEG C, under the conditions of finally pressure is -0.1~-0.04MPa in kettle, temperature is 300~350 DEG C
The reaction was continued 10~30min;S5, the mixture in S4 pour into dryer, the temperature of dryer is adjusted to 60-70
Degree Celsius, it will control the time at 30-50 minutes, after drying is completed, condensation product carries out pelletizing, finished product is obtained, finished particle
Diameter be less than 1CM, be modified by olefin(e) acid salt by the organic acid with amino, can be improved olefin(e) acid salt water solubility and its with
The compatibility of nylon matrix, modified olefin(e) acid salt can be uniformly dispersed in nylon matrix, can also produce between nylon molecules chain
Stable chemical action is given birth to, the nylon resin being prepared has both excellent toughness and the splendid transparency, while addition has
The intensity and wearability of nylon resin can be improved in machine stabilizer and lactams.
Detailed description of the invention
Fig. 1 is comparative experiments table figure of the present invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Referring to Fig. 1, the present invention provides three kinds of technical solutions: a kind of preparation method of high-strength wearable damage property nylon resin,
Specifically include following embodiment:
Embodiment 1
S1,16 portions of diluted acid salt, 13 parts of organic acids and 8 parts of organic bases are chosen, by 16 portions of diluted acid salt of selection, 13 parts of organic acids
Put into 8 parts of organic bases into blender, starting blender is stirred, be then added 13 parts of polyhydroxy-alcohols, 17 parts it is organic steady
Determine agent and 16 parts of lactams, mixing time is 25 minutes, is mixed them thoroughly uniformly;
S2, the mixture then by mixing completion are put into polymerization reaction kettle, are reacted under the protection of nitrogen, will
The temperature of polymerization reaction kettle is controlled at 215 degrees Celsius, and pressure is controlled pressure maintaining 2.5 hours under conditions of 1.9MPa;
S3, the mixture in S2 is taken out, is poured into blender, 4 parts of catalyst are then added, is stirred, is stirred
It mixes 35 minutes, 10 parts of poly- nitrile rubber solution is then added, stir 23 minutes, whipping temp is controlled at 25 DEG C;
S4,7 parts of silane coupling agents and 10 parts of deionized waters will be added in the mixture in step S3, stirs 45 minutes, makes
It is sufficiently mixed, and again puts into mixture into polymerization reaction kettle, is reacted under the protection of nitrogen, 215 DEG C with
Pressure maintaining 5.5h under 1.9MPa, then being vented makes pressure in kettle be gradually decrease to normal pressure, and gradually rises temperature in the kettle to 325 DEG C,
The reaction was continued under the conditions of finally pressure is -0.07MPa in kettle, temperature is 325 DEG C 20min;
S5, the mixture in S4 pour into dryer, the temperature of dryer is adjusted to 65 degrees Celsius, by the time
Control was at 40 minutes, and after drying is completed, condensation product carries out pelletizing, obtained finished product, and the diameter of finished particle is less than 1CM.
Embodiment 2
S1,14 portions of diluted acid salt, 10 parts of organic acids and 5 parts of organic bases are chosen, by 14 portions of diluted acid salt of selection, 10 parts of organic acids
Put into 5 parts of organic bases into blender, starting blender is stirred, be then added 11 parts of polyhydroxy-alcohols, 15 parts it is organic steady
Determine agent and 12 parts of lactams, mixing time is 20 minutes, is mixed them thoroughly uniformly;
S2, the mixture then by mixing completion are put into polymerization reaction kettle, are reacted under the protection of nitrogen, will
The temperature of polymerization reaction kettle is controlled at 210 degrees Celsius, and pressure is controlled pressure maintaining 1 hour under conditions of 1.8MPa;
S3, the mixture in S2 is taken out, is poured into blender, 2 parts of catalyst are then added, is stirred, is stirred
It mixes 30 minutes, 7 parts of poly- nitrile rubber solution is then added, stir 20 minutes, whipping temp is controlled at 20 DEG C;
S4,5 parts of silane coupling agents and 7 parts of deionized waters will be added in the mixture in step S3, stirs 40 minutes, makes
It is sufficiently mixed, and again puts into mixture into polymerization reaction kettle, is reacted under the protection of nitrogen, 210 DEG C with
Pressure maintaining 1h under 1.8MPa, then being vented makes pressure in kettle be gradually decrease to normal pressure, and gradually rises temperature in the kettle to 300 DEG C, most
The reaction was continued under the conditions of pressure is -0.1MPa in kettle afterwards, temperature is 300 DEG C 10min;
S5, the mixture in S4 pour into dryer, the temperature of dryer is adjusted to 60 degrees Celsius, by the time
Control was at 30 minutes, and after drying is completed, condensation product carries out pelletizing, obtained finished product, and the diameter of finished particle is less than 1CM.
Embodiment 3
S1,18 portions of diluted acid salt, 15 parts of organic acids and 12 parts of organic bases are chosen, by dilute 18 parts of hydrochlorates of selection, 15 parts it is organic
Acid and 12 parts of organic bases put into blender, starting blender be stirred, then be added 15 parts of polyhydroxy-alcohols, 20 parts it is organic
Stabilizer and 20 parts of lactams, mixing time are 30 minutes, are mixed them thoroughly uniformly;
S2, the mixture then by mixing completion are put into polymerization reaction kettle, are reacted under the protection of nitrogen, will
The temperature of polymerization reaction kettle is controlled at 220 degrees Celsius, and pressure is controlled pressure maintaining 4 hours under conditions of 2.0MPa;
S3, the mixture in S2 is taken out, is poured into blender, 6 parts of catalyst are then added, is stirred, is stirred
It mixes 40 minutes, 12 parts of poly- nitrile rubber solution is then added, stir 25 minutes, whipping temp is controlled at 30 DEG C;
S4,10 parts of silane coupling agents and 12 parts of deionized waters will be added in the mixture in step S3, stirs 50 minutes, makes
It is sufficiently mixed, and again puts into mixture into polymerization reaction kettle, is reacted under the protection of nitrogen, 220 DEG C with
Pressure maintaining 4h under 2.0MPa, then being vented makes pressure in kettle be gradually decrease to normal pressure, and gradually rises temperature in the kettle to 350 DEG C, most
The reaction was continued under the conditions of pressure is -0.04MPa in kettle afterwards, temperature is 350 DEG C 30min;
S5, the mixture in S4 pour into dryer, the temperature of dryer is adjusted to 70 degrees Celsius, by the time
Control was at 50 minutes, and after drying is completed, condensation product carries out pelletizing, obtained finished product, and the diameter of finished particle is less than 1CM.
Comparative experiments
Certain nylon resin manufacturer randomly selects the nylon resin that 30 workers produce the embodiment of the present invention and surveys
Examination, randomly selects the nylon resin that 10 workers produce embodiment 1 and tests, and chooses 10 workers to embodiment 2
The nylon resin of production is tested, and the nylon resin that remaining 10 workers produce embodiment 3 is tested, and to test
Result recorded.
As shown in Figure 1, the effect for the nylon resin that the present embodiment 1 produces is best, rub proofness is 7 grades, tensile strength
Conservation rate is 90%, and for comparative example 2 and embodiment 3, effect is best, by olefin(e) acid salt by the organic acid with amino into
Row is modified, and the water solubility of olefin(e) acid salt and the compatibility of itself and nylon matrix can be improved, and modified olefin(e) acid salt is can be uniformly dispersed
In nylon matrix, stable chemical action can be also produced between nylon molecules chain, the nylon resin being prepared has both
Excellent toughness and the splendid transparency, while organic stabilizer and lactams is added, can be improved nylon resin intensity and
Wearability.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (7)
1. a kind of preparation method of high-strength wearable damage property nylon resin, it is characterised in that: specifically includes the following steps:
S1, it chooses in right amount than the diluted acid salt, organic acid and organic base of part, the diluted acid salt, organic acid and organic base of selection is put into
Into in blender, starting blender is stirred, and is then added in right amount than the polyhydroxy-alcohol of part, organic stabilizer and lactams,
Mixing time is 20-30 minutes, is mixed them thoroughly uniformly;
S2, the mixture then by mixing completion are put into polymerization reaction kettle, are reacted, will be polymerize under the protection of nitrogen
The temperature of reaction kettle is controlled at 210-220 degrees Celsius, and by pressure control pressure maintaining 1-4 hours under conditions of 1.8-2.0MPa;
S3, the mixture in S2 is taken out, pours into blender, the catalyst in right amount than part is then added, is stirred,
Then suitable poly- nitrile rubber solution is added in stirring 30-40 minutes, stir 20-25 minutes, and whipping temp is controlled in 20-30
℃;
S4, suitable silane coupling agent and deionized water will be added in the mixture in step S3, stirs 40-50 minutes, makes it
Be sufficiently mixed, again put into mixture into polymerization reaction kettle, reacted under the protection of nitrogen, 210~220 DEG C with
1~4h of pressure maintaining under 1.8~2.0MPa, then being vented makes pressure in kettle be gradually decrease to normal pressure, and make temperature in the kettle gradually rise to
300~350 DEG C, the reaction was continued under the conditions of finally pressure is -0.1~-0.04MPa in kettle, temperature is 300~350 DEG C 10~
30min;
S5, the mixture in S4 pour into dryer, the temperature of dryer be adjusted to 60-70 degrees Celsius, by the time
Control was at 30-50 minutes, and after drying is completed, condensation product carries out pelletizing, obtained finished product, and the diameter of finished particle is less than 1CM.
2. a kind of preparation method of high-strength wearable damage property nylon resin according to claim 1, it is characterised in that: the step
Raw material components specifically include in rapid S1: 14-18 parts of diluted acid salt, 10-15 parts of organic acid, 5-12 parts of organic base, polyhydroxy-alcohol 11-15
Part, 15-20 parts of organic stabilizer and 12-20 parts of lactams.
3. a kind of preparation method of high-strength wearable damage property nylon resin according to claim 1, it is characterised in that: the step
Raw material components specifically include in rapid S3: 7-12 parts of 2-6 parts of catalyst and poly- nitrile rubber solution.
4. a kind of preparation method of high-strength wearable damage property nylon resin according to claim 1, it is characterised in that: the step
Raw material components specifically include in rapid S3: 5-10 parts and deionized water 7-12 parts of silane coupling agent.
5. a kind of preparation method of high-strength wearable damage property nylon resin according to claim 1, it is characterised in that: the alkene
Hydrochlorate is one or more of Magnesium Acrylate Prepared, calcium acrylate, zinc acrylate resin, acrylic acid copper and zinc methacrylate, described to have
Machine acid is one or more of alanine, aminocaproic acid and aminoundecanoic acid, and the organic base is triethylamine, pyridine and four
One or more of methyl ethylenediamine.
6. a kind of preparation method of high-strength wearable damage property nylon resin according to claim 1, it is characterised in that: described to urge
Agent is phosphoric acid, phosphorous acid, hypophosphorous acid and one of its salt and the derivative of ester, the catalyst and organic stabilizer
Mass ratio is 1:0.5~1:2.
7. a kind of preparation method of high-strength wearable damage property nylon resin according to claim 1, it is characterised in that: described to have
Machine stabilizer is one of phenolic group, amido, phosphorus base and thioether based stabilizer, and the polyhydroxy-alcohol is ethylene vinyl alcohol copolymer
One or more of object, polyvinyl alcohol and dipentaerythritol, the silane coupling agent are Silane coupling agent KH550.
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CN201910745655.4A CN110498918A (en) | 2019-08-13 | 2019-08-13 | A kind of preparation method of high-strength wearable damage property nylon resin |
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Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107446129A (en) * | 2017-08-16 | 2017-12-08 | 株洲时代新材料科技股份有限公司 | A kind of preparation method of anti-aging semi-aromatic nylon resin |
CN107513163A (en) * | 2017-09-18 | 2017-12-26 | 株洲时代新材料科技股份有限公司 | A kind of preparation method of high-transparency high-toughness nylon 66 resin |
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2019
- 2019-08-13 CN CN201910745655.4A patent/CN110498918A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107446129A (en) * | 2017-08-16 | 2017-12-08 | 株洲时代新材料科技股份有限公司 | A kind of preparation method of anti-aging semi-aromatic nylon resin |
CN107513163A (en) * | 2017-09-18 | 2017-12-26 | 株洲时代新材料科技股份有限公司 | A kind of preparation method of high-transparency high-toughness nylon 66 resin |
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Application publication date: 20191126 |