CN115368716B - Preparation method of efficient flame-retardant plastic - Google Patents
Preparation method of efficient flame-retardant plastic Download PDFInfo
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- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
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Abstract
The invention discloses a preparation method of high-efficiency flame-retardant plastic, which belongs to the technical field of functional plastic and comprises the following steps: and respectively adding PET resin, modified glass fiber and a toughening agent into a uniform mixing tank, uniformly mixing and stirring, then adding ammonium polyphosphate, an antioxidant and a lubricant, uniformly mixing and stirring, and finally heating to melt extrusion through a double-screw extruder to obtain the high-efficiency flame-retardant plastic. According to the invention, the glass fiber is modified, and the flexible organic molecular long chain is grafted on the surface of the glass fiber, so that the interfacial compatibility of the glass fiber and the PET matrix can be improved, and the flexible molecular chain can also play a role in toughening, so that the mechanical property of the plastic is improved; in addition, the organic molecular chain contains N-P flame retardant components, so that the flame retardant property of the plastic can be improved to a certain extent, and the organic molecular chain has a synergistic effect with ammonium polyphosphate, so that the plastic is endowed with high-efficiency flame retardant property; finally, the plastic with high mechanical property and high flame retardant property is obtained, and the plastic has wide application range.
Description
Technical Field
The invention belongs to the technical field of functional plastics, and particularly relates to a preparation method of high-efficiency flame-retardant plastics.
Background
Polyethylene terephthalate (PET) is a linear thermoplastic polymer which can maintain excellent physical and mechanical properties in a wide temperature range, is excellent in fatigue resistance, aging resistance, electrical insulation and abrasion resistance, and is excellent in processability, stable to most inorganic acids and organic solvents, and thus is widely used in the fields of producing fibers, bottle flakes, films, engineering plastics and the like, has very important effects on industrial production and human life, has a limiting burning oxygen index (LOI) of 20% -22%, belongs to flammable materials, is easy to burn and causes fire, and can suffocate people and animals by a large amount of smoke generated in the burning process, thereby causing serious threat to life. Because of the linear structure characteristic of PET, the PET produces serious molten drops in the combustion process, and the molten drops become a secondary fire ignition source, so that the situation of fire is continuously expanded. Therefore, the meaning of flame retardant modification of PET is very important.
In the prior art, for example, the invention patent of CN112300543A carries out flame retardant modification by adding zinc hypophosphite and nitrogen flame retardant, but the system is a fiber-free flame retardant system, the problem of compatibility between the halogen-free flame retardant and glass fiber is not solved, and the thermal performance and physical and mechanical properties of the fiber-free flame retardant system are low, so that the application range of the material is greatly limited.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of high-efficiency flame-retardant plastic.
According to the invention, the glass fiber is modified, and the flexible organic molecular long chain is grafted on the surface of the glass fiber, so that the interfacial compatibility of the glass fiber and the PET matrix can be improved, and the flexible molecular chain can also play a role in toughening, so that the mechanical property of the plastic is improved; in addition, the organic molecular chain contains N-P flame retardant components, so that the flame retardant property of the plastic can be improved to a certain extent, and the organic molecular chain has a synergistic effect with ammonium polyphosphate, so that the plastic is endowed with high-efficiency flame retardant property; finally, the plastic with high mechanical property and high flame retardant property is obtained, and the plastic has wide application range.
The aim of the invention can be achieved by the following technical scheme:
a preparation method of high-efficiency flame-retardant plastic comprises the following steps:
the first step, preparing the following raw materials in parts by weight: 100 parts of PET resin, 15-20 parts of modified glass fiber, 12-16 parts of ammonium polyphosphate, 2-3 parts of toughening agent, 1.0-1.2 parts of antioxidant and 1.2-1.4 parts of lubricant;
and secondly, respectively adding PET resin, modified glass fiber and a toughening agent into a uniform mixing tank, uniformly mixing and stirring, then adding ammonium polyphosphate, an antioxidant and a lubricant, uniformly mixing and stirring, and finally heating to melt extrusion by a double-screw extruder, wherein the melt extrusion temperature is 240-260 ℃, and the screw rotation speed is 400-500r/min, so as to obtain the high-efficiency flame-retardant plastic.
Further, the toughening agent is POE-g-GMA (glycidyl methacrylate grafted polyolefin elastomer) or ethylene-methyl acrylate-glycidyl methacrylate.
Further, the antioxidant is antioxidant 1010, antioxidant 168 or antioxidant 1098.
Further, the lubricant is pentaerythritol stearate (PETS), polyethylene wax or silicone powder.
Further, the modified glass fiber is prepared by the following steps:
s1, adding glass fiber and n-butanol into a flask, stirring for 5min, performing ultrasonic treatment for 15min, heating to stabilize the system temperature at 90 ℃, slowly dropwise adding a coupling agent solution, stirring at the temperature for reaction for 6h, performing centrifugal separation after the reaction is finished, washing with absolute ethyl alcohol for 3-4 times, and finally drying the product in a vacuum drying oven at 60 ℃ to obtain the pre-modified glass fiber; the dosage ratio of the n-butyl alcohol, the glass fiber and the coupling agent solution is 20mL:1g:8mL; the coupling agent solution is prepared by uniformly mixing and stirring a silane coupling agent KH550, deionized water and absolute ethyl alcohol according to a mass ratio of 1:1:9;
glass fiber is treated by a silane coupling agent KH550, and a molecular chain of the silane coupling agent KH550 is bonded on the surface of the glass fiber to obtain a pre-modified glass fiber, wherein the bonded molecular chain terminal contains-NH 2 The group lays a reaction site for subsequent reaction;
s2, at N 2 Under the protection, adding polytetrahydrofuran ether glycol and hexamethylene diisocyanate into a four-neck flask provided with a condensing device, a stirring device and a thermometer, heating to 80 ℃ for reaction for 90-100min, adding DBTDL (dibutyl tin dilaurate, a catalyst), and reacting for 4h at a constant temperature of 80 ℃ to obtain an intermediate 1;
under the action of DBTDL, the-OH at two ends of polytetrahydrofuran ether glycol reacts with the-NCO on hexamethylene diisocyanate molecules to generate polyester with the-NCO at two ends, and the reaction process is as follows:
polytetrahydrofuran ether glycol has a structural formula of HO-R-OH, R isThe molecular weight of polytetrahydrofuran ether glycol is 2000;
s3, adding 2-carboxyethyl phenyl hypophosphorous acid and acetone into the intermediate 1, continuously stirring and reacting for 2 hours at the constant temperature of 80 ℃, cooling the reaction mixture to room temperature, adding triethylamine and acetone, stirring and treating for 1 hour, and removing the acetone by rotary evaporation after the reaction is finished to obtain an intermediate 2;
the ratio of polytetrahydrofuran ether glycol, hexamethylene diisocyanate, DBTDL, 2-carboxyethylphenyl hypophosphorous acid, triethylamine and acetone used in steps S2 and S3 was 0.1mol:0.2mol:1.8g:21.4g:10.1g:600mL; the amount of acetone added is the same for the two times;
the-NCO at the end of the molecular chain of the intermediate 1 reacts with-OH on the 2-carboxyethylphenyl hypophosphorous acid molecule, and only one-NCO at one end of the intermediate 1 participates in the reaction by controlling the molar quantity of the 2-carboxyethylphenyl hypophosphorous acid to form an intermediate 2, wherein the reaction process is as follows:
s4, mixing the pre-modified glass fiber and DMF (N, N-dimethylformamide) and then carrying out ultrasonic treatment at room temperature for 10min, transferring the mixed solution into a three-neck flask, adding the intermediate 2 into a system, continuously stirring for 1h, then adding EDC-HCl (1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and a coupling agent), transferring the three-neck flask into a water bath at 60 ℃ for continuously stirring and reacting for 6h, carrying out centrifugal separation, washing with DMF and absolute ethyl alcohol for 4-5 times in sequence to remove unreacted substances, and finally, putting the product into a vacuum drying box at 50 ℃ for drying to constant weight to obtain the modified glass fiber; the dosage ratio of the pre-modified glass fiber, DMF, the intermediate 2 and EDC-HCl is 0.1g:30mL:20g:6mg;
the surface of the obtained modified glass fiber is grafted with an organic molecular long chain through chemical bonding, on one hand, the surface of the obtained modified glass fiber is grafted with the organic molecular long chain, so that the interface compatibility of the glass fiber and a PET matrix can be improved, the uniform dispersion of the glass fiber in the PET is promoted, the interface bonding performance between the glass fiber and the PET is improved, the texture uniformity of the material is improved, and the mechanical property of plastics is further improved; the organic molecular long chain is a flexible molecular long chain, and ester groups, amide groups, ether bonds and the like contained on the organic molecular long chain can form hydrogen bond action with PET molecular chains, and the flexible molecular chains are inserted between the PET molecular chains and form hydrogen bond action with the PET molecular chains, so that the toughening effect can be achieved; on the other hand, the grafted organic molecular chain contains phosphate groups and nitrogen-containing groups, the phosphate groups and the nitrogen-containing groups belong to P-N synergistic flame retardant components, flame retardance can be realized from multiple layers of condensed phases and gas phases, the flame retardant components are uniformly distributed in PET along with glass fibers, and further flame retardance of plastics is improved to a certain extent, and the flame retardant components can produce synergistic effect with ammonium polyphosphate, so that efficient flame retardance of PET plastics is endowed.
The invention has the beneficial effects that:
according to the invention, the glass fiber is modified, and the flexible organic molecular long chain is grafted on the surface of the glass fiber, so that the interfacial compatibility of the glass fiber and the PET matrix can be improved, and the flexible molecular chain can also play a role in toughening, so that the mechanical property of the plastic is improved; in addition, the organic molecular chain contains N-P flame retardant components, so that the flame retardant property of the plastic can be improved to a certain extent, and the organic molecular chain has a synergistic effect with ammonium polyphosphate, so that the plastic is endowed with high-efficiency flame retardant property; finally, the plastic with high mechanical property and high flame retardant property is obtained, and the plastic has wide application range.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Preparing modified glass fiber:
s1, adding 10g of glass fiber and 200mL of n-butanol into a flask, stirring for 5min, performing ultrasonic treatment for 15min, heating to stabilize the system temperature at 90 ℃, slowly dropwise adding 80mL of coupling agent solution into the flask, stirring at the temperature for reaction for 6h, performing centrifugal separation after the reaction is finished, washing with absolute ethyl alcohol for 3 times, and finally drying the product in a vacuum drying oven at 60 ℃ to obtain the pre-modified glass fiber; the coupling agent solution is prepared by uniformly mixing and stirring a silane coupling agent KH550, deionized water and absolute ethyl alcohol according to a mass ratio of 1:1:9;
s2, at N 2 Under the protection, adding 0.1mol of polytetrahydrofuran ether glycol and 0.2mol of hexamethylene diisocyanate into a four-neck flask provided with a condensing device, a stirring device and a thermometer, heating to 80 ℃ for reaction for 90min, adding 1.8g of DBTDL (dibutyl tin dilaurate, catalyst), and reacting for 4h at a constant temperature of 80 ℃ to obtain an intermediate 1;
s3, adding 21.4g of 2-carboxyethyl phenyl hypophosphorous acid and 300mL of acetone into the intermediate 1, continuously stirring at the constant temperature of 80 ℃ for reacting for 2 hours, cooling the reaction mixture to room temperature, adding 10.1g of triethylamine and 300mL of acetone, stirring for 1 hour, and removing the acetone by rotary evaporation after the reaction is finished to obtain an intermediate 2;
s4, mixing 1g of the pre-modified glass fiber and 300mL of DMF (N, N-dimethylformamide), carrying out ultrasonic treatment at room temperature for 10min, transferring the mixed solution into a three-neck flask, adding 200g of intermediate 2 into the system, continuously stirring for 1h, then adding 60mg of EDC-HCl (1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and a coupling agent), transferring the three-neck flask into a water bath at 60 ℃ for continuously stirring and reacting for 6h, carrying out centrifugal separation, washing with DMF and absolute ethyl alcohol for 4 times in sequence to remove unreacted substances, and finally, putting the product into a vacuum drying box at 50 ℃ for drying to constant weight to obtain the modified glass fiber.
Example 2
Preparing modified glass fiber:
s1, adding 2g of glass fiber and 40mL of n-butanol into a flask, stirring for 5min, performing ultrasonic treatment for 15min, heating to stabilize the system temperature at 90 ℃, slowly dropwise adding 16mL of coupling agent solution into the flask, stirring at the temperature for reaction for 6h, performing centrifugal separation after the reaction is finished, washing with absolute ethyl alcohol for 4 times, and finally drying the product in a vacuum drying oven at 60 ℃ to obtain the pre-modified glass fiber; the coupling agent solution is prepared by uniformly mixing and stirring a silane coupling agent KH550, deionized water and absolute ethyl alcohol according to a mass ratio of 1:1:9;
s2, at N 2 Under the protection, adding 0.2mol of polytetrahydrofuran ether glycol and 0.4mol of hexamethylene diisocyanate into a four-neck flask provided with a condensing device, a stirring device and a thermometer, heating to 80 ℃ for reaction for 90-100min, adding 3.6g of DBTDL (dibutyl tin dilaurate, catalyst), and reacting for 4h at the constant temperature of 80 ℃ to obtain an intermediate 1;
s3, adding 42.8g of 2-carboxyethyl phenyl hypophosphorous acid and 600mL of acetone into the intermediate 1, continuously stirring at the constant temperature of 80 ℃ for reacting for 2 hours, cooling the reaction mixture to room temperature, adding 20.2g of triethylamine and 600mL of acetone, stirring for 1 hour, and removing the acetone by rotary evaporation after the reaction is finished to obtain an intermediate 2;
s4, mixing 2g of the pre-modified glass fiber with 600mL of DMF (N, N-dimethylformamide), carrying out ultrasonic treatment at room temperature for 10min, transferring the mixed solution into a three-neck flask, adding 400g of intermediate 2 into the system, continuously stirring for 1h, then adding 120mg of EDC-HCl (1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and a coupling agent), transferring the three-neck flask into a water bath at 60 ℃ for continuously stirring and reacting for 6h, carrying out centrifugal separation, washing with DMF and absolute ethyl alcohol for 5 times in sequence to remove unreacted substances, and finally, putting the product into a vacuum drying box at 50 ℃ for drying to constant weight to obtain the modified glass fiber.
Example 3
A preparation method of high-efficiency flame-retardant plastic comprises the following steps:
the first step, preparing the following raw materials in parts by weight: 100 parts of PET resin, 15 parts of modified glass fiber prepared in example 1, 12 parts of ammonium polyphosphate, 2 parts of POE-g-GMA, 10101.0 parts of antioxidant and 1.2 parts of pentaerythritol stearate;
and secondly, respectively adding PET resin, modified glass fiber and POE-g-GMA into a uniform mixing tank, uniformly mixing and stirring, then adding ammonium polyphosphate, an antioxidant 1010 and pentaerythritol stearate, uniformly mixing and stirring, and finally heating to melt extrusion by a double-screw extruder, wherein the melt extrusion temperature is 240 ℃, and the screw rotation speed is 400r/min, so as to obtain the high-efficiency flame-retardant plastic.
Example 4
A preparation method of high-efficiency flame-retardant plastic comprises the following steps:
the first step, preparing the following raw materials in parts by weight: 100 parts of PET resin, 17.5 parts of modified glass fiber prepared in example 2, 14 parts of ammonium polyphosphate, 2.5 parts of ethylene-methyl acrylate-glycidyl methacrylate, 1681.1 parts of antioxidant and 1.3 parts of polyethylene wax;
secondly, respectively adding PET resin, modified glass fiber and ethylene-methyl acrylate-glycidyl methacrylate into a uniform mixing tank, uniformly mixing and stirring, then adding ammonium polyphosphate, an antioxidant 168 and polyethylene wax, uniformly mixing and stirring, and finally heating to melt extrusion by a double-screw extruder, wherein the melt extrusion temperature is 250 ℃, and the screw rotation speed is 450r/min, so as to obtain the high-efficiency flame-retardant plastic.
Example 5
A preparation method of high-efficiency flame-retardant plastic comprises the following steps:
the first step, preparing the following raw materials in parts by weight: 100 parts of PET resin, 20 parts of modified glass fiber prepared in example 1, 16 parts of ammonium polyphosphate, 3 parts of POE-g-GMA, 10981.2 parts of antioxidant and 1.4 parts of silicone powder;
and secondly, respectively adding PET resin, modified glass fiber and POE-g-GMA into a uniform mixing tank, uniformly mixing and stirring, then adding ammonium polyphosphate, an antioxidant 1098 and silicone powder, uniformly mixing and stirring, and finally heating to melt extrusion by a double-screw extruder, wherein the melt extrusion temperature is 260 ℃, and the screw rotation speed is 500r/min, so as to obtain the high-efficiency flame-retardant plastic.
Comparative example
The modified glass fiber in example 3 was changed to a common glass fiber, and the remaining raw materials and the preparation process were unchanged.
The plastics obtained in examples 3-5 and comparative examples were cut into test samples and subjected to the following performance tests:
tensile properties: according to GB/T1040.1-2018K Standard test of the general rule of the section 1 of determination of Plastic tensile Property;
impact property is tested according to GB/T1843-2008 "determination of impact Strength of Plastic cantilever beam";
the thermal deformation temperature is tested according to ISO75-2004, the load is 1.80MPa, and the heating rate is 2 ℃/min;
limiting oxygen index test (LOI): according to the oxygen index method of the plastic combustion performance test method (GB/T2406), a flat vulcanizing instrument is adopted to heat, melt and tabletting the plastic, and then a critical oxygen index analyzer is used for testing, so as to obtain the limiting oxygen index of the sample;
vertical combustion test: according to the flame retardant property test method-vertical combustion method (GB 240984), a spline is fixed at a position 30.0cm away from a base, absorbent cotton with the thickness of 0.5cm is placed at the base, a fire source is used for continuously acting on the lower part of the spline for 10s, the spline acts for 10s after being extinguished, and the test phenomenon is recorded and compared with the test-horizontal method and vertical method (GB/T2408-2008) of the plastic combustion property;
the results are shown in the following table:
as can be seen from the data in the table, the PET plastic obtained by the invention has good mechanical properties and flame retardant properties, and the data in the comparative example are combined to show that after the glass fiber is modified, a flexible organic molecular chain is introduced into the surface, so that the interfacial compatibility of the glass fiber and PET can be improved, the toughening effect can be achieved, and the mechanical properties of the plastic can be further effectively improved; and the glass fiber can be modified to introduce N-P flame retardant components to have a synergistic effect with ammonium polyphosphate, so that the flame retardant effect of the plastic is effectively improved.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.
Claims (6)
1. The preparation method of the high-efficiency flame-retardant plastic is characterized by comprising the following steps of:
the first step, preparing the following raw materials in parts by weight: 100 parts of PET resin, 15-20 parts of modified glass fiber, 12-16 parts of ammonium polyphosphate, 2-3 parts of toughening agent, 1.0-1.2 parts of antioxidant and 1.2-1.4 parts of lubricant;
secondly, respectively adding PET resin, modified glass fiber and a toughening agent into a uniform mixing tank, uniformly mixing and stirring, then adding ammonium polyphosphate, an antioxidant and a lubricant, uniformly mixing and stirring, and finally heating to melt extrusion through a double-screw extruder to obtain the high-efficiency flame-retardant plastic;
wherein, the modified glass fiber is prepared by the following steps:
s1, adding glass fiber and n-butanol into a flask, stirring for 5min, performing ultrasonic treatment for 15min, heating to stabilize the system temperature at 90 ℃, slowly dropwise adding a coupling agent solution, stirring at the temperature for reaction for 6h, performing centrifugal separation after the reaction is finished, washing with absolute ethyl alcohol for 3-4 times, and finally drying the product in a vacuum drying oven at 60 ℃ to obtain the pre-modified glass fiber; the dosage ratio of the n-butyl alcohol, the glass fiber and the coupling agent solution is 20mL:1g:8mL; the coupling agent solution is prepared by uniformly mixing and stirring a silane coupling agent KH550, deionized water and absolute ethyl alcohol according to a mass ratio of 1:1:9;
s2, at N 2 Under the protection, adding polytetrahydrofuran ether glycol and hexamethylene diisocyanate into a four-neck flask with a condensing device, a stirring device and a thermometer, heating to 80 ℃ for reaction for 90-100min, adding DBTDL, and reacting for 4h at the constant temperature of 80 ℃ to obtain an intermediate 1;
s3, adding 2-carboxyethyl phenyl hypophosphorous acid and acetone into the intermediate 1, continuously stirring and reacting for 2 hours at the constant temperature of 80 ℃, cooling the reaction mixture to room temperature, adding triethylamine and acetone, stirring and treating for 1 hour, and removing the acetone by rotary evaporation after the reaction is finished to obtain an intermediate 2;
s4, mixing the pre-modified glass fiber and DMF, performing ultrasonic treatment at room temperature for 10min, transferring the mixed solution into a three-neck flask, adding the intermediate 2 into the system, continuously stirring for 1h, then adding EDC-HCl, transferring the three-neck flask into a water bath at 60 ℃ for continuously stirring and reacting for 6h, performing centrifugal separation, washing with DMF and absolute ethyl alcohol for 4-5 times in sequence to remove unreacted substances, and finally, putting the product into a vacuum drying oven at 50 ℃ for drying to constant weight to obtain the modified glass fiber.
2. The method for preparing high-efficiency flame-retardant plastic according to claim 1, wherein the toughening agent is POE-g-GMA or ethylene-methyl acrylate-glycidyl methacrylate.
3. The method for preparing high-efficiency flame-retardant plastic according to claim 1, wherein the lubricant is pentaerythritol stearate, polyethylene wax or silicone powder.
4. The method for preparing high-efficiency flame-retardant plastic according to claim 1, wherein the melt extrusion temperature in the second step is 240-260 ℃ and the screw rotation speed is 400-500r/min.
5. The method for preparing high-efficiency flame-retardant plastic according to claim 1, wherein the dosages of polytetrahydrofuran ether glycol, hexamethylene diisocyanate, DBTDL, 2-carboxyethyl phenyl phosphinic acid, triethylamine and acetone in the steps S2 and S3 are 0.1mol:0.2mol:1.8g:21.4g:10.1g:600mL; the amount of acetone added was the same for both additions.
6. The method for preparing high-efficiency flame-retardant plastic according to claim 1, wherein the dosage ratio of the pre-modified glass fiber, DMF, intermediate 2 and EDC-HCl in the step S4 is 0.1g:30mL:20g:6mg.
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| CN116253951B (en) * | 2023-02-20 | 2023-09-29 | 江苏骅腾电力科技有限公司 | Flame-retardant polypropylene plastic |
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| CN107117833A (en) * | 2017-05-14 | 2017-09-01 | 常州力纯数码科技有限公司 | A kind of preparation method of glass fiber infiltration agent |
| WO2018090802A1 (en) * | 2016-11-16 | 2018-05-24 | 金发科技股份有限公司 | Glass fiber-reinforced, halogen-free, and flame-retardant polypropylene material and preparation method and application of same |
| CN112126201A (en) * | 2020-09-30 | 2020-12-25 | 黎明职业大学 | Halogen-free flame-retardant reinforced PET composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2018090802A1 (en) * | 2016-11-16 | 2018-05-24 | 金发科技股份有限公司 | Glass fiber-reinforced, halogen-free, and flame-retardant polypropylene material and preparation method and application of same |
| CN107117833A (en) * | 2017-05-14 | 2017-09-01 | 常州力纯数码科技有限公司 | A kind of preparation method of glass fiber infiltration agent |
| CN112126201A (en) * | 2020-09-30 | 2020-12-25 | 黎明职业大学 | Halogen-free flame-retardant reinforced PET composite material and preparation method thereof |
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