CN115058088A - High-melt-index impact-resistant polystyrene based on liquid alkane modification and preparation method thereof - Google Patents
High-melt-index impact-resistant polystyrene based on liquid alkane modification and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L25/00—Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
- C08L25/02—Homopolymers or copolymers of hydrocarbons
- C08L25/04—Homopolymers or copolymers of styrene
- C08L25/08—Copolymers of styrene
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic System
- C07F9/02—Phosphorus compounds
- C07F9/547—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
- C07F9/6558—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom containing at least two different or differently substituted hetero rings neither condensed among themselves nor condensed with a common carbocyclic ring or ring system
- C07F9/65586—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom containing at least two different or differently substituted hetero rings neither condensed among themselves nor condensed with a common carbocyclic ring or ring system at least one of the hetero rings does not contain nitrogen as ring hetero atom
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- C—CHEMISTRY; METALLURGY
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
Abstract
The invention discloses high-melt-index impact-resistant polystyrene modified based on liquid alkane and a preparation method thereof, wherein the polystyrene comprises the following raw materials in parts by weight: 30-50 parts of modified polystyrene, 50-70 parts of liquid alkane, 10-15 parts of SBS resin and 8-15 parts of modified glass fiber; the modified polystyrene is prepared by soaking liquid alkane in the modified polystyrene, so that the melt index of the high-melt-index impact-resistant polystyrene can reach 20-30, the molecular distance of the modified polystyrene is increased by the modified polystyrene through a modified monomer, the side chain contains a large number of flexible chain segments, the toughness of the modified polystyrene is enhanced, meanwhile, the side chain contains oxyacid of phosphorus and hindered phenol structure, the flame retardance and the aging resistance of the high-melt-index impact-resistant polystyrene are improved, the mechanical property of the high-melt-index impact-resistant polystyrene is greatly improved by the modified glass fiber, and the problem that the material becomes brittle after the modified glass fiber is added is well solved by the modified polystyrene.
Description
Technical Field
The invention relates to the technical field of preparation of high polymer materials, in particular to high-melt-index impact-resistant polystyrene based on liquid alkane modification and a preparation method thereof.
Background
The polystyrene material is a polymer synthesized by styrene monomer through free radical addition polymerization, is thermoplastic plastic, and has the advantages of high transparency, good insulativity, easy coloring, good chemical corrosion resistance and the like, the high impact polystyrene is a thermoplastic material prepared by elastomer modified polystyrene, and is a two-phase system consisting of a rubber phase and a continuous polystyrene phase, and the high impact polystyrene has higher impact resistance than the polystyrene material, and is widely applied to automobiles, instruments, electric products, furniture, computers, disposable articles, medicines, packaging and entertainment markets; however, the existing polystyrene material has a low melt index value, so that the polystyrene material is difficult to process or modify, and has poor self-impact resistance, a common modification means is to add glass fiber to increase the mechanical property of polystyrene, and the brittleness of polystyrene is further improved due to the addition of the glass fiber, so that the normal use of polystyrene is influenced; a solution is now proposed to address the technical drawback in this respect.
Disclosure of Invention
The invention aims to provide high-melt-index impact-resistant polystyrene based on liquid alkane modification and a preparation method thereof, and solves the problems that the polystyrene has low melt index, is difficult to process and has poor mechanical properties at the present stage.
The purpose of the invention can be realized by the following technical scheme:
a high-melt-index impact-resistant polystyrene modified based on liquid alkane comprises the following raw materials in parts by weight: 30-50 parts of modified polystyrene, 50-70 parts of liquid alkane, 10-15 parts of SBS resin and 8-15 parts of modified glass fiber; further, the modified polystyrene is prepared by the following steps:
dissolving sodium chloride in deionized water, adding Arabic gum powder, mixing, stirring and adding styrene, benzoyl peroxide and a modified monomer under the conditions that the rotation speed is 150-200r/min and the temperature is 75-85 ℃, heating to 90-95 ℃, reacting for 6-8h, and filtering to remove filtrate to obtain the modified polystyrene.
Further, the dosage ratio of the sodium chloride, the deionized water, the gum arabic powder, the styrene, the benzoyl peroxide and the modified monomer is 10 g: 135mL of: 2.4 g: 20mL of: 0.25 g: 10 g.
Further, the modified monomer is prepared by the following steps:
step A1: adding phosphorus oxychloride into a reaction kettle, carrying out heat preservation treatment at the temperature of 80-90 ℃ until no hydrogen chloride gas is generated, adding benzyltriethylammonium bromide, continuing to preserve heat, dropwise adding 2, 2' -diallyl bisphenol A, reacting at the rotation speed of 150-;
the reaction process is as follows:
step A2: dissolving the intermediate 1, cardanol and triethylamine in chloroform, carrying out reflux reaction for 3-5h under the conditions that the rotation speed is 200-80 ℃ and the temperature is 70-80 ℃, cooling to room temperature, filtering, removing filter residues, distilling the filtrate, removing the solvent, dissolving the substrate in N, N-dimethylformamide, adding diethanolamine, carrying out reaction for 20-25h under the conditions that the rotation speed is 150-200r/min and the temperature is 40-50 ℃, distilling to remove the solvent, mixing and stirring the substrate and acetone for 2-3h, and filtering to remove the filtrate to obtain an intermediate 2;
the reaction process is as follows:
step A3: uniformly mixing an intermediate 2, 3-chloroperoxybenzoic acid and dichloromethane, reacting for 2-4h at the rotation speed of 300-500r/min and the temperature of 0-3 ℃, filtering, washing the filtrate for 3 times by using a sodium carbonate solution and deionized water respectively, distilling to remove the solvent, dissolving a substrate in N, N-dimethylformamide, adding triethylamine, stirring and dropwise adding acryloyl chloride at the rotation speed of 150-200r/min and the temperature of 0-3 ℃, heating to 20-25 ℃ after dropwise adding, reacting for 10-15h, filtering to remove filter residues, mixing the filter cake with isopropanol, and filtering again to remove the filtrate to obtain an intermediate 3;
the reaction process is as follows:
step A4: dissolving the intermediate 3 in N, N-dimethylformamide, adding 3, 5-di-tert-butyl-4-hydroxyphenyl methanol and boron trifluoride, reacting for 3-5h at the rotation speed of 200-300r/min and the temperature of 100-120 ℃, filtering to remove filter residues, distilling the filtrate, and removing the solvent to obtain the modified monomer.
Further, the molar ratio of the phosphorus oxychloride and the 2, 2' -diallyl bisphenol A in the step A1 is 1.5: 2.3.
further, the molar ratio of the intermediate 1, cardanol and triethylamine in the step A2 is 1: 4: 4, the molar ratio of the substrate to the diethanolamine is 1: 2.
further, the molar ratio of the intermediate 2 and the 3-chloroperoxybenzoic acid in the step A3 is 1: 8, the molar ratio of the used substrate to the used acryloyl chloride is 1: and 4, the mass fraction of the sodium carbonate solution is 5%.
Further, the molar ratio of the intermediate 3 and the 3, 5-di-tert-butyl-4-hydroxyphenyl methanol in the step A4 is 1: 8.
further, the modified glass fiber is prepared by the following steps:
step B1: uniformly mixing concentrated sulfuric acid and hydrogen peroxide, adding glass fiber, stirring for 1-1.5h at the rotation speed of 200-;
step B2: uniformly mixing activated glass fiber, epoxy chloropropane and a sodium hydroxide solution, reacting for 10-15h at the rotation speed of 150-200r/min and the temperature of 30-40 ℃, filtering to remove filtrate, washing a filter cake for 3 times by using deionized water for 10-15s each time, and drying after washing to obtain a dried substance;
step B3: dispersing p-hydroxybenzonitrile in deionized water, stirring at the rotation speed of 200-300r/min and the temperature of 80-90 ℃ until the p-hydroxybenzonitrile is completely dissolved, adding a drying material and boron trifluoride, reacting for 4-6h, and filtering to remove filtrate to obtain the modified glass fiber.
Further, the dosage ratio of the concentrated sulfuric acid, the hydrogen peroxide and the glass fiber in the step B1 is 7 mL: 3mL of: 2g, the mass fraction of concentrated sulfuric acid is 98%, and the mass fraction of hydrogen peroxide is 30%.
Further, the dosage ratio of the activated glass fiber, the epichlorohydrin and the sodium hydroxide solution in the step B2 is 2 g: 5mL of: 10mL, and the mass fraction of the sodium hydroxide solution is 2%.
Further, the mass ratio of the p-hydroxybenzonitrile in the step B3 to the dried substance is 3: 1.
the preparation method of the high-melt-index impact-resistant polystyrene based on liquid alkane modification specifically comprises the following steps:
adding modified polystyrene into liquid alkane, soaking for 1-1.5h under the conditions that the pressure is 0.5-0.8MPa and the temperature is 25-35 ℃, adding SBS resin and modified glass fiber, uniformly mixing, adding into a vacuum granulator, and extruding and granulating under the conditions that the temperature is 200-300 ℃ to obtain the high-index impact-resistant polystyrene.
The invention has the following beneficial effects:
the invention is prepared by soaking liquid alkane in modified polystyrene in the process of preparing high-melt-index impact-resistant polystyrene based on liquid alkane modification, so that the melt index of the high-melt-index impact-resistant polystyrene can reach 20-30, and the modified polystyrene and modified glass fiber are prepared in the preparation process, the modified polystyrene takes phosphorus oxychloride as a raw material to react with 2, 2 '-diallyl bisphenol A, one chlorine atom site on the phosphorus oxychloride reacts with phenolic hydroxyl on the 2, 2' -diallyl bisphenol A through excessive phosphorus oxychloride to prepare an intermediate 1, the intermediate 1 reacts with cardanol, so that the rest chlorine atom sites on the intermediate 1 react with the phenolic hydroxyl on the cardanol, diethanolamine is added to carry out Michael addition reaction to prepare an intermediate 2, and the intermediate 2 is further treated, epoxidizing unsaturated double bonds of side chains, adding acryloyl chloride, performing acryloyl acylation on alcohol hydroxyl groups to prepare an intermediate 3, reacting the intermediate 3 with 3, 5-di-tert-butyl-4-hydroxyphenyl methanol to react epoxy groups on the intermediate 3 with hydroxyl groups on the 3, 5-di-tert-butyl-4-hydroxyphenyl methanol to prepare a modified monomer, copolymerizing the modified monomer with styrene to prepare modified polystyrene, increasing the molecular distance of the modified polystyrene by the modified monomer, and enabling the side chains to contain a large number of flexible chain segments to enhance the toughness of the modified polystyrene, meanwhile, the side chains contain oxyacid of phosphorus and hindered phenol structures to improve the flame retardance and the aging resistance of high-melt-index impact-resistant polystyrene, wherein the modified glass fibers are prepared by activating the surfaces of glass fibers and grafting the glass fibers with epoxy chloride filter cakes, the surface of the glass fiber is grafted with the epoxy group, and then the hydroxyl group reacts with the epoxy group by adding the p-hydroxybenzonitrile, so that a large number of cyano groups are grafted on the surface of the glass fiber, the cyano groups belong to strong polar groups and can enhance the viscosity of the modified glass fiber and the modified polystyrene, the compatibility of the modified glass fiber is increased, the mechanical property of the high-melt-index impact-resistant polystyrene is greatly improved by the modified glass fiber, and the problem that the material becomes brittle after the modified glass fiber is added is well solved by the modified polystyrene.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A high-melt-index impact-resistant polystyrene modified based on liquid alkane comprises the following raw materials in parts by weight: 30 parts of modified polystyrene, 50 parts of normal hexane, 10 parts of SBS resin and 8 parts of modified glass fiber;
the high-melt-index impact-resistant polystyrene is prepared by the following steps:
adding modified polystyrene into n-hexane, soaking for 1h under the conditions of pressure of 0.5MPa and temperature of 25 ℃, adding SBS resin and modified glass fiber, uniformly mixing, adding into a vacuum granulator, and extruding and granulating at the temperature of 200 ℃ to obtain the high-melt-index impact-resistant polystyrene.
The modified polystyrene is prepared by the following steps:
dissolving sodium chloride in deionized water, adding Arabic gum powder, mixing, stirring and adding styrene, benzoyl peroxide, a modified monomer and N, N-dimethylformamide under the conditions that the rotation speed is 150r/min and the temperature is 75 ℃, heating to 90 ℃, reacting for 6 hours, and filtering to remove filtrate to obtain the modified polystyrene.
The modified monomer is prepared by the following steps:
step A1: adding phosphorus oxychloride into a reaction kettle, carrying out heat preservation treatment at the temperature of 80 ℃ until no hydrogen chloride gas is generated, adding benzyl triethyl ammonium bromide, continuing to preserve heat, dropwise adding 2, 2' -diallyl bisphenol A, reacting at the rotation speed of 150r/min until no white smoke gas is generated, heating to 100 ℃, continuing to react for 1h, then heating to 120 ℃ again, and distilling to remove phosphorus oxychloride to obtain an intermediate 1;
step A2: dissolving the intermediate 1, cardanol and triethylamine in chloroform, performing reflux reaction for 3 hours at the rotation speed of 200r/min and the temperature of 70 ℃, cooling to room temperature, filtering, removing filter residues, distilling the filtrate, removing the solvent, dissolving the substrate in N, N-dimethylformamide, adding diethanolamine, performing reaction for 20 hours at the rotation speed of 150r/min and the temperature of 40 ℃, distilling to remove the solvent, mixing and stirring the substrate and acetone for 2 hours, and filtering to remove the filtrate to obtain an intermediate 2;
step A3: uniformly mixing the intermediate 2, 3-chloroperoxybenzoic acid and dichloromethane, reacting for 2 hours at the rotation speed of 300r/min and the temperature of 0 ℃, filtering, washing the filtrate for 3 times by using a sodium carbonate solution and deionized water respectively, distilling to remove the solvent, dissolving a substrate in N, N-dimethylformamide, adding triethylamine, stirring and dropwise adding acryloyl chloride at the rotation speed of 150r/min and the temperature of 0 ℃, heating to the temperature of 20 ℃ after dropwise adding, reacting for 10 hours, filtering to remove filter residues, mixing the filter cake with isopropanol, and filtering again to remove the filtrate to obtain an intermediate 3;
step A4: dissolving the intermediate 3 in N, N-dimethylformamide, adding 3, 5-di-tert-butyl-4-hydroxyphenyl methanol and boron trifluoride, reacting for 3h at 100 ℃ at a rotation speed of 200r/min, filtering to remove filter residue, distilling the filtrate, and removing the solvent to obtain the modified monomer.
The modified glass fiber is prepared by the following steps:
step B1: uniformly mixing concentrated sulfuric acid and hydrogen peroxide, adding glass fiber, stirring for 1h at the rotation speed of 200r/min and the temperature of 100 ℃, filtering to remove filtrate, washing a filter cake to be neutral by using deionized water, and drying to obtain activated glass fiber;
step B2: uniformly mixing activated glass fiber, epoxy chloropropane and a sodium hydroxide solution, reacting for 10 hours at the rotation speed of 150r/min and the temperature of 30 ℃, filtering to remove filtrate, washing a filter cake with deionized water for 3 times, each time for 10s, and drying after washing to obtain a dried substance;
step B3: dispersing p-hydroxybenzonitrile in deionized water, stirring the mixture until the p-hydroxybenzonitrile is completely dissolved at the rotation speed of 200r/min and the temperature of 80 ℃, adding a drying material and boron trifluoride to react for 4 hours, and filtering to remove filtrate to obtain the modified glass fiber.
Example 2
A high-melt-index impact-resistant polystyrene modified based on liquid alkane comprises the following raw materials in parts by weight: 40 parts of modified polystyrene, 60 parts of n-pentane, 13 parts of SBS resin and 10 parts of modified glass fiber;
the high-melt-index impact-resistant polystyrene is prepared by the following steps:
adding modified polystyrene into n-pentane, soaking for 1.3h under the conditions of pressure of 0.6MPa and temperature of 30 ℃, adding SBS resin and modified glass fiber, mixing uniformly, adding into a vacuum granulator, and extruding and granulating at the temperature of 250 ℃ to obtain the high-melt-index impact-resistant polystyrene.
The modified polystyrene is prepared by the following steps:
dissolving sodium chloride in deionized water, adding Arabic gum powder, mixing, stirring and adding styrene, benzoyl peroxide, a modified monomer and N, N-dimethylformamide under the conditions that the rotating speed is 180r/min and the temperature is 80 ℃, heating to 93 ℃, reacting for 7 hours, and filtering to remove filtrate to obtain the modified polystyrene.
The modified monomer is prepared by the following steps:
step A1: adding phosphorus oxychloride into a reaction kettle, carrying out heat preservation treatment at the temperature of 85 ℃ until no hydrogen chloride gas is generated, adding benzyl triethyl ammonium bromide, continuing to preserve heat, dropwise adding 2, 2' -diallyl bisphenol A, reacting at the rotation speed of 180r/min until no white smoke gas is generated, heating to 105 ℃, continuing to react for 1.3h, heating to 125 ℃ again, and distilling to remove phosphorus oxychloride to obtain an intermediate 1;
step A2: dissolving the intermediate 1, cardanol and triethylamine in chloroform, performing reflux reaction for 4 hours at the rotation speed of 200r/min and the temperature of 75 ℃, cooling to room temperature, filtering, removing filter residues, distilling the filtrate, removing the solvent, dissolving the substrate in N, N-dimethylformamide, adding diethanolamine, performing reaction for 23 hours at the rotation speed of 180r/min and the temperature of 45 ℃, distilling to remove the solvent, mixing and stirring the substrate and acetone for 2.5 hours, and filtering to remove the filtrate to obtain an intermediate 2;
step A3: uniformly mixing the intermediate 2, 3-chloroperoxybenzoic acid and dichloromethane, reacting for 3 hours at the rotation speed of 500r/min and the temperature of 2 ℃, filtering, washing the filtrate for 3 times by using a sodium carbonate solution and deionized water respectively, distilling to remove a solvent, dissolving a substrate in N, N-dimethylformamide, adding triethylamine, stirring and dropwise adding acryloyl chloride at the rotation speed of 180r/min and the temperature of 2 ℃, heating to the temperature of 23 ℃ after dropwise adding, reacting for 13 hours, filtering to remove filter residues, mixing a filter cake with isopropanol, and filtering again to remove the filtrate to obtain an intermediate 3;
step A4: dissolving the intermediate 3 in N, N-dimethylformamide, adding 3, 5-di-tert-butyl-4-hydroxyphenyl methanol and boron trifluoride, reacting for 4h at the rotation speed of 200r/min and the temperature of 110 ℃, filtering to remove filter residues, distilling the filtrate, and removing the solvent to obtain the modified monomer.
The modified glass fiber is prepared by the following steps:
step B1: uniformly mixing concentrated sulfuric acid and hydrogen peroxide, adding glass fiber, stirring for 1.3h at the rotation speed of 300r/min and the temperature of 110 ℃, filtering to remove filtrate, washing a filter cake to be neutral by deionized water, and drying to obtain activated glass fiber;
step B2: uniformly mixing activated glass fiber, epoxy chloropropane and a sodium hydroxide solution, reacting for 13 hours at the rotation speed of 180r/min and the temperature of 35 ℃, filtering to remove filtrate, washing a filter cake with deionized water for 3 times for 13s each time, and drying after washing to obtain a dried substance;
step B3: dispersing p-hydroxybenzonitrile in deionized water, stirring until the p-hydroxybenzonitrile is completely dissolved at the rotation speed of 300r/min and the temperature of 85 ℃, adding a drying material and boron trifluoride, reacting for 5 hours, and filtering to remove filtrate to obtain the modified glass fiber.
Example 3
A high-melt-index impact-resistant polystyrene modified based on liquid alkane comprises the following raw materials in parts by weight: 50 parts of modified polystyrene, 70 parts of n-octane, 15 parts of SBS resin and 15 parts of modified glass fiber;
the high-melt-index impact-resistant polystyrene is prepared by the following steps:
adding the modified polystyrene into n-octane, soaking for 1.5h under the conditions that the pressure is 0.8MPa and the temperature is 35 ℃, adding SBS resin and modified glass fiber, uniformly mixing, adding into a vacuum granulator, and extruding and granulating at the temperature of 300 ℃ to obtain the high-melt-index impact-resistant polystyrene.
The modified polystyrene is prepared by the following steps:
dissolving sodium chloride in deionized water, adding Arabic gum powder, mixing, stirring and adding styrene, benzoyl peroxide, a modified monomer and N, N-dimethylformamide under the conditions that the rotation speed is 200r/min and the temperature is 85 ℃, heating to 95 ℃, reacting for 8 hours, and filtering to remove filtrate to obtain the modified polystyrene.
The modified monomer is prepared by the following steps:
step A1: adding phosphorus oxychloride into a reaction kettle, carrying out heat preservation treatment at the temperature of 90 ℃ until no hydrogen chloride gas is generated, adding benzyl triethyl ammonium bromide, continuing to preserve heat, dropwise adding 2, 2' -diallyl bisphenol A, reacting at the rotation speed of 200r/min until no white smoke gas is generated, heating to the temperature of 110 ℃, continuing to react for 1.5h, heating to the temperature of 130 ℃ again, and distilling to remove phosphorus oxychloride to obtain an intermediate 1;
step A2: dissolving the intermediate 1, cardanol and triethylamine in chloroform, performing reflux reaction for 5 hours at the rotation speed of 300r/min and the temperature of 80 ℃, cooling to room temperature, filtering, removing filter residues, distilling the filtrate, removing the solvent, dissolving the substrate in N, N-dimethylformamide, adding diethanolamine, performing reaction for 25 hours at the rotation speed of 200r/min and the temperature of 50 ℃, distilling to remove the solvent, mixing and stirring the substrate and acetone for 3 hours, and filtering to remove the filtrate to obtain an intermediate 2;
step A3: uniformly mixing the intermediate 2, 3-chloroperoxybenzoic acid and dichloromethane, reacting for 4 hours at the rotation speed of 500r/min and the temperature of 3 ℃, filtering, washing the filtrate for 3 times by using a sodium carbonate solution and deionized water respectively, distilling to remove the solvent, dissolving a substrate in N, N-dimethylformamide, adding triethylamine, stirring and dropwise adding acryloyl chloride at the rotation speed of 200r/min and the temperature of 3 ℃, heating to the temperature of 25 ℃ after dropwise adding, reacting for 15 hours, filtering to remove filter residues, mixing the filter cake with isopropanol, and filtering again to remove the filtrate to obtain an intermediate 3;
step A4: dissolving the intermediate 3 in N, N-dimethylformamide, adding 3, 5-di-tert-butyl-4-hydroxyphenyl methanol and boron trifluoride, reacting for 5h at the rotation speed of 300r/min and the temperature of 120 ℃, filtering to remove filter residues, distilling the filtrate, and removing the solvent to obtain the modified monomer.
The modified glass fiber is prepared by the following steps:
step B1: uniformly mixing concentrated sulfuric acid and hydrogen peroxide, adding glass fiber, stirring for 1.5h at the rotation speed of 300r/min and the temperature of 115 ℃, filtering to remove filtrate, washing a filter cake to be neutral by using deionized water, and drying to obtain activated glass fiber;
step B2: uniformly mixing activated glass fiber, epoxy chloropropane and a sodium hydroxide solution, reacting for 15 hours at the rotation speed of 200r/min and the temperature of 40 ℃, filtering to remove filtrate, washing a filter cake with deionized water for 3 times, each time for 15s, and drying after washing to obtain a dried substance;
step B3: dispersing p-hydroxybenzonitrile in deionized water, stirring until the p-hydroxybenzonitrile is completely dissolved at the rotation speed of 300r/min and the temperature of 90 ℃, adding a drying material and boron trifluoride, reacting for 6 hours, and filtering to remove filtrate to obtain the modified glass fiber.
Comparative example 1
This comparative example differs from example 3 in that polystyrene is used in place of modified polystyrene, and the remaining steps are the same.
Comparative example 2
This comparative example differs from example 3 in that no modified glass fiber was added and the remaining steps were the same.
Comparative example 3
This comparative example is the polystyrene prepared in example 11 of chinese patent CN 105585789A.
Comparative example 4
Compared with example 1, the comparative example is not soaked by n-hexane, and the rest steps are the same.
The polystyrene obtained in examples 1 to 3 and comparative examples 1 to 4 was tested for flexural strength in accordance with GB/T9341-2008, notched impact strength in accordance with GB/T1843-2008 and melt index in accordance with ASTM D1238-04, and the results are shown in the following table:
as is apparent from the above table, the polystyrene obtained in examples 1 to 3 had a flexural strength of 82.7 to 83.2MPa and a notched impact strength of 23.5 to 25.4kJ/m 2 The melt index is 28.1-29.3, which shows that the invention has good mechanical property and high melt index property.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (7)
1. High-melt-index impact-resistant polystyrene modified based on liquid alkane is characterized in that: the feed comprises the following raw materials in parts by weight: 30-50 parts of modified polystyrene, 50-70 parts of liquid alkane, 10-15 parts of SBS resin and 8-15 parts of modified glass fiber; the modified polystyrene is prepared by the following steps:
dissolving sodium chloride in deionized water, adding Arabic gum powder, mixing, stirring and adding styrene, benzoyl peroxide and a modified monomer under the conditions that the rotation speed is 150-200r/min and the temperature is 75-85 ℃, heating to 90-95 ℃, reacting for 6-8h, and filtering to remove filtrate to obtain the modified polystyrene.
2. The liquid alkane modified based high melt index high impact polystyrene of claim 1, wherein: the modified monomer is prepared by the following steps:
step A1: adding phosphorus oxychloride into a reaction kettle, carrying out heat preservation treatment until no hydrogen chloride gas is generated, adding benzyl triethyl ammonium bromide, continuing heat preservation, dropwise adding 2, 2' -diallyl bisphenol A, heating for reaction, and distilling to remove phosphorus oxychloride to obtain an intermediate 1;
step A2: dissolving the intermediate 1, cardanol and triethylamine in chloroform, performing reflux reaction, cooling to room temperature, filtering, removing filter residues, distilling the filtrate, removing the solvent, dissolving a substrate in N, N-dimethylformamide, adding diethanolamine, performing reaction, distilling to remove the solvent, mixing and stirring the substrate and acetone, and filtering to remove the filtrate to obtain an intermediate 2;
step A3: mixing the intermediate 2, 3-chloroperoxybenzoic acid and dichloromethane for reaction, filtering, washing filtrate with a sodium carbonate solution and deionized water respectively, distilling to remove a solvent, dissolving a substrate in N, N-dimethylformamide, adding triethylamine, stirring, dropwise adding acryloyl chloride, heating for reaction after dropwise addition is finished, filtering to remove filter residues, mixing a filter cake with isopropanol, and filtering again to remove the filtrate to obtain an intermediate 3;
step A4: dissolving the intermediate 3 in N, N-dimethylformamide, adding 3, 5-di-tert-butyl-4-hydroxyphenyl methanol and boron trifluoride, reacting, filtering to remove filter residue, distilling the filtrate, and removing the solvent to obtain the modified monomer.
3. The liquid alkane modified based high melt index high impact polystyrene of claim 2, wherein: the molar ratio of the phosphorus oxychloride to the 2, 2' -diallyl bisphenol A in the step A1 is 1.5: 2.3.
4. the liquid alkane modified based high melt index high impact polystyrene of claim 2, wherein: the molar ratio of the intermediate 1, cardanol and triethylamine in the step A2 is 1: 4: 4, the molar ratio of the substrate to the diethanolamine is 1: 2.
5. the liquid alkane modified based high melt index high impact polystyrene of claim 2, wherein: the molar ratio of the intermediate 2 and the 3-chloroperoxybenzoic acid in the step A3 is 1: 8, the molar ratio of the used substrate to the used acryloyl chloride is 1: 4.
6. the liquid alkane modified based high melt index high impact polystyrene of claim 2, wherein: the molar ratio of the intermediate 3 and the 3, 5-di-tert-butyl-4-hydroxyphenyl methanol in the step A4 is 1: 8.
7. the method for preparing high-melt-index impact-resistant polystyrene based on liquid alkane modification according to claim 1, wherein the method comprises the following steps: the method specifically comprises the following steps:
adding modified polystyrene into liquid alkane, soaking for 1-1.5h under the conditions that the pressure is 0.5-0.8MPa and the temperature is 25-35 ℃, adding SBS resin and modified glass fiber, uniformly mixing, adding into a vacuum granulator, and extruding and granulating under the conditions that the temperature is 200-300 ℃ to obtain the high-index impact-resistant polystyrene.
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CN115678132A (en) * | 2022-09-13 | 2023-02-03 | 芜湖佳先传动轴有限公司 | Anti-fatigue rubber material for automobile bearing sealing ring |
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