CN113527813A - Preparation process of polypropylene modified plastic - Google Patents
Preparation process of polypropylene modified plastic Download PDFInfo
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- CN113527813A CN113527813A CN202110898306.3A CN202110898306A CN113527813A CN 113527813 A CN113527813 A CN 113527813A CN 202110898306 A CN202110898306 A CN 202110898306A CN 113527813 A CN113527813 A CN 113527813A
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- -1 polypropylene Polymers 0.000 title claims abstract description 41
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 38
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 38
- 239000004033 plastic Substances 0.000 title claims abstract description 24
- 229920003023 plastic Polymers 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000000463 material Substances 0.000 claims abstract description 37
- 239000000654 additive Substances 0.000 claims abstract description 33
- 230000000996 additive effect Effects 0.000 claims abstract description 32
- 239000000203 mixture Substances 0.000 claims abstract description 24
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 23
- 239000001116 FEMA 4028 Substances 0.000 claims abstract description 23
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims abstract description 23
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims abstract description 23
- 229960004853 betadex Drugs 0.000 claims abstract description 23
- 229920005610 lignin Polymers 0.000 claims abstract description 19
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000005303 weighing Methods 0.000 claims abstract description 6
- 239000011256 inorganic filler Substances 0.000 claims abstract description 5
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 90
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 38
- 238000003756 stirring Methods 0.000 claims description 37
- 238000002156 mixing Methods 0.000 claims description 36
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 22
- 239000007864 aqueous solution Substances 0.000 claims description 15
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000000047 product Substances 0.000 claims description 13
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000003054 catalyst Substances 0.000 claims description 12
- 235000019441 ethanol Nutrition 0.000 claims description 12
- 238000000227 grinding Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 239000003822 epoxy resin Substances 0.000 claims description 11
- 229920000647 polyepoxide Polymers 0.000 claims description 11
- 239000003513 alkali Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000001291 vacuum drying Methods 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 239000006227 byproduct Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000011830 basic ionic liquid Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims 1
- 239000007858 starting material Substances 0.000 claims 1
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 13
- 239000003063 flame retardant Substances 0.000 abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052799 carbon Inorganic materials 0.000 abstract description 4
- 238000002844 melting Methods 0.000 abstract description 4
- 230000008018 melting Effects 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 230000002209 hydrophobic effect Effects 0.000 abstract description 3
- 230000002195 synergetic effect Effects 0.000 abstract description 3
- 239000002861 polymer material Substances 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 7
- 239000011159 matrix material Substances 0.000 description 6
- 239000005543 nano-size silicon particle Substances 0.000 description 6
- 235000012239 silicon dioxide Nutrition 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 229910019142 PO4 Inorganic materials 0.000 description 3
- 229940057995 liquid paraffin Drugs 0.000 description 3
- QOHMWDJIBGVPIF-UHFFFAOYSA-N n',n'-diethylpropane-1,3-diamine Chemical compound CCN(CC)CCCN QOHMWDJIBGVPIF-UHFFFAOYSA-N 0.000 description 3
- 239000010452 phosphate Substances 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 238000012644 addition polymerization Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to a preparation process of polypropylene modified plastics, which belongs to the technical field of high polymer materials, and comprises the first step of preparing an additive; secondly, weighing the following raw materials in parts by weight: 100-150 parts of polypropylene, 3-15 parts of additive, 10-15 parts of lignin, 5-15 parts of auxiliary agent and 3-5 parts of inorganic filler; step three, respectively preparing a mixture A and a mixture B; fourthly, adding the mixture B into the mixture A, and extruding and granulating after melting to prepare the polypropylene modified plastic; the prepared primary material is of a hollow round table structure, the inner cavity of the primary material has good oleophylic and hydrophobic properties, beta-cyclodextrin is a polyhydroxy compound, so that the primary material is easy to form carbon and can play a synergistic flame retardant role with the intermediate 2, and then the intermediate 2 and the primary material are mixed in absolute ethyl alcohol in step S4, so that the primary material can be used for inclusion and adsorption of the intermediate 2, and further can form a stable structure with the intermediate 2.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a preparation process of polypropylene modified plastics.
Background
Polypropylene is a polymer of propylene produced by addition polymerization. Is white wax-like material, and has transparent and light appearance. Can resist corrosion of acid, alkali, salt solution and various organic solvents at the temperature of below 80 ℃, and can be decomposed at high temperature and under the action of oxidation. The polypropylene is widely applied to the production of fiber products such as clothes, blankets and the like, medical instruments, automobiles, bicycles, parts, conveying pipelines, chemical containers and the like, and is also used for packaging foods and medicines.
In the production process of polypropylene plastics, in order to improve the flame retardant property of the polypropylene plastics, bromide and antimony trioxide are mainly replaced by hydroxide or phosphorus-containing flame retardant, but the hydroxide has poor flame retardant effect, and needs to be added in a large amount, so that the polypropylene plastics cannot be used due to the reduction of the process fluidity and the deterioration of the mechanical property, and the phosphorus-containing flame retardant cannot be stably compounded with a material matrix due to the self characteristics.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a preparation process of polypropylene modified plastics.
The purpose of the invention can be realized by the following technical scheme:
a preparation process of polypropylene modified plastics comprises the following steps:
firstly, preparing an additive;
secondly, weighing the following raw materials in parts by weight: 100-150 parts of polypropylene, 3-15 parts of additive, 10-15 parts of lignin, 5-15 parts of auxiliary agent and 3-5 parts of inorganic filler;
thirdly, mixing the polypropylene, the lignin and the inorganic filler, and uniformly mixing at the rotating speed of 100-150r/min to prepare a mixture A; mixing the additive and the auxiliary agent, and uniformly mixing at the rotating speed of 500-700r/min to prepare a mixture B;
and fourthly, adding the mixture B into the mixture A, stirring for 30min at the rotating speed of 1200r/min through 1000-.
Further, the additive is prepared by the following steps:
step S1, adding phenol into 75% sodium hydroxide aqueous solution by mass fraction in an equivalent manner for three times, stirring at a constant speed to prepare a suspensoid solution, then slowly dropwise adding phosphorus oxychloride, controlling the temperature to be 10-20 ℃ after dropwise adding, stirring at a constant speed, reacting for 2 hours, washing after the reaction is finished to prepare an intermediate 1, and controlling the weight ratio of the phenol to the sodium hydroxide aqueous solution to the phosphorus oxychloride to be 9-9.5: 10-11: 5-5.5;
in step S1, phenol reacts with sodium hydroxide to generate an intermediate a, and then reacts with phosphorus oxychloride to generate an intermediate 1, wherein the reaction process is as follows:
s2, placing the intermediate 1 into a three-neck flask, adding resorcinol and a catalyst respectively, heating to 100 ℃ and 120 ℃, preserving heat at the temperature, reacting for 4 hours, carrying out reduced pressure distillation, removing by-products to obtain an intermediate 2, controlling the molar ratio of the intermediate 1 to the resorcinol to be 1: 2, and controlling the dosage of the catalyst to be 0.1-0.15% of the sum of the weights of the intermediate 1 and the resorcinol;
in the step S2, the intermediate 1 and resorcinol react under the action of a catalyst to generate an intermediate 2, and the reaction process is as follows:
step S3, sequentially adding beta-cyclodextrin and sodium hydroxide into deionized water, heating to 80 ℃, uniformly stirring until the system is uniform, slowly adding the solution A, keeping the temperature for 6 hours to obtain a product, washing the product, removing unreacted beta-cyclodextrin and epoxy resin, drying in vacuum, grinding to obtain a primary material, and controlling the weight ratio of the beta-cyclodextrin to the sodium hydroxide to the solution A to be 1: 10;
and step S4, dispersing the primary material in absolute ethyl alcohol, uniformly stirring at 70 ℃ until the system is uniform, slowly dropwise adding an ethanol solution of the intermediate 2, heating to 75 ℃ after dropwise adding, uniformly stirring, reacting for 4 hours, filtering, vacuum drying for 10 hours at 100 ℃, grinding to obtain the additive, and controlling the weight ratio of the primary material to the intermediate 2 to be 2: 1.
The intermediate 2 is prepared, the intermediate 2 is a phosphate compound and has excellent flame retardant performance, but the phosphate compound is micromolecular viscous liquid and cannot be well compounded with a matrix when in use, so that beta-cyclodextrin is treated and dried in step S3 to prepare a primary material, the primary material is in a hollow round table structure, an inner cavity of the primary material has good oleophylic and hydrophobic performance, the beta-cyclodextrin is a polyhydroxy compound with high carbon content, so that the beta-cyclodextrin is easy to form carbon and can play a role in synergistic flame retardant with the intermediate 2, and then the intermediate 2 and the primary material are mixed in absolute ethyl alcohol in step S4, the primary material can encapsulate and adsorb the intermediate 2, and further can form a stable structure with the intermediate 2, so that the technical problem of good compounding of the intermediate 2 and the matrix is solved.
Further, the catalyst in step S2 is a basic ionic liquid.
Further, in step S3, the solution A is prepared by mixing epoxy resin and dimethyl sulfoxide according to a molar ratio of 0.5: 10.
Further, the ethanol solution of the intermediate 2 in the step S4 is formed by mixing the intermediate 2 and absolute ethanol according to the weight ratio of 1: 5.
Further, the lignin is any one of alkali lignin, acetic acid lignin or enzymolysis lignin.
The invention has the beneficial effects that:
the polypropylene modified plastic of the invention takes polypropylene as a matrix, an additive is taken as a modifier, the prepared polypropylene plastic is endowed with excellent flame retardant property, the additive firstly reacts with sodium hydroxide to generate an intermediate a in the preparation process, then reacts with phosphorus oxychloride to generate an intermediate 1, then the intermediate 1 reacts with resorcinol under the action of a catalyst to generate an intermediate 2, the intermediate 2 is a phosphate compound, and has excellent flame retardant property, but is a micromolecular viscous liquid which cannot be well compounded with the matrix in use, so that beta-cyclodextrin is treated and dried in step S3 to prepare a primary material, the primary material is in a hollow round table structure, the inner cavity of the primary material has good oleophylic and hydrophobic properties, and the beta-cyclodextrin is a polyhydroxy compound, so that the primary material is easy to form carbon and can play a role of synergistic flame retardant with the intermediate 2, and then step S4, mixing the intermediate 2 with the initial material in absolute ethyl alcohol, wherein the initial material can carry out inclusion and adsorption on the intermediate 2, and further can form a stable structure with the intermediate 2, so that the technical problem of good compounding of the intermediate 2 and a matrix is solved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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
The additive is prepared by the following steps:
step S1, adding phenol into 75% sodium hydroxide aqueous solution by mass fraction in an equivalent manner for three times, stirring at a constant speed to prepare a suspensoid solution, then slowly dropwise adding phosphorus oxychloride, controlling the temperature to be 10 ℃ after dropwise adding, stirring at a constant speed, reacting for 2 hours, washing after the reaction is finished to prepare an intermediate 1, and controlling the weight ratio of the phenol to the sodium hydroxide aqueous solution to the phosphorus oxychloride to be 9: 10: 5;
step S2, placing the intermediate 1 into a three-neck flask, respectively adding resorcinol and a sodium hydroxide aqueous solution with the mass fraction of 15%, heating to 100 ℃, preserving heat at the temperature, reacting for 4 hours, carrying out reduced pressure distillation, removing by-products, and preparing an intermediate 2, wherein the molar ratio of the intermediate 1 to the resorcinol is controlled to be 1: 2, and the dosage of the catalyst is 0.1% of the sum of the weight of the intermediate 1 and the weight of the resorcinol;
step S3, sequentially adding beta-cyclodextrin and sodium hydroxide into deionized water, heating to 80 ℃, uniformly stirring until the system is uniform, slowly adding the solution A, keeping the temperature for 6 hours to obtain a product, washing the product, removing unreacted beta-cyclodextrin and epoxy resin, drying in vacuum, grinding to obtain a primary material, and controlling the weight ratio of the beta-cyclodextrin to the sodium hydroxide to the solution A to be 1: 10;
the solution A is formed by mixing epoxy resin and dimethyl sulfoxide according to a molar ratio of 0.5: 10.
And step S4, dispersing the primary material in absolute ethyl alcohol, uniformly stirring at 70 ℃ until the system is uniform, slowly dropwise adding an ethanol solution of the intermediate 2, heating to 75 ℃ after dropwise adding, uniformly stirring, reacting for 4 hours, filtering, vacuum drying for 10 hours at 100 ℃, grinding to obtain the additive, and controlling the weight ratio of the primary material to the intermediate 2 to be 2: 1.
The ethanol solution of the intermediate 2 is formed by mixing the intermediate 2 and absolute ethanol according to the weight ratio of 1: 5.
Example 2
The additive is prepared by the following steps:
step S1, adding phenol into 75% sodium hydroxide aqueous solution by mass fraction in an equivalent manner for three times, stirring at a constant speed to prepare a suspensoid solution, then slowly dropwise adding phosphorus oxychloride, controlling the temperature to be 15 ℃ after dropwise adding, stirring at a constant speed, reacting for 2 hours, washing after the reaction is finished to prepare an intermediate 1, and controlling the weight ratio of the phenol to the sodium hydroxide aqueous solution to the phosphorus oxychloride to be 9.2: 10.5: 5.3;
step S2, placing the intermediate 1 into a three-neck flask, respectively adding resorcinol and a sodium hydroxide aqueous solution with the mass fraction of 15%, heating to 110 ℃, preserving heat at the temperature, reacting for 4 hours, carrying out reduced pressure distillation, removing by-products, and preparing an intermediate 2, wherein the molar ratio of the intermediate 1 to the resorcinol is controlled to be 1: 2, and the dosage of the catalyst is 0.12% of the sum of the weights of the intermediate 1 and the resorcinol;
step S3, sequentially adding beta-cyclodextrin and sodium hydroxide into deionized water, heating to 80 ℃, uniformly stirring until the system is uniform, slowly adding the solution A, keeping the temperature for 6 hours to obtain a product, washing the product, removing unreacted beta-cyclodextrin and epoxy resin, drying in vacuum, grinding to obtain a primary material, and controlling the weight ratio of the beta-cyclodextrin to the sodium hydroxide to the solution A to be 1: 10;
the solution A is formed by mixing epoxy resin and dimethyl sulfoxide according to a molar ratio of 0.5: 10.
And step S4, dispersing the primary material in absolute ethyl alcohol, uniformly stirring at 70 ℃ until the system is uniform, slowly dropwise adding an ethanol solution of the intermediate 2, heating to 75 ℃ after dropwise adding, uniformly stirring, reacting for 4 hours, filtering, vacuum drying for 10 hours at 100 ℃, grinding to obtain the additive, and controlling the weight ratio of the primary material to the intermediate 2 to be 2: 1.
The ethanol solution of the intermediate 2 is formed by mixing the intermediate 2 and absolute ethanol according to the weight ratio of 1: 5.
Example 3
The additive is prepared by the following steps:
step S1, adding phenol into 75% sodium hydroxide aqueous solution by mass fraction in an equivalent manner for three times, stirring at a constant speed to prepare a suspensoid solution, then slowly dropwise adding phosphorus oxychloride, controlling the temperature to be 18 ℃ after dropwise adding, stirring at a constant speed, reacting for 2 hours, washing after the reaction is finished to prepare an intermediate 1, and controlling the weight ratio of the phenol to the sodium hydroxide aqueous solution to the phosphorus oxychloride to be 9.3: 10.8: 5.3;
step S2, placing the intermediate 1 into a three-neck flask, respectively adding resorcinol and a sodium hydroxide aqueous solution with the mass fraction of 15%, heating to 120 ℃, preserving heat at the temperature, reacting for 4 hours, carrying out reduced pressure distillation, removing by-products, and preparing an intermediate 2, wherein the molar ratio of the intermediate 1 to the resorcinol is controlled to be 1: 2, and the dosage of the catalyst is 0.15% of the sum of the weights of the intermediate 1 and the resorcinol;
step S3, sequentially adding beta-cyclodextrin and sodium hydroxide into deionized water, heating to 80 ℃, uniformly stirring until the system is uniform, slowly adding the solution A, keeping the temperature for 6 hours to obtain a product, washing the product, removing unreacted beta-cyclodextrin and epoxy resin, drying in vacuum, grinding to obtain a primary material, and controlling the weight ratio of the beta-cyclodextrin to the sodium hydroxide to the solution A to be 1: 10;
the solution A is formed by mixing epoxy resin and dimethyl sulfoxide according to a molar ratio of 0.5: 10.
And step S4, dispersing the primary material in absolute ethyl alcohol, uniformly stirring at 70 ℃ until the system is uniform, slowly dropwise adding an ethanol solution of the intermediate 2, heating to 75 ℃ after dropwise adding, uniformly stirring, reacting for 4 hours, filtering, vacuum drying for 10 hours at 100 ℃, grinding to obtain the additive, and controlling the weight ratio of the primary material to the intermediate 2 to be 2: 1.
The ethanol solution of the intermediate 2 is formed by mixing the intermediate 2 and absolute ethanol according to the weight ratio of 1: 5.
Example 4
The additive is prepared by the following steps:
step S1, adding phenol into 75% sodium hydroxide aqueous solution by mass fraction in an equivalent manner for three times, stirring at a constant speed to prepare a suspensoid solution, then slowly dropwise adding phosphorus oxychloride, controlling the temperature to be 20 ℃ after dropwise adding, stirring at a constant speed, reacting for 2 hours, washing after the reaction is finished to prepare an intermediate 1, and controlling the weight ratio of the phenol to the sodium hydroxide aqueous solution to the phosphorus oxychloride to be 9.5: 11: 5.5;
step S2, placing the intermediate 1 into a three-neck flask, respectively adding resorcinol and a sodium hydroxide aqueous solution with the mass fraction of 15%, heating to 120 ℃, preserving heat at the temperature, reacting for 4 hours, carrying out reduced pressure distillation, removing by-products, and preparing an intermediate 2, wherein the molar ratio of the intermediate 1 to the resorcinol is controlled to be 1: 2, and the dosage of the catalyst is 0.15% of the sum of the weights of the intermediate 1 and the resorcinol;
step S3, sequentially adding beta-cyclodextrin and sodium hydroxide into deionized water, heating to 80 ℃, uniformly stirring until the system is uniform, slowly adding the solution A, keeping the temperature for 6 hours to obtain a product, washing the product, removing unreacted beta-cyclodextrin and epoxy resin, drying in vacuum, grinding to obtain a primary material, and controlling the weight ratio of the beta-cyclodextrin to the sodium hydroxide to the solution A to be 1: 10;
the solution A is formed by mixing epoxy resin and dimethyl sulfoxide according to a molar ratio of 0.5: 10.
And step S4, dispersing the primary material in absolute ethyl alcohol, uniformly stirring at 70 ℃ until the system is uniform, slowly dropwise adding an ethanol solution of the intermediate 2, heating to 75 ℃ after dropwise adding, uniformly stirring, reacting for 4 hours, filtering, vacuum drying for 10 hours at 100 ℃, grinding to obtain the additive, and controlling the weight ratio of the primary material to the intermediate 2 to be 2: 1.
The ethanol solution of the intermediate 2 is formed by mixing the intermediate 2 and absolute ethanol according to the weight ratio of 1: 5.
Example 5
A preparation process of polypropylene modified plastics comprises the following steps:
first, an additive was prepared as in example 1;
secondly, weighing the following raw materials in parts by weight: 100 parts of polypropylene, 3 parts of additive, 10 parts of alkali lignin, 5 parts of auxiliary agent and 3 parts of nano silicon dioxide;
thirdly, mixing the polypropylene, the alkali lignin and the nano silicon dioxide, and uniformly mixing at the rotating speed of 100r/min to prepare a mixture A; mixing the additive and the auxiliary agent, and uniformly mixing at the rotating speed of 500r/min to prepare a mixture B;
and fourthly, adding the mixture B into the mixture A, stirring for 30min at the rotating speed of 1000r/min, then heating to 190 ℃, and extruding and granulating after melting to obtain the polypropylene modified plastic.
The auxiliary agent is formed by mixing liquid paraffin and diethylaminopropylamine according to the weight ratio of 1: 1.
Example 6
A preparation process of polypropylene modified plastics comprises the following steps:
first, an additive was prepared as in example 1;
secondly, weighing the following raw materials in parts by weight: 120 parts of polypropylene, 10 parts of additive, 12 parts of alkali lignin, 10 parts of auxiliary agent and 4 parts of nano silicon dioxide;
thirdly, mixing the polypropylene, the alkali lignin and the nano silicon dioxide, and uniformly mixing at the rotating speed of 150r/min to prepare a mixture A; mixing the additive and the auxiliary agent, and uniformly mixing at the rotating speed of 700r/min to prepare a mixture B;
and fourthly, adding the mixture B into the mixture A, stirring for 30min at the rotating speed of 1200r/min, then heating to 200 ℃, and extruding and granulating after melting to obtain the polypropylene modified plastic.
The auxiliary agent is formed by mixing liquid paraffin and diethylaminopropylamine according to the weight ratio of 1: 1.
Example 7
A preparation process of polypropylene modified plastics comprises the following steps:
first, an additive was prepared as in example 1;
secondly, weighing the following raw materials in parts by weight: 150 parts of polypropylene, 15 parts of additive, 15 parts of alkali lignin, 15 parts of auxiliary agent and 5 parts of nano silicon dioxide;
thirdly, mixing the polypropylene, the alkali lignin and the nano silicon dioxide, and uniformly mixing at the rotating speed of 150r/min to prepare a mixture A; mixing the additive and the auxiliary agent, and uniformly mixing at the rotating speed of 700r/min to prepare a mixture B;
and fourthly, adding the mixture B into the mixture A, stirring for 30min at the rotating speed of 1200r/min, then heating to 200 ℃, and extruding and granulating after melting to obtain the polypropylene modified plastic.
The auxiliary agent is formed by mixing liquid paraffin and diethylaminopropylamine according to the weight ratio of 1: 1.
Comparative example 1
This comparative example compares to example 5 with no additives.
Comparative example 2
This comparative example compares to example 5 with an IFR flame retardant in place of the additive.
Comparative example 3
The comparative example was a commercially available polypropylene plastic (Yanshan petrochemical) from a company.
The mechanical properties and flame retardant properties of examples 5 to 7 and comparative examples 1 to 3 were measured, and the results are shown in the following table:
tensile strength and elongation at break: GB/T1040-2006;
notched impact strength: GB/T1043-;
flame retardancy: the vertical burning performance is tested according to UL-94 vertical burning standard, and the vertical burning performance is 3.2mm thick cut into strips.
From the above table, the polypropylene plastic prepared by the method has excellent flame retardant property without affecting the mechanical property of the polypropylene plastic.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to 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 invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. 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 illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (7)
1. The preparation process of the polypropylene modified plastic is characterized by comprising the following steps:
firstly, preparing an additive;
secondly, weighing the following raw materials in parts by weight: 100-150 parts of polypropylene, 3-15 parts of additive, 10-15 parts of lignin, 5-15 parts of auxiliary agent and 3-5 parts of inorganic filler;
thirdly, mixing the polypropylene, the lignin and the inorganic filler, and uniformly stirring and mixing to obtain a mixture A; mixing the additive and the auxiliary agent, and stirring and mixing uniformly to obtain a mixture B;
and fourthly, adding the mixture B into the mixture A, stirring for 30min, then heating to 190-.
2. The process for preparing polypropylene modified plastic according to claim 1, wherein the additive is prepared by the following steps:
step S1, adding phenol into 75% sodium hydroxide aqueous solution by mass fraction in an equivalent manner for three times, stirring at a constant speed to prepare a suspensoid solution, then slowly dropwise adding phosphorus oxychloride, controlling the temperature to be 10-20 ℃ after dropwise adding, stirring at a constant speed, reacting for 2 hours, and washing after the reaction is finished to prepare an intermediate 1;
step S2, placing the intermediate 1 in a three-neck flask, adding resorcinol and a catalyst respectively, heating to 100 ℃ and 120 ℃, preserving heat at the temperature, reacting for 4 hours, and performing reduced pressure distillation to remove byproducts to obtain an intermediate 2;
step S3, sequentially adding beta-cyclodextrin and sodium hydroxide into deionized water, heating to 80 ℃, uniformly stirring until the system is uniform, slowly adding the solution A, carrying out heat preservation reaction for 6 hours to obtain a product, washing the product, carrying out vacuum drying, and grinding to obtain a primary material;
and step S4, dispersing the primary material in absolute ethyl alcohol, uniformly stirring at 70 ℃ until the system is uniform, then slowly dropwise adding the ethanol solution of the intermediate 2, heating to 75 ℃ after dropwise adding, uniformly stirring, reacting for 4 hours, filtering, vacuum drying for 10 hours at 100 ℃, and grinding to obtain the additive.
3. The process of claim 2, wherein the catalyst in step S2 is a basic ionic liquid.
4. The process of claim 2, wherein the solution A in step S3 is prepared by mixing epoxy resin and dimethyl sulfoxide at a molar ratio of 0.5: 10.
5. The process of claim 2, wherein the ethanol solution of intermediate 2 in step S4 is prepared by mixing intermediate 2 and absolute ethanol at a weight ratio of 1: 5.
6. The process of claim 2, wherein the weight ratio of phenol, aqueous sodium hydroxide solution and phosphorus oxychloride is controlled to 9-9.5: 10-11: 5-5.5 in step S1, the molar ratio of intermediate 1 to resorcinol is controlled to 1: 2 in step S2, the amount of catalyst is 0.1-0.15% of the weight sum of intermediate 1 and resorcinol, the weight ratio of β -cyclodextrin, sodium hydroxide and solution A is controlled to 1: 10 in step S3, and the weight ratio of starting material to intermediate 2 is controlled to 2: 1 in step S4.
7. The preparation process of the polypropylene modified plastic as claimed in claim 1, wherein the lignin is any one of alkali lignin, acetic acid lignin or enzymolysis lignin.
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