CN113604035A - Flame-retardant wear-resistant plastic particle and processing technology thereof - Google Patents
Flame-retardant wear-resistant plastic particle and processing technology thereof Download PDFInfo
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- CN113604035A CN113604035A CN202110962948.5A CN202110962948A CN113604035A CN 113604035 A CN113604035 A CN 113604035A CN 202110962948 A CN202110962948 A CN 202110962948A CN 113604035 A CN113604035 A CN 113604035A
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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
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
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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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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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
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
Abstract
The invention discloses a flame-retardant wear-resistant plastic particle and a processing technology thereof, belonging to the technical field of plastic particle preparation, wherein the flame-retardant wear-resistant plastic particle comprises the following raw materials in parts by weight: 40-60 parts of polyamide resin, 8.2-10.4 parts of glass fiber, 1.1-1.7 parts of calcium stearate, 2.3-4.3 parts of toughening agent, 3.5-7.7 parts of antioxidant, 0.5-1.3 parts of coupling agent and 8.2-10.2 parts of flame retardant, and the flame retardant wear-resistant plastic particles are prepared by steps of mixing, extruding and the like, wherein a flame retardant is added, the flame retardant has excellent flame retardant effects of a phosphorus flame retardant and a nitrogen flame retardant, vanillin which is a natural source and furfuryl amine which is a biological matrix are used, and the natural vanillin and the furfuryl amine do not contain halogen, so that the flame retardant has excellent environmental protection performance, and the problems that the conventional flame retardant for polyamide mostly has poor flame retardant effect, large using amount, potential environmental protection and the like are solved effectively.
Description
Technical Field
The invention relates to the technical field of plastic particle preparation, in particular to flame-retardant wear-resistant plastic particles and a processing technology thereof.
Background
Polyamide is a polycondensation type high molecular compound with a-CONH structure in the molecule, is usually obtained by polycondensation of dibasic acid and diamine, is an engineering plastic widely applied in the industry at present, has good comprehensive properties including mechanical property, heat resistance, wear resistance, oil resistance, chemical resistance, dimensional stability and self-lubricity, and is low in friction coefficient, moderate in cost and easy to process. However, polyamide generally has the characteristic of poor flame retardance, in the prior art, a flame retardant is added to improve the flame retardance of polyamide, but the existing flame retardant for polyamide mostly has the problems of poor flame retardance, large using amount, potential environmental protection hazards and the like.
Disclosure of Invention
The invention aims to provide flame-retardant wear-resistant plastic particles and a processing technology thereof, which are used for solving the problems in the background art.
The purpose of the invention can be realized by the following technical scheme:
the flame-retardant wear-resistant plastic particle comprises the following raw materials in parts by weight: 40-60 parts of polyamide resin, 8.2-10.4 parts of glass fiber, 1.1-1.7 parts of calcium stearate, 2.3-4.3 parts of toughening agent, 3.5-7.7 parts of antioxidant, 0.5-1.3 parts of coupling agent and 8.2-10.2 parts of flame retardant;
the flame-retardant wear-resistant plastic particle is prepared by the following steps:
the method comprises the following steps: stirring and mixing polyamide resin, a toughening agent and a coupling agent at the rotation speed of 500r/min, then adding calcium stearate, an antioxidant and a flame retardant, and mixing at the rotation speed of 200 and 400r/min to obtain a first material;
step two: and adding the material I and the glass fiber into a double-screw extruder, setting the rotating speed of the screw at 300r/min and the temperature at 150-.
Further, the toughening agent is an ethylene-octene copolymer or an ethylene-vinyl acetate copolymer.
Further, the antioxidant is any one of hindered phenol antioxidants, hindered amine antioxidants and phosphite antioxidants.
Further, the coupling agent is a silane coupling agent.
Further, the flame retardant is prepared by the following steps:
step S1: adding carbazole and tetrahydrofuran into a flask, then adding sodium hydride, stirring for 30min at room temperature, then heating to 60 ℃, adding phosphorus oxychloride into the flask, carrying out reflux reaction for 2-3h, adding a saturated ammonium chloride solution after the reaction is finished, and carrying out quenching reaction to obtain an intermediate 1; the dosage ratio of carbazole, tetrahydrofuran, sodium hydride and phosphorus oxychloride is 0.011 mol: 20mL of: 0.022 mol: 0.01 mol;
the reaction process is as follows:
step S2: adding vanillin, acetone and anhydrous sodium carbonate into a flask, introducing nitrogen, stirring for 1h, adding the intermediate 1, heating to 55 ℃, reacting for 6-7h, and cooling to obtain an intermediate 2; the dosage ratio of the vanillin, the acetone, the anhydrous sodium carbonate and the intermediate 1 is 0.8 mol: 400 mL: 90 g: 0.81 mol;
the reaction process is as follows:
step S3: adding the intermediate 2 and furfuryl amine into a flask filled with absolute ethyl alcohol, heating to 70 ℃, keeping the temperature, reacting for 5 hours, and standing at-4 ℃ for 12 hours to prepare a flame retardant; the dosage ratio of the intermediate 2, the furfuryl amine and the absolute ethyl alcohol is 0.1 mol: 0.23 mol: 150 mL;
the reaction process is as follows:
the invention provides flame-retardant wear-resistant plastic particles and a processing technology thereof. Compared with the prior art, the method has the following beneficial effects: the invention adds a flame retardant to prepare an intermediate 1 by reacting carbazole with active chlorine of phosphorus oxychloride when preparing plastic particles, then prepares an intermediate 2 by reacting the intermediate 1 with hydroxyl of vanillin, and then combines aldehyde group of the intermediate 2 with amino group of furfuryl amine through ammonia-aldehyde condensation reaction to prepare the flame retardant, wherein the flame retardant has excellent flame retardant effects of phosphorus flame retardant and nitrogen flame retardant, and uses natural vanillin and furfuryl amine of biological matrix, and does not contain halogen, thereby having excellent environmental protection performance, and effectively solving the problems of poor flame retardant effect, large dosage, environmental protection hidden trouble and the like of the existing flame retardant for polyamide.
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
Preparing a flame retardant, wherein the flame retardant is prepared by the following steps:
step S1: adding carbazole and tetrahydrofuran into a flask, then adding sodium hydride, stirring for 30min at room temperature, then heating to 60 ℃, adding phosphorus oxychloride into the flask, carrying out reflux reaction for 2h, adding a saturated ammonium chloride solution after the reaction is finished, and carrying out quenching reaction to obtain an intermediate 1; the dosage ratio of carbazole, tetrahydrofuran, sodium hydride and phosphorus oxychloride is 0.011 mol: 20mL of: 0.022 mol: 0.01 mol;
step S2: adding vanillin, acetone and anhydrous sodium carbonate into a flask, introducing nitrogen, stirring for 1h, adding the intermediate 1, heating to 55 ℃, reacting for 6h, and cooling to obtain an intermediate 2; the dosage ratio of the vanillin, the acetone, the anhydrous sodium carbonate and the intermediate 1 is 0.8 mol: 400 mL: 90 g: 0.81 mol;
step S3: adding the intermediate 2 and furfuryl amine into a flask filled with absolute ethyl alcohol, heating to 70 ℃, keeping the temperature, reacting for 5 hours, and standing at-4 ℃ for 12 hours to prepare a flame retardant; the dosage ratio of the intermediate 2, the furfuryl amine and the absolute ethyl alcohol is 0.1 mol: 0.23 mol: 150 mL.
Example 2
Preparing a flame retardant, wherein the flame retardant is prepared by the following steps:
step S1: adding carbazole and tetrahydrofuran into a flask, then adding sodium hydride, stirring for 30min at room temperature, then heating to 60 ℃, adding phosphorus oxychloride into the flask, carrying out reflux reaction for 2.5h, adding a saturated ammonium chloride solution after the reaction is finished, and carrying out quenching reaction to obtain an intermediate 1; the dosage ratio of carbazole, tetrahydrofuran, sodium hydride and phosphorus oxychloride is 0.011 mol: 20mL of: 0.022 mol: 0.01 mol;
step S2: adding vanillin, acetone and anhydrous sodium carbonate into a flask, introducing nitrogen, stirring for 1h, adding the intermediate 1, heating to 55 ℃, reacting for 6.5h, and cooling to obtain an intermediate 2; the dosage ratio of the vanillin, the acetone, the anhydrous sodium carbonate and the intermediate 1 is 0.8 mol: 400 mL: 90 g: 0.81 mol;
step S3: adding the intermediate 2 and furfuryl amine into a flask filled with absolute ethyl alcohol, heating to 70 ℃, keeping the temperature, reacting for 5 hours, and standing at-4 ℃ for 12 hours to prepare a flame retardant; the dosage ratio of the intermediate 2, the furfuryl amine and the absolute ethyl alcohol is 0.1 mol: 0.23 mol: 150 mL.
Example 3
Preparing a flame retardant, wherein the flame retardant is prepared by the following steps:
step S1: adding carbazole and tetrahydrofuran into a flask, then adding sodium hydride, stirring for 30min at room temperature, then heating to 60 ℃, adding phosphorus oxychloride into the flask, carrying out reflux reaction for 3h, adding a saturated ammonium chloride solution after the reaction is finished, and carrying out quenching reaction to obtain an intermediate 1; the dosage ratio of carbazole, tetrahydrofuran, sodium hydride and phosphorus oxychloride is 0.011 mol: 20mL of: 0.022 mol: 0.01 mol;
step S2: adding vanillin, acetone and anhydrous sodium carbonate into a flask, introducing nitrogen, stirring for 1h, adding the intermediate 1, heating to 55 ℃, reacting for 7h, and cooling to obtain an intermediate 2; the dosage ratio of the vanillin, the acetone, the anhydrous sodium carbonate and the intermediate 1 is 0.8 mol: 400 mL: 90 g: 0.81 mol;
step S3: adding the intermediate 2 and furfuryl amine into a flask filled with absolute ethyl alcohol, heating to 70 ℃, keeping the temperature, reacting for 5 hours, and standing at-4 ℃ for 12 hours to prepare a flame retardant; the dosage ratio of the intermediate 2, the furfuryl amine and the absolute ethyl alcohol is 0.1 mol: 0.23 mol: 150 mL.
Example 4
The flame-retardant wear-resistant plastic particle comprises the following raw materials in parts by weight: 40 parts of polyamide resin, 8.2 parts of glass fiber, 1.1 parts of calcium stearate, 2.3 parts of toughening agent, 3.5 parts of antioxidant, 0.5 part of coupling agent and 8.2 parts of flame retardant prepared in example 2;
the flame-retardant wear-resistant plastic particle is prepared by the following steps:
the method comprises the following steps: stirring and mixing polyamide resin, a toughening agent and a coupling agent at the rotation speed of 500r/min, then adding calcium stearate, an antioxidant and a flame retardant, and mixing at the rotation speed of 200r/min to obtain a first material;
step two: and adding the first material and glass fiber into a double-screw extruder, setting the rotating speed of the screws to be 300r/min and the temperature to be 150 ℃, and extruding and granulating to obtain the flame-retardant wear-resistant plastic particles.
Example 5
The flame-retardant wear-resistant plastic particle comprises the following raw materials in parts by weight: 50 parts of polyamide resin, 9.3 parts of glass fiber, 1.4 parts of calcium stearate, 3.3 parts of toughening agent, 5.6 parts of antioxidant, 0.9 part of coupling agent and 9.2 parts of flame retardant prepared in example 2;
the flame-retardant wear-resistant plastic particle is prepared by the following steps:
the method comprises the following steps: stirring and mixing polyamide resin, a toughening agent and a coupling agent at the rotating speed of 500r/min, then adding calcium stearate, an antioxidant and a flame retardant, and mixing at the rotating speed of 300r/min to obtain a first material;
step two: and adding the first material and glass fiber into a double-screw extruder, setting the screw rotation speed at 300r/min and the temperature at 175 ℃, and extruding and granulating to obtain the flame-retardant wear-resistant plastic particles.
Example 6
The flame-retardant wear-resistant plastic particle comprises the following raw materials in parts by weight: 60 parts of polyamide resin, 10.4 parts of glass fiber, 1.7 parts of calcium stearate, 4.3 parts of toughening agent, 7.7 parts of antioxidant, 1.3 parts of coupling agent and 10.2 parts of flame retardant prepared in example 2;
the flame-retardant wear-resistant plastic particle is prepared by the following steps:
the method comprises the following steps: stirring and mixing polyamide resin, a toughening agent and a coupling agent at the rotating speed of 500r/min, then adding calcium stearate, an antioxidant and a flame retardant, and mixing at the rotating speed of 400r/min to obtain a first material;
step two: and adding the first material and glass fiber into a double-screw extruder, setting the rotating speed of the screws at 300r/min and the temperature at 200 ℃, and extruding and granulating to obtain the flame-retardant wear-resistant plastic particles.
Comparative example 1: no flame retardant was added compared to example 5.
Comparative example 2: intermediate 2 prepared in example 2 was added as a flame retardant compared to example 5.
Comparative example 3: example 1 of the patent application No. 201610828315.4.
The examples 4 to 6 and comparative examples 1 to 3 were subjected to the performance test, the flame retardancy was measured in accordance with UL94 standard using a horizontal/vertical flame tester, and the heat distortion temperature was measured in accordance with GB/T1634.2-2004, and the results were as shown in the following table:
it can be seen from the above table that examples 4-6 have good flame retardant properties.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. The flame-retardant wear-resistant plastic particle is characterized by comprising the following raw materials in parts by weight: 40-60 parts of polyamide resin, 8.2-10.4 parts of glass fiber, 1.1-1.7 parts of calcium stearate, 2.3-4.3 parts of toughening agent, 3.5-7.7 parts of antioxidant, 0.5-1.3 parts of coupling agent and 8.2-10.2 parts of flame retardant;
the flame retardant is prepared by the following steps:
step S1: adding carbazole and tetrahydrofuran into a flask, then adding sodium hydride, stirring for 30min at room temperature, then heating to 60 ℃, adding phosphorus oxychloride, and carrying out reflux reaction for 2-3h to obtain an intermediate 1;
step S2: adding vanillin, acetone and anhydrous sodium carbonate into a flask, introducing nitrogen, stirring for 1h, adding the intermediate 1, heating to 55 ℃, and reacting for 6-7h to obtain an intermediate 2;
step S3: adding the intermediate 2 and furfuryl amine into a flask filled with absolute ethyl alcohol, heating to 70 ℃, preserving heat, reacting for 5 hours, and standing at-4 ℃ for 12 hours to obtain the flame retardant.
2. The flame-retardant wear-resistant plastic particles as claimed in claim 1, wherein in step S1, the amount ratio of carbazole, tetrahydrofuran, sodium hydride and phosphorus oxychloride is 0.011 mol: 20mL of: 0.022 mol: 0.01 mol.
3. The flame-retardant wear-resistant plastic granules according to claim 1, wherein the amount ratio of vanillin, acetone, anhydrous sodium carbonate and intermediate 1 in step S2 is 0.8 mol: 400 mL: 90 g: 0.81 mol.
4. The flame-retardant wear-resistant plastic particle as claimed in claim 1, wherein the ratio of the intermediate 2, the furfuryl amine and the absolute ethyl alcohol in step S3 is 0.1 mol: 0.23 mol: 150 mL.
5. The flame retardant and wear resistant plastic granules according to claim 1, wherein the toughening agent is an ethylene-octene copolymer or an ethylene-vinyl acetate copolymer.
6. The flame-retardant wear-resistant plastic particle as claimed in claim 1, wherein the antioxidant is any one of hindered phenolic, hindered amine and phosphite antioxidants.
7. The flame retardant, abrasion resistant plastic granules according to claim 1, wherein said coupling agent is a silane coupling agent.
8. The processing technology of the flame-retardant wear-resistant plastic particles as claimed in claim 1, which is characterized by comprising the following steps:
the method comprises the following steps: stirring and mixing polyamide resin, a toughening agent and a coupling agent at the rotation speed of 500r/min, then adding calcium stearate, an antioxidant and a flame retardant, and mixing at the rotation speed of 200 and 400r/min to obtain a first material;
step two: and adding the material I and the glass fiber into a double-screw extruder, setting the rotating speed of the screw at 300r/min and the temperature at 150-.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116410227A (en) * | 2023-04-03 | 2023-07-11 | 上海辉纳思光电科技有限公司 | Phosphonic acid derivative of carbazole, quantum dot light emitting device and perovskite solar cell |
| CN116410227B (en) * | 2023-04-03 | 2024-05-14 | 上海辉纳思光电科技有限公司 | Phosphonic acid derivative of carbazole, quantum dot light emitting device and perovskite solar cell |
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| CN113121906A (en) * | 2021-05-27 | 2021-07-16 | 湛宗鉴 | Wear-resistant flame-retardant plastic and preparation method thereof |
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| CN116410227A (en) * | 2023-04-03 | 2023-07-11 | 上海辉纳思光电科技有限公司 | Phosphonic acid derivative of carbazole, quantum dot light emitting device and perovskite solar cell |
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