CN114456497A - Preparation method of antistatic high-strength PP material - Google Patents
Preparation method of antistatic high-strength PP material Download PDFInfo
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- CN114456497A CN114456497A CN202210286051.XA CN202210286051A CN114456497A CN 114456497 A CN114456497 A CN 114456497A CN 202210286051 A CN202210286051 A CN 202210286051A CN 114456497 A CN114456497 A CN 114456497A
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- 239000000463 material Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000004743 Polypropylene Substances 0.000 claims abstract description 136
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 89
- 229920000570 polyether Polymers 0.000 claims abstract description 89
- 150000002148 esters Chemical class 0.000 claims abstract description 85
- -1 silicon quaternary ammonium salt Chemical class 0.000 claims abstract description 83
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 81
- 238000006243 chemical reaction Methods 0.000 claims abstract description 70
- 239000000203 mixture Substances 0.000 claims abstract description 55
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000002216 antistatic agent Substances 0.000 claims abstract description 47
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 45
- 239000010703 silicon Substances 0.000 claims abstract description 45
- 229920001155 polypropylene Polymers 0.000 claims abstract description 36
- 239000002131 composite material Substances 0.000 claims abstract description 35
- OXYZDRAJMHGSMW-UHFFFAOYSA-N 3-chloropropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCCl OXYZDRAJMHGSMW-UHFFFAOYSA-N 0.000 claims abstract description 29
- CRVGTESFCCXCTH-UHFFFAOYSA-N methyl diethanolamine Chemical compound OCCN(C)CCO CRVGTESFCCXCTH-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000002994 raw material Substances 0.000 claims abstract description 29
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000003495 polar organic solvent Substances 0.000 claims abstract description 9
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000001125 extrusion Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000003054 catalyst Substances 0.000 claims abstract description 3
- 239000002904 solvent Substances 0.000 claims description 26
- 239000012046 mixed solvent Substances 0.000 claims description 18
- 238000001746 injection moulding Methods 0.000 claims description 14
- 230000035484 reaction time Effects 0.000 claims description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- 229920000728 polyester Polymers 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 3
- 229920001577 copolymer Polymers 0.000 claims description 2
- 229920001707 polybutylene terephthalate Polymers 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- 238000005956 quaternization reaction Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 abstract description 13
- 238000010438 heat treatment Methods 0.000 abstract description 12
- 239000007788 liquid Substances 0.000 abstract description 12
- 238000002390 rotary evaporation Methods 0.000 abstract description 12
- 230000007547 defect Effects 0.000 abstract description 3
- 239000002344 surface layer Substances 0.000 abstract description 2
- 239000008187 granular material Substances 0.000 description 13
- 238000010008 shearing Methods 0.000 description 13
- 230000015572 biosynthetic process Effects 0.000 description 12
- 238000002844 melting Methods 0.000 description 12
- 230000008018 melting Effects 0.000 description 12
- 238000003786 synthesis reaction Methods 0.000 description 12
- 238000005303 weighing Methods 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 8
- 239000011159 matrix material Substances 0.000 description 4
- 230000002195 synergetic effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920006228 ethylene acrylate copolymer Polymers 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
Classifications
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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
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/017—Additives being an antistatic agent
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/04—Antistatic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention belongs to the technical field of PP materials, and discloses a preparation method of an antistatic high-strength PP material. The preparation method of the antistatic high-strength PP material comprises the following steps: (1) putting N-methyldiethanolamine and gamma-chloropropyltrimethoxysilane in a reaction kettle, heating with potassium iodide as a catalyst and isopropanol and methanol as polar organic solvents to dissolve and uniformly mix the raw materials, transferring the mixture to a microwave reaction device, cooling, standing, separating liquid and performing rotary evaporation after the reaction is finished to obtain organosilicon quaternary ammonium salt; (2) firstly, drying the high-molecular antistatic agent polyether ester and the obtained organic silicon quaternary ammonium salt, then uniformly mixing the high-molecular antistatic agent polyether ester and the obtained organic silicon quaternary ammonium salt with PP (polypropylene), and carrying out melt blending and extrusion molding in a double-screw extruder to obtain the antistatic high-strength polypropylene composite material. According to the method, the macromolecular antistatic agent and the micromolecular antistatic agent are added, so that the antistatic performance is improved from the two aspects of the bulk phase and the surface layer of the polypropylene, and the defect of insufficient antistatic performance of the polypropylene material is overcome.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a preparation method of an antistatic high-strength PP material.
Background
Polypropylene is a general-purpose plastic with excellent characteristics of light weight, corrosion resistance, high temperature resistance and the like, and is widely applied to the fields of electronic devices, medical treatment, automobile industry and the like. However, polypropylene has good insulation property, charges are easily accumulated on the surface of the polypropylene through friction, accumulated static charges easily adsorb dust, the attractiveness of the PP product is affected, even fire and explosion can be caused when the PP product is serious, and the rapid development of the PP product is greatly limited. In order to improve the service performance of the PP material and further expand the application range of the PP material, a new antistatic high-strength PP product is needed to meet the market demand.
The antistatic agent is added into the PP material, and the surface polar groups absorb moisture in the air to form a conductive layer by improving the surface hydrophilicity of the PP material, so that the leakage of accumulated static charges can be accelerated, the antistatic capability of the PP material is improved, and the preparation method is one of preparation methods of the antistatic PP material. The invention discloses a long-acting antistatic PP material and a preparation method thereof, and a Chinese invention patent (application number: 201811629424.9) discloses that a permanent antistatic PP material is obtained by adding a macromolecular antistatic agent ethylene-acrylate copolymer into the PP material. However, the antistatic agent is used in a large amount in the patent technology, and when 50 parts of the antistatic agent is added, the surface resistivity of the PP material reaches 5.05 multiplied by 108Omega/sq, and the addition of a large amount of antistatic materials not only increases the production cost, but also influences the mechanical properties of PP materials.
Disclosure of Invention
The invention aims to overcome the defects of the background technology and provide a preparation method of an antistatic high-strength PP material. According to the method, the macromolecular antistatic agent and the micromolecular antistatic agent are added, so that the antistatic performance is improved from the two aspects of the bulk phase and the surface layer of the polypropylene, and the defect of insufficient antistatic performance of the polypropylene material is overcome.
Specifically, polyether ester high-molecular antistatic agents with different molecular weights are blended with polypropylene, and the high-molecular antistatic agents form a network structure in a polypropylene matrix by regulating and controlling parameters such as flowability, polarity and the like of the high-molecular antistatic agents, so that the antistatic performance of a polypropylene material can be improved, and meanwhile, the tensile strength and the impact strength of the polypropylene can be obviously improved due to strong acting force among molecules of the high-molecular antistatic agents. The antistatic effect of the macromolecular antistatic agent is not as good as that of the micromolecular antistatic agent, so that the micromolecular antistatic agent is further added into the polypropylene on the basis that the macromolecular antistatic agent forms a network structure in the polypropylene matrix, and the micromolecular antistatic agent tends to be distributed on the surface of the polypropylene material, so that the polypropylene has good surface antistatic performance. Therefore, the antistatic high-strength polypropylene material is obtained by using the macromolecular antistatic agent and the micromolecular antistatic agent in a synergistic manner.
In order to achieve the purpose of the invention, the preparation method of the antistatic high-strength PP material comprises the following steps:
(1) n-methyldiethanolamine and gamma-chloropropyltrimethoxysilane are used as raw materials to synthesize the organosilicon quaternary ammonium salt through quaternization, and the specific process comprises the following steps:
more specifically, N-methyldiethanolamine and gamma-chloropropyltrimethoxysilane are placed in a reaction kettle, potassium iodide is used as a catalyst, a mixed solvent of isopropanol and methanol is used as a polar organic solvent, the mixture is heated to dissolve and uniformly mix the added raw materials, then the mixture is transferred to a microwave reaction device for reaction, and after the reaction is finished, the mixture is cooled, kept stand, separated and steamed in a rotating mode to obtain organic silicon quaternary ammonium salt;
(2) firstly, drying the high-molecular antistatic agent polyether ester and the organic silicon quaternary ammonium salt obtained in the step (1), then uniformly mixing with PP, and carrying out melt blending and extrusion molding in a double-screw extruder to obtain the antistatic high-strength polypropylene composite material.
Further, in some embodiments of the present invention, the material ratio in the step (1) is n (γ -chloropropyltrimethoxysilane): n (N-methyldiethanolamine) ═ 1.0 to 1.5: 1.0.
further, in some embodiments of the present invention, in the step (1), the amount ratio of the solvent is m (solvent): m (raw material) ═ 0.5-1.0: 1.0.
further, in some embodiments of the present invention, the mass ratio of isopropanol to methanol in the step (1) is 1.0 to 3.0: 1.0.
further, in some embodiments of the present invention, the reaction time in step (1) is 8 to 16 hours.
Further, in some embodiments of the present invention, the reaction temperature in step (1) is 120-.
Further, in some embodiments of the present invention, the microwave power in step (1) is 500-.
Further, in some embodiments of the present invention, the polyether ester in step (2) is a copolymer composed of polyester and polyether, the polyester is polybutylene terephthalate, and the polyether is a polymer of ethylene glycol.
Preferably, in some embodiments of the present invention, the molecular weight of the polyether ester in the step (2) is 1000-50000. One or more of polyether esters with different molecular weights can be added in the step (2), wherein the mass ratio of polyether ester with the molecular weight of 1000 to polyether ester with the molecular weight of 10000 to polyether ester with the molecular weight of 50000 is 1-4: 3-4: 0-3, the optimal ratio is polyether ester with the molecular weight of 1000 to 10000, and the molecular weight of 50000 to 1: 1: 1.
further, in some embodiments of the present invention, the mass ratio of the polyether ester, the silicone quaternary ammonium salt and the PP in the step (2) is 4-12: 0.8-5: 86-96, preferably 9: 5: 86.
further, in some embodiments of the present invention, the drying temperature in the step (2) is 80 to 120 ℃, and the drying time is 1 to 5 hours.
Further, in some embodiments of the present invention, in the step (2), the extrusion temperature of the twin-screw extruder is 160-.
Compared with the prior art, the invention has the following advantages:
(1) the invention utilizes the synergistic effect of the macromolecular antistatic agent and the micromolecular antistatic agent to improve the antistatic property of the PP composite material, so that the PP composite material reaches or even is superior to the quality of similar products.
(2) The polyether ester high-molecular antistatic agent adopted by the invention forms a network structure in a polypropylene matrix, and the mechanical property of the PP composite material is improved.
(3) The price of the polymer antistatic agent used in the invention is low, the synthesis process of the organosilicon quaternary ammonium salt is simple, the cost is low, and the preparation process of the antistatic high-strength PP composite material is simple, thereby being beneficial to industrial production.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention. It is to be understood that the following description is only illustrative of the present invention and is not to be construed as limiting the present invention.
The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "either" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
The indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the number clearly indicates the singular.
Furthermore, the description below of the terms "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., means 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 are not necessarily intended to refer to the same embodiment or example. Further, the technical features of the embodiments of the present invention may be combined with each other as long as they do not conflict with each other.
Example 1
(1) And (3) synthesis of organosilicon quaternary ammonium salt: weighing certain amounts of N-methyldiethanolamine and gamma-chloropropyltrimethoxysilane [ N (gamma-chloropropyltrimethoxysilane) ], wherein N (N-methyldiethanolamine) ═ 1.2: 1.0] adding the mixture into a high-pressure reaction kettle, adding a mixed solvent of isopropanol and methanol, wherein the dosage of the solvent is m (solvent): m (raw material): 0.8:1.0 and m (isopropanol): m (methanol): 1.0), and the mixed solvent is a polar organic solvent, heating to dissolve and mix the added raw materials uniformly, transferring the mixture to a microwave reaction device, setting the microwave power to be 800W, the reaction time to be 12h and the reaction temperature to be 170 ℃, cooling, standing, separating liquid and carrying out rotary evaporation after the reaction is finished, and obtaining the organic silicon quaternary ammonium salt.
(2) Preparing an antistatic high-strength polypropylene material: the polyether ester and the organic silicon quaternary ammonium salt are firstly treated in an oven at 100 ℃ for 3 hours, then the polyether ester (2 wt% of polyether ester with the molecular weight of 1000, 3 wt% of polyether ester with the molecular weight of 10000 and 2 wt% of polyether ester with the molecular weight of 50000), 1 wt% of organic silicon quaternary ammonium salt and 91 wt% of PP are mixed for 30 minutes in a high-speed mixer at the rotating speed of 800r/min, and then the mixture is placed in a double-screw extruder at the temperature of 170-210 ℃ and the rotating speed of 60 r/min. Under the action of screw shearing and heat, the PP, the high-molecular antistatic agent polyether ester and the organic silicon quaternary ammonium salt are further subjected to melting reaction, conveyed to the head of an extruder, extruded, cooled, dried and granulated to obtain the antistatic high-strength PP composite material granules. And (3) obtaining the required sample strip from the antistatic high-strength PP composite material in an injection molding machine at 170-200 ℃.
Example 2
(1) Synthesis of organosilicon quaternary ammonium salt: weighing certain amounts of N-methyldiethanolamine and gamma-chloropropyltrimethoxysilane [ N (gamma-chloropropyltrimethoxysilane) ], wherein N (N-methyldiethanolamine) ═ 1.2: 1.0] adding the mixture into a high-pressure reaction kettle, adding a mixed solvent of isopropanol and methanol, wherein the dosage of the solvent is m (solvent), m (raw material) is 1.0:1.0, and m (isopropanol) is m (methanol) is 1.0:1.0, heating to dissolve and mix the added raw materials uniformly, transferring the mixture to a microwave reaction device, setting the microwave power to be 800W, the reaction time to be 12h and the reaction temperature to be 170 ℃, cooling, standing, separating liquid and carrying out rotary evaporation after the reaction is finished, and obtaining the organic silicon quaternary ammonium salt.
(2) Preparing an antistatic high-strength polypropylene material: the polyether ester and the organic silicon quaternary ammonium salt are firstly treated in an oven at 100 ℃ for 3 hours, then the polyether ester (1 weight percent of polyether ester with the molecular weight of 1000, 3 weight percent of polyether ester with the molecular weight of 10000 and 1 weight percent of polyether ester with the molecular weight of 50000), 2 weight percent of organic silicon quaternary ammonium salt and 93 weight percent of PP are mixed for 30 minutes in a high-speed mixer at the rotating speed of 800r/min, and then the mixture is placed in a double-screw extruder at the temperature of 170-210 ℃ and the rotating speed of 60 r/min. Under the action of screw shearing and heat, the PP, the high-molecular antistatic agent polyether ester and the organic silicon quaternary ammonium salt are further subjected to melting reaction, conveyed to the head of an extruder, extruded, cooled, dried and granulated to obtain the antistatic high-strength PP composite material granules. And (3) obtaining the required sample strip from the antistatic high-strength PP composite material in an injection molding machine at 170-200 ℃.
Example 3
(1) Synthesis of organosilicon quaternary ammonium salt: weighing certain amounts of N-methyldiethanolamine and gamma-chloropropyltrimethoxysilane [ N (gamma-chloropropyltrimethoxysilane) ], wherein the weight ratio of N (N-methyldiethanolamine) ═ 1.0:1.0] adding the mixture into a high-pressure reaction kettle, adding a mixed solvent of isopropanol and methanol, wherein the dosage of the solvent is m (solvent), m (raw material) is 1.0:1.0, and m (isopropanol) is m (methanol) is 1.0:1.0, heating to dissolve and mix the added raw materials uniformly, transferring the mixture to a microwave reaction device, setting the microwave power to be 800W, the reaction time to be 12h and the reaction temperature to be 170 ℃, cooling, standing, separating liquid and carrying out rotary evaporation after the reaction is finished, and obtaining the organic silicon quaternary ammonium salt.
(2) Preparing an antistatic high-strength polypropylene material: the polyether ester and the organic silicon quaternary ammonium salt are firstly treated in an oven at 100 ℃ for 3 hours, then the polyether ester (1 weight percent of polyether ester with the molecular weight of 1000, 3 weight percent of polyether ester with the molecular weight of 10000 and 2 weight percent of polyether ester with the molecular weight of 50000), 2 weight percent of organic silicon quaternary ammonium salt and 92 weight percent of PP are mixed for 30 minutes in a high-speed mixer at the rotating speed of 800r/min, and then the mixture is placed in a double-screw extruder at the temperature of 170-210 ℃ and the rotating speed of 60 r/min. Under the action of screw shearing and heat, the PP, the high-molecular antistatic agent polyether ester and the organosilicon quaternary ammonium salt are further subjected to a melting reaction, conveyed to the head of an extruder, extruded, cooled, dried and granulated to obtain the antistatic high-strength PP composite material granules. And (3) obtaining the required sample strip from the antistatic high-strength PP composite material in an injection molding machine at 170-200 ℃.
Example 4
(1) Synthesis of organosilicon quaternary ammonium salt: weighing certain amounts of N-methyldiethanolamine and gamma-chloropropyltrimethoxysilane [ N (gamma-chloropropyltrimethoxysilane) ], wherein the weight ratio of N (N-methyldiethanolamine) ═ 1.0:1.0] adding the mixture into a high-pressure reaction kettle, adding a mixed solvent of isopropanol and methanol, wherein the dosage of the solvent is m (solvent): m (raw material): 0.8:1.0 and m (isopropanol): m (methanol): 1.0), and the mixed solvent is a polar organic solvent, heating to dissolve and mix the added raw materials uniformly, transferring the mixture to a microwave reaction device, setting the microwave power to be 800W, the reaction time to be 12h and the reaction temperature to be 170 ℃, cooling, standing, separating liquid and carrying out rotary evaporation after the reaction is finished, and obtaining the organic silicon quaternary ammonium salt.
(2) Preparing an antistatic high-strength polypropylene material: the polyether ester and the organic silicon quaternary ammonium salt are firstly treated in an oven at 100 ℃ for 3 hours, then the polyether ester (4 wt% of polyether ester with the molecular weight of 1000 and 4 wt% of polyether ester with the molecular weight of 10000), the organic silicon quaternary ammonium salt and the PP (91 wt%) are mixed for 30 minutes in a high-speed mixer at the rotating speed of 800r/min, and then the mixture is placed in a double-screw extruder at the temperature of 170-210 ℃ and the rotating speed of 60 r/min. Under the action of screw shearing and heat, the PP, the high-molecular antistatic agent polyether ester and the organic silicon quaternary ammonium salt are further subjected to melting reaction, conveyed to the head of an extruder, extruded, cooled, dried and granulated to obtain the antistatic high-strength PP composite material granules. And (3) obtaining the required sample strip from the antistatic high-strength PP composite material in an injection molding machine at 170-200 ℃.
Example 5
(1) Synthesis of organosilicon quaternary ammonium salt: weighing certain amounts of N-methyldiethanolamine and gamma-chloropropyltrimethoxysilane [ N (gamma-chloropropyltrimethoxysilane) ], wherein N (N-methyldiethanolamine) ═ 1.5: 1.0] adding the mixture into a high-pressure reaction kettle, adding a mixed solvent of isopropanol and methanol, wherein the dosage of the solvent is m (solvent), m (raw material) is 1.0:1.0, and m (isopropanol) is m (methanol) is 1.0:1.0, heating to dissolve and mix the added raw materials uniformly, transferring the mixture to a microwave reaction device, setting the microwave power to be 800W, the reaction time to be 12h and the reaction temperature to be 170 ℃, cooling, standing, separating liquid and carrying out rotary evaporation after the reaction is finished, and obtaining the organic silicon quaternary ammonium salt.
(2) Preparing an antistatic high-strength polypropylene material: the polyether ester and the organic silicon quaternary ammonium salt are firstly treated in an oven at 100 ℃ for 3 hours, then the polyether ester (1 weight percent of polyether ester with the molecular weight of 1000, 3 weight percent of polyether ester with the molecular weight of 10000 and 3 weight percent of polyether ester with the molecular weight of 50000), 2 weight percent of organic silicon quaternary ammonium salt and 91 weight percent of PP are mixed for 30 minutes in a high-speed mixer at the rotating speed of 800r/min, and then the mixture is placed in a double-screw extruder at the temperature of 170-210 ℃ and the rotating speed of 60 r/min. Under the action of screw shearing and heat, the PP, the high-molecular antistatic agent polyether ester and the organic silicon quaternary ammonium salt are further subjected to melting reaction, conveyed to the head of an extruder, extruded, cooled, dried and granulated to obtain the antistatic high-strength PP composite material granules. And (3) obtaining the required sample strip from the antistatic high-strength PP composite material in an injection molding machine at 170-200 ℃.
Example 6
(1) Synthesis of organosilicon quaternary ammonium salt: weighing certain amounts of N-methyldiethanolamine and gamma-chloropropyltrimethoxysilane [ N (gamma-chloropropyltrimethoxysilane) ], wherein N (N-methyldiethanolamine) ═ 1.5: 1.0] adding the mixture into a high-pressure reaction kettle, adding a mixed solvent of isopropanol and methanol, wherein the dosage of the solvent is m (solvent): m (raw material): 0.8:1.0 and m (isopropanol): m (methanol): 1.0), and the mixed solvent is a polar organic solvent, heating to dissolve and mix the added raw materials uniformly, transferring the mixture to a microwave reaction device, setting the microwave power to be 800W, the reaction time to be 12h and the reaction temperature to be 170 ℃, cooling, standing, separating liquid and carrying out rotary evaporation after the reaction is finished, and obtaining the organic silicon quaternary ammonium salt.
(2) Preparing an antistatic high-strength polypropylene material: the polyether ester and the organic silicon quaternary ammonium salt are firstly treated in an oven at 100 ℃ for 3 hours, then the polyether ester (3 weight percent of polyether ester with the molecular weight of 1000, 4 weight percent of polyether ester with the molecular weight of 10000 and 3 weight percent of polyether ester with the molecular weight of 50000) with the mass fraction of 10 weight percent, the organic silicon quaternary ammonium salt and the PP with the mass fraction are mixed for 30 minutes in a high-speed mixer with the rotating speed of 800r/min, and then the mixture is placed in a double-screw extruder with the temperature of 170-210 ℃ and the rotating speed of 60 r/min. Under the action of screw shearing and heat, the PP, the high-molecular antistatic agent polyether ester and the organic silicon quaternary ammonium salt are further subjected to melting reaction, conveyed to the head of an extruder, extruded, cooled, dried and granulated to obtain the antistatic high-strength PP composite material granules. And (3) obtaining the required sample strip from the antistatic high-strength PP composite material in an injection molding machine at 170-200 ℃.
Example 7
(1) And (3) synthesis of organosilicon quaternary ammonium salt: weighing certain amounts of N-methyldiethanolamine and gamma-chloropropyltrimethoxysilane [ N (gamma-chloropropyltrimethoxysilane) ], wherein N (N-methyldiethanolamine) ═ 1.3: 1.0] adding the mixture into a high-pressure reaction kettle, adding a mixed solvent of isopropanol and methanol, wherein the dosage of the solvent is m (solvent), m (raw material) is 1.0:1.0, and m (isopropanol) is m (methanol) is 1.0:1.0, heating to dissolve and mix the added raw materials uniformly, transferring the mixture to a microwave reaction device, setting the microwave power to be 800W, the reaction time to be 12h and the reaction temperature to be 170 ℃, cooling, standing, separating liquid and carrying out rotary evaporation after the reaction is finished, and obtaining the organic silicon quaternary ammonium salt.
(2) Preparing an antistatic high-strength polypropylene material: the polyether ester and the organic silicon quaternary ammonium salt are firstly treated in an oven at 100 ℃ for 3 hours, then the polyether ester (3 weight percent of polyether ester with the molecular weight of 1000, 3 weight percent of polyether ester with the molecular weight of 10000 and 3 weight percent of polyether ester with the molecular weight of 50000) with the mass fraction of 9 weight percent, the organic silicon quaternary ammonium salt and the PP with the mass fraction are mixed for 30 minutes in a high-speed mixer with the rotating speed of 800r/min, and then the mixture is placed in a double-screw extruder with the temperature of 170-210 ℃ and the rotating speed of 60 r/min. Under the action of screw shearing and heat, the PP, the high-molecular antistatic agent polyether ester and the organic silicon quaternary ammonium salt are further subjected to melting reaction, conveyed to the head of an extruder, extruded, cooled, dried and granulated to obtain the antistatic high-strength PP composite material granules. And (3) obtaining the required sample strip from the antistatic high-strength PP composite material in an injection molding machine at 170-200 ℃.
Example 8
(1) Synthesis of organosilicon quaternary ammonium salt: weighing certain amounts of N-methyldiethanolamine and gamma-chloropropyltrimethoxysilane [ N (gamma-chloropropyltrimethoxysilane) ], wherein N (N-methyldiethanolamine) ═ 1.3: 1.0] adding the mixture into a high-pressure reaction kettle, adding a mixed solvent of isopropanol and methanol, wherein the using amount of the solvent is m (solvent): m (raw material): 0.8:1.0, and m (isopropanol): m (methanol): 1.0, as a polar organic solvent, heating to dissolve and uniformly mix the added raw materials, transferring the mixture to a microwave reaction device, setting the microwave power at 800W, the reaction time at 12h and the reaction temperature at 170 ℃, cooling, standing, liquid separation and rotary evaporation after the reaction is finished, and obtaining the organic silicon quaternary ammonium salt.
(2) Preparing an antistatic high-strength polypropylene material: the polyether ester and the organic silicon quaternary ammonium salt are firstly treated in an oven at 100 ℃ for 3 hours, then the polyether ester (3 weight percent of polyether ester with the molecular weight of 1000, 3 weight percent of polyether ester with the molecular weight of 10000 and 3 weight percent of polyether ester with the molecular weight of 50000), 5 weight percent of organic silicon quaternary ammonium salt and 86 weight percent of PP are mixed for 30 minutes in a high-speed mixer at the rotating speed of 800r/min, and then the mixture is placed in a double-screw extruder at the temperature of 170-210 ℃ and the rotating speed of 60 r/min. Under the action of screw shearing and heat, the PP, the high-molecular antistatic agent polyether ester and the organic silicon quaternary ammonium salt are further subjected to melting reaction, conveyed to the head of an extruder, extruded, cooled, dried and granulated to obtain the antistatic high-strength PP composite material granules. And (3) obtaining the required sample strip from the antistatic high-strength PP composite material in an injection molding machine at 170-200 ℃.
Example 9
(1) Synthesis of organosilicon quaternary ammonium salt: weighing certain amounts of N-methyldiethanolamine and gamma-chloropropyltrimethoxysilane [ N (gamma-chloropropyltrimethoxysilane) ], wherein the weight ratio of N (N-methyldiethanolamine) ═ 1.4: 1.0] adding the mixture into a high-pressure reaction kettle, adding a mixed solvent of isopropanol and methanol, wherein the dosage of the solvent is m (solvent), m (raw material) is 1.0:1.0, and m (isopropanol) is m (methanol) is 1.0:1.0, heating to dissolve and mix the added raw materials uniformly, transferring the mixture to a microwave reaction device, setting the microwave power to be 800W, the reaction time to be 12h and the reaction temperature to be 170 ℃, cooling, standing, separating liquid and carrying out rotary evaporation after the reaction is finished, and obtaining the organic silicon quaternary ammonium salt.
(2) Preparing an antistatic high-strength polypropylene material: the polyether ester and the organic silicon quaternary ammonium salt are firstly treated in an oven at 100 ℃ for 3 hours, then the polyether ester (1 weight percent of polyether ester with the molecular weight of 1000, 2 weight percent of polyether ester with the molecular weight of 10000 and 1 weight percent of polyether ester with the molecular weight of 50000), the organic silicon quaternary ammonium salt and the PP with the mass fraction of 4 weight percent are mixed for 30 minutes in a high-speed mixer with the rotating speed of 800r/min, and then the mixture is placed in a double-screw extruder with the temperature of 170-210 ℃ and the rotating speed of 60 r/min. Under the action of screw shearing and heat, the PP, the high-molecular antistatic agent polyether ester and the organic silicon quaternary ammonium salt are further subjected to melting reaction, conveyed to the head of an extruder, extruded, cooled, dried and granulated to obtain the antistatic high-strength PP composite material granules. And (3) obtaining the required sample strip from the antistatic high-strength PP composite material in an injection molding machine at 170-200 ℃.
Example 10
(1) Synthesis of organosilicon quaternary ammonium salt: weighing certain amounts of N-methyldiethanolamine and gamma-chloropropyltrimethoxysilane [ N (gamma-chloropropyltrimethoxysilane) ], wherein the weight ratio of N (N-methyldiethanolamine) ═ 1.4: 1.0] adding the mixture into a high-pressure reaction kettle, adding a mixed solvent of isopropanol and methanol, wherein the dosage of the solvent is m (solvent): m (raw material): 0.8:1.0 and m (isopropanol): m (methanol): 1.0), and the mixed solvent is a polar organic solvent, heating to dissolve and mix the added raw materials uniformly, transferring the mixture to a microwave reaction device, setting the microwave power to be 800W, the reaction time to be 12h and the reaction temperature to be 170 ℃, cooling, standing, separating liquid and carrying out rotary evaporation after the reaction is finished, and obtaining the organic silicon quaternary ammonium salt.
(2) Preparing an antistatic high-strength polypropylene material: the polyether ester and the organic silicon quaternary ammonium salt are firstly treated in an oven at 100 ℃ for 3 hours, then the polyether ester (2 wt% of polyether ester with the molecular weight of 1000, 3 wt% of polyether ester with the molecular weight of 10000 and 2 wt% of polyether ester with the molecular weight of 50000), 3 wt% of organic silicon quaternary ammonium salt and 89 wt% of PP are mixed for 30 minutes in a high-speed mixer at the rotating speed of 800r/min, and then the mixture is placed in a double-screw extruder at the temperature of 170-210 ℃ and the rotating speed of 60 r/min. Under the action of screw shearing and heat, the PP, the high-molecular antistatic agent polyether ester and the organic silicon quaternary ammonium salt are further subjected to melting reaction, conveyed to the head of an extruder, extruded, cooled, dried and granulated to obtain the antistatic high-strength PP composite material granules. And (3) obtaining the required sample strip from the antistatic high-strength PP composite material in an injection molding machine at 170-200 ℃.
Comparative example 1
And (3) placing the PP into a double-screw extruder with the temperature of 170-210 ℃ and the rotating speed of 60 r/min. And under the action of screw shearing and heat, further carrying out melt reaction on the PP, conveying the PP to the head of an extruder, and carrying out extrusion, cooling, drying and grain cutting on the PP to obtain PP material granules. And (3) obtaining the needed sample strip from the PP material in an injection molding machine at 170-200 ℃.
Comparative example 2
(1) Synthesis of organosilicon quaternary ammonium salt: weighing certain amounts of N-methyldiethanolamine and gamma-chloropropyltrimethoxysilane [ N (gamma-chloropropyltrimethoxysilane) ], wherein N (N-methyldiethanolamine) ═ 1.2: 1.0] adding the mixture into a high-pressure reaction kettle, adding a mixed solvent of isopropanol and methanol, wherein the dosage of the solvent is m (solvent): m (raw material): 0.8:1.0 and m (isopropanol): m (methanol): 1.0), and the mixed solvent is a polar organic solvent, heating to dissolve and mix the added raw materials uniformly, transferring the mixture to a microwave reaction device, setting the microwave power to be 800W, the reaction time to be 12h and the reaction temperature to be 170 ℃, cooling, standing, separating liquid and carrying out rotary evaporation after the reaction is finished, and obtaining the organic silicon quaternary ammonium salt.
(2) Preparing an antistatic high-strength polypropylene material: the organosilicon quaternary ammonium salt is firstly treated in an oven at 100 ℃ for 3 hours, then 1 wt% of organosilicon quaternary ammonium salt and 99 wt% of PP are mixed for 30 minutes in a high-speed mixer at the rotating speed of 800r/min, and then the mixture is placed in a double-screw extruder at the temperature of 170-210 ℃ and the rotating speed of 60 r/min. Under the action of screw shearing and heat, the PP and the organosilicon quaternary ammonium salt are further subjected to melting reaction, conveyed to the head of an extruder, extruded, cooled, dried and granulated to obtain the antistatic high-strength PP composite material granules. And (3) obtaining the required sample strip from the antistatic high-strength PP composite material in an injection molding machine at 170-200 ℃.
Comparative example 3
Preparing an antistatic high-strength polypropylene material: the polyether ester is firstly treated in an oven at 100 ℃ for 3 hours, then polyether ester (2 weight percent of polyether ester with the molecular weight of 1000, polyether ester with the molecular weight of 3 weight percent of 10000 and polyether ester with the molecular weight of 2 weight percent of 50000) with the mass fraction of 8 weight percent and PP (92 weight percent) are mixed for 30 minutes in a high-speed mixer with the rotating speed of 800r/min, and then the mixture is placed in a double-screw extruder with the temperature of 170-210 ℃ and the rotating speed of 60 r/min. Under the action of screw shearing and heat, PP and the high-molecular antistatic agent polyether ester are further subjected to melting reaction, conveyed to the head of an extruder, extruded, cooled, dried and granulated to obtain the antistatic high-strength PP composite material granules. And (3) obtaining the required sample strip from the antistatic high-strength PP composite material in an injection molding machine at 170-200 ℃.
Performance test
The tensile strength of the material is carried out according to GB/T1040.1-2006, and the speed is 50 mm/min; the notch impact strength is carried out according to GB/T1043.1-2008, and the notch is V-shaped; the surface resistivity is in accordance with GB/T1410-2006 standard, PP surface resistivity test sample bar needs to be processed in a constant temperature and humidity box for 48h, the relative humidity is 65 +/-0.2%, and the temperature is 23 +/-0.2 ℃.
TABLE 1 tables of Properties of the materials of examples 1-10 and comparative examples 1-3
| Test item | Surface resistivity (omega/sq) | Tensile Strength (MPa) | Notched impact Strength at Normal temperature (kJ/m)2) |
| Example 1 | 8.21×109 | 55.8 | 12.3 |
| Example 2 | 5.39×108 | 49.4 | 10.8 |
| Example 3 | 3.56×108 | 42.9 | 9.2 |
| Example 4 | 9.37×109 | 47.6 | 9.9 |
| Example 5 | 1.26×108 | 43.6 | 9.5 |
| Example 6 | 9.39×108 | 51.7 | 10.4 |
| Example 7 | 3.59×109 | 50.6 | 10.6 |
| Example 8 | 1.07×107 | 56.5 | 13.5 |
| Example 9 | 3.34×107 | 52.3 | 11.1 |
| Example 10 | 8.96×107 | 50.3 | 11.7 |
| Comparative example 1 | 3.06×1016 | 28.1 | 3.5 |
| Comparative example 2 | 4.29×1010 | 29.7 | 6.9 |
| Comparative example 3 | 6.16×1012 | 41.9 | 9.1 |
According to the embodiment and the comparative example, the surface resistivity of the PP composite material is reduced by utilizing the macromolecular antistatic agent and the micromolecular antistatic agent, the antistatic property of the PP composite material is improved, and meanwhile, the mechanical property of the PP composite material is also improved. The tensile strength and the notch impact strength of the PA66 can be greatly improved by compounding the macromolecular antistatic agent and the micromolecular antistatic agent and independently using one of the macromolecular antistatic agent and the micromolecular antistatic agent, mainly because the macromolecular antistatic agent forms a network structure in a polypropylene matrix, the micromolecular antistatic agent tends to be distributed on the surface of a polypropylene material, the polypropylene material is endowed with good surface antistatic performance, and the antistatic high-strength PP composite material is obtained by synergistic use.
It will be understood by those skilled in the art that the foregoing is only exemplary of the present invention, and is not intended to limit the invention, which is intended to cover any variations, equivalents, or improvements therein, which fall within the spirit and scope of the invention.
Claims (10)
1. The preparation method of the antistatic high-strength PP material is characterized by comprising the following steps of:
(1) n-methyldiethanolamine and gamma-chloropropyltrimethoxysilane are used as raw materials to synthesize organosilicon quaternary ammonium salt through quaternization;
(2) firstly, drying the high-molecular antistatic agent polyether ester and the organic silicon quaternary ammonium salt obtained in the step (1), then uniformly mixing with PP, and carrying out melt blending and extrusion molding in a double-screw extruder to obtain the antistatic high-strength polypropylene composite material.
2. The preparation method of the antistatic high-strength PP material according to claim 1, wherein in the step (1), N-methyldiethanolamine and gamma-chloropropyltrimethoxysilane are taken in a reaction kettle, potassium iodide is used as a catalyst, a mixed solvent of isopropanol and methanol is used as a polar organic solvent, the raw materials are heated to be dissolved and uniformly mixed, then the mixture is transferred to a microwave reaction device for reaction, and after the reaction is finished, the mixture is cooled, kept stand, separated and steamed in a rotary mode to obtain the organosilicon quaternary ammonium salt.
3. The method for preparing the antistatic high-strength PP material according to claim 1 or 2, wherein the material ratio in the step (1) is n (gamma-chloropropyltrimethoxysilane): n (N-methyldiethanolamine) ═ 1.0 to 1.5: 1.0.
4. the preparation method of the antistatic high-strength PP material according to claim 2, wherein the amount of the solvent in the step (1) is m (solvent): m (raw material) ═ 0.5-1.0: 1.0.
5. the method for preparing the antistatic high-strength PP material according to claim 2, wherein the mass ratio of the isopropanol to the methanol in the step (1) is 1.0-3.0: 1.0.
6. the method for preparing the antistatic high-strength PP material according to claim 2, wherein the reaction time in the step (1) is 8-16 h; preferably, the reaction temperature in the step (1) is 120-200 ℃; preferably, the microwave power in the step (1) is 500-.
7. The method for preparing antistatic high strength PP material according to claim 1, wherein the polyether ester in the step (2) is a copolymer consisting of polyester and polyether, the polyester is polybutylene terephthalate, and the polyether is a polymer of ethylene glycol; preferably, the molecular weight of the polyether ester in the step (2) is 1000-50000, the mass ratio of the polyether ester with the molecular weight of 1000 to the polyether ester with the molecular weight of 10000 to the polyether ester with the molecular weight of 50000 is 1-4: 3-4: 0 to 3; further preferably, the molecular weight is 1000 polyetherester to 10000 polyetherester to 50000 polyetherester to 1: 1: 1.
8. the preparation method of the antistatic high-strength PP material according to claim 1, wherein the mass ratio of the polyether ester, the silicone quaternary ammonium salt and the PP in the step (2) is 4-12: 0.8-5: 86-96, preferably 4-9: 3-5: 86-92, more preferably 9: 5: 86.
9. the method for preparing the antistatic high-strength PP material according to claim 1, wherein the drying temperature in the step (2) is 80-120 ℃ and the drying time is 1-5 h.
10. The method for preparing the antistatic high-strength PP material as claimed in claim 1, wherein the extrusion temperature of the twin-screw extruder in the step (2) is 160-220 ℃, the screw rotation speed of the extruder is 50-80r/min, and the injection molding temperature is 150-200 ℃.
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Denomination of invention: A preparation method of anti-static high-strength PP material Effective date of registration: 20231202 Granted publication date: 20230602 Pledgee: Agricultural Bank of China Limited Dongyang sub branch Pledgor: HENGDIAN GROUP DEBANG ENGINEERING PLASTIC CO.,LTD. Registration number: Y2023330002892 |