Functional composite material and preparation method thereof

文档序号:461324 发布日期:2021-12-31 浏览:5次 中文

阅读说明:本技术 一种功能性复合材料及其制备方法 (Functional composite material and preparation method thereof ) 是由 张兴光 于 2021-10-18 设计创作,主要内容包括:本发明公开了一种功能性复合材料及其制备方法。所述功能性复合材料包括基体合成树脂、IFPs及分散润滑剂。制备方法为:将分散润滑剂、IFPs、基体合成树脂在干燥设备中除去水分;将干燥后的分散润滑剂、IFPs混合搅拌均匀,然后挤出造粒,得到分散润滑剂处理后的IFPs;将经过干燥的基体合成树脂加入到分散润滑剂处理后的IFPs中进行混合,搅拌均匀,然后挤出造粒,即得功能性复合新材料。本发明统一了功能性复合新材料的制备方法,不同的基体合成树脂的功能性复合新材料均可按照本发明公开的方法而进行制备。本发明提供的高分散性功能性复合新材料的制备工艺简单,无特殊设备。且工艺灵活。(The invention discloses a functional composite material and a preparation method thereof. The functional composite material comprises matrix synthetic resin, IFPs and a dispersing lubricant. The preparation method comprises the following steps: removing water from the dispersion lubricant, IFPs and the matrix synthetic resin in a drying device; mixing and stirring the dried dispersed lubricant and IFPs uniformly, and then extruding and granulating to obtain IFPs treated by the dispersed lubricant; and adding the dried matrix synthetic resin into the IFPs treated by the dispersed lubricant, mixing, uniformly stirring, and then extruding and granulating to obtain the novel functional composite material. The invention unifies the preparation method of the new functional composite material, and the new functional composite materials of different matrix synthetic resins can be prepared according to the method disclosed by the invention. The preparation process of the high-dispersity functional composite new material provided by the invention is simple and has no special equipment. And the process is flexible.)

1. A functional composite material is characterized by comprising 35-78 parts of matrix synthetic resin, 20-50 parts of IFPs and 2-15 parts of dispersing lubricant in parts by mass; the matrix synthetic resin is a high molecular polymer which can form a flowing melt after the temperature reaches the melting temperature of the matrix synthetic resin.

2. The functional composite according to claim 1, wherein the matrix synthetic resin is polyolefin, modified polymer of polyolefin, polyester, polyamide, polylactic acid, or engineering plastic.

3. The functional composite according to claim 2, wherein the polyolefin is at least one of polyethylene, polypropylene and polyvinyl chloride; the modified polymer of the polyolefin is maleic anhydride modified polyolefin; the polyester is at least one of polyethylene terephthalate, polytrimethylene terephthalate, polybutylene terephthalate and polyethylene naphthalate; the polyamide is at least one of polyamide 6, polyamide 66, polyamide 610 and polyamide 1010; the polylactic acid is poly butylene succinate; the engineering plastics are at least one of polyacrylonitrile-butadiene-styrene plastics, polystyrene, styrene acrylonitrile, polycarbonate and polymethyl methacrylate.

4. The functional composite of claim 1, wherein the IFPs are CuO, Cu2O、ZnO、TiO2、SiO2At least one of them, the average particle diameter is 25nm-2 μm.

5. The functional composite according to claim 1 or 4, wherein the IFPs are treated with at least one coupling agent selected from the group consisting of silane coupling agents and phthalate coupling agents, and the amount of the IFPs added is 0.5 to 3% by mass based on the IFPs.

6. The functional composite according to claim 5, wherein the silane coupling agent is KH550, KH560 or KH 570.

7. The functional composite according to claim 1, wherein the dispersing lubricant is at least one of liquid paraffin, white wax, polyethylene wax, carboxylated polyethylene wax, oxidized polyethylene wax, high boiling paraffin wax, microcrystalline paraffin wax, solid paraffin wax, polypropylene wax, stearic acid, calcium stearate, zinc stearate, stearamide, N ' -methylene bis stearamide, N ' -ethylene bis stearamide, and N, N ' -ethylene bis stearamide polar modifiers.

8. The functional composite of claim 7, wherein the polar modifier of N, N '-ethylene bis stearamide comprises hydroxyethyl ethylene bis stearamide and N, N' -ethylene bis-12-hydroxystearamide.

9. The method for preparing a functional composite according to any one of claims 1 to 8, comprising the steps of:

the first step is as follows: removing water from the dispersion lubricant, IFPs and the matrix synthetic resin in a drying device; mixing and stirring the dried dispersed lubricant and IFPs uniformly, and then extruding and granulating to obtain IFPs treated by the dispersed lubricant;

the second step is that: and adding the dried matrix synthetic resin into the IFPs treated by the dispersed lubricant, mixing, uniformly stirring, and then extruding and granulating to obtain the novel functional composite material.

10. The method of claim 9, wherein the first step and the second step are performed at a stirring speed of 30 to 3000 rpm for 1 to 60 minutes.

11. The method for preparing the functional composite material according to claim 9, wherein the extrusion granulation in the first step and the second step is a single-screw extrusion granulator, a twin-screw extrusion granulator, an internal mixing matched single-screw extrusion granulator, an internal mixing matched twin-screw extrusion granulator or a two-stage extrusion granulator; the temperature of granulation in the first step is set to be in the range of 80 to 190 ℃.

Technical Field

The invention relates to a functional composite material and a preparation method thereof, belonging to the technical field of preparation of functional high polymer materials.

Background

The novel antibacterial composite material is prepared by uniformly mixing inorganic functional powder and common synthetic resin slices according to a certain mass ratio, and the obtained downstream product contains a certain amount of inorganic antibacterial powder particles, so that the downstream product has an antibacterial function. For convenience of description, the "Inorganic Functional powder" is hereinafter referred to by the acronym IFPs (Inorganic-Functional Powders).

The downstream products include:

(1) if the antibacterial polyester yarn is applied to spinning, the obtained yarn has an antibacterial function and can be used in the textile industry;

(2) if the antibacterial non-woven fabric is applied to non-woven fabrics, the obtained non-woven fabrics have an antibacterial function;

(3) if the antibacterial plastic film is applied to the plastic film, the obtained plastic film has an antibacterial function;

(4) if the antibacterial agent is applied to various plastic bottles and plastic barrels, the corresponding products have the antibacterial function;

(5) in the application of other plastic fields, the obtained related plastic products have the antibacterial function.

The related literature reports and published patents about the preparation method and preparation process of the novel antibacterial composite material are many, for example:

(1) application No.: 201210466062.2, respectively; name: a method for preparing antibacterial masterbatch for fruit and vegetable fresh-keeping packaging materials. The invention discloses a preparation method of an antibacterial master batch for a fruit and vegetable fresh-keeping packaging material, wherein the antibacterial master batch comprises the following components in percentage by weight: 12-14% of nano montmorillonite, 7-9% of nano titanium dioxide, 6-8% of silane coupling agent, 6-8% of oxidized polyethylene wax, 4-6% of glycerol monostearate, 3-5% of hindered amine stabilizer and the balance of polyethylene resin; the preparation method comprises the following steps: fully mixing the materials by using a high-speed mixer for 55-65 minutes at the rotation speed of 280-300 revolutions per minute; then kneading the mixture on a double-screw extrusion granulator and extruding the mixture to prepare master batches, wherein the kneading time is 35 to 45 minutes, the screw temperature is 160 ℃ and 170 ℃, and the screw rotating speed is 270 ℃ and 280 r/min. Among them, oxidized polyethylene wax and glycerol monostearate can be used as dispersing lubricant, but the mixing of all the raw materials together will make oxidized polyethylene wax and glycerol monostearate not completely and fully act on IFPs nano titanium dioxide alone, so the mixing granulation mode can not fully exert the dispersing function of dispersing lubricant on IFPs, and make them fully and uniformly dispersed.

(2) Application No.: CN 201710821215.3; name: an antibacterial masterbatch for polypropylene plastics and a preparation method thereof. The invention relates to an antibacterial master batch for polypropylene plastics, which comprises the following components in percentage by weight: 520% of Unined RM antibacterial agent, 0.30.7% of lubricant, 0.10.3% of coupling agent and the balance of polypropylene plastic resin. The antibacterial master batch adopts various compounds, has good dispersibility and compatibility when compounded with polypropylene plastic resin, shows excellent ageing resistance and better mechanical property when added into polypropylene plastics such as polypropylene PP, other propylene copolymers or other polyolefins and the like, greatly prolongs the service life, has the functions of resisting common germs, inhibiting drug resistance germs, has high efficiency and durable washing resistance, plays the roles of purifying the environment, eliminating peculiar smell, self-cleaning and health care, does not pollute the environment and has no side effect on human bodies, and is beneficial to people to obtain more health benefits.

(3) Application No.: cn202010680444. x; name: an antibacterial masterbatch and its preparation method and application are provided. The invention discloses an antibacterial master batch and a preparation method and application thereof. The antibacterial master batch comprises a nano glass antibacterial agent, polypropylene resin and a dispersing agent; the nano glass antibacterial agent is one or more of a nano glass silver-loaded antibacterial agent, a nano glass zinc-loaded antibacterial agent and a nano glass copper-loaded antibacterial agent; the content of the nano glass antibacterial agent is 5-12%; the percentage is the mass percentage of the nano glass antibacterial agent in the antibacterial master batch; the dispersing agent does not contain ions which chemically react with silver ions, zinc ions or copper ions.

(4) Application No.: CN 201811359220.8; name: polyamide antibacterial master batch and a production process thereof. The invention discloses a polyamide antibacterial master batch and a production process thereof, wherein the production process comprises the following steps: (1) weighing the raw materials in parts by weight; (2) mixing the raw materials in a high-speed mixer for 15-20min, adding into a double-screw extruder, and performing melt extrusion, cooling and granulation to obtain the final product.

The main defects of the prior art are as follows:

(1) the dispersibility of inorganic antibacterial powder particles in matrix synthetic resin needs to be improved. Numerous prior art techniques, briefly summarized: weighing various raw materials, an auxiliary agent, an antibacterial agent and the like according to a certain mass ratio, uniformly mixing, and granulating to obtain the antibacterial master batch. The granulation process is carried out at a temperature higher than the melting temperature of the matrix synthetic resin, and the inorganic antibacterial powder particles cannot be completely dispersed in the matrix synthetic resin through one granulation process. The smaller the particle size of the inorganic antibacterial powder particles, the greater the dispersion difficulty.

(2) The production process can be further simplified. The kinds of the new antibacterial composite materials (antibacterial master batches) are also various according to the kinds of the matrix synthetic resins. In the prior art, the preparation processes of different types of novel antibacterial composite materials are not unified, and each novel antibacterial composite material corresponds to one preparation process.

Disclosure of Invention

The technical problem to be solved by the invention is as follows: how to improve the dispersibility of inorganic antibacterial powder particles in matrix synthetic resin and how to further simplify the production process.

In order to solve the technical problem, the invention provides a functional composite material, which comprises 35-78 parts of matrix synthetic resin, 20-50 parts of IFPs and 2-15 parts of dispersing lubricant in parts by mass; the matrix synthetic resin is a high molecular polymer which can form a flowing melt after the temperature reaches the melting temperature of the matrix synthetic resin.

Preferably, the synthetic resin matrix is polyolefin, modified polyolefin polymer, polyester, polyamide, polylactic acid or engineering plastic.

More preferably, the polyolefin is at least one of Polyethylene (PE), polypropylene (PP) and polyvinyl chloride (PVC); the modified polymer of the polyolefin is maleic anhydride modified polyolefin (maleic anhydride modified polyethylene, maleic anhydride modified polypropylene and the like); the polyester is at least one of polyethylene terephthalate (PET), polytrimethylene terephthalate (PTT), polybutylene terephthalate (PBT) and polyethylene naphthalate (PEN); the polyamide is at least one of polyamide 6(PA6), polyamide 66(PA66), polyamide 610(PA610) and polyamide 1010(PA 1010); the polylactic acid (PLA) is Poly Butylene Succinate (PBS); the engineering plastic is at least one of polyacrylonitrile-butadiene-styrene plastic (ABS), Polystyrene (PS), Styrene Acrylonitrile (SAN), Polycarbonate (PC) and polymethyl methacrylate (PMMA).

Preferably, the IFPs adopt CuO and Cu2O、ZnO、TiO2、SiO2At least one of them, the average particle diameter is 25nm-2 μm.

Preferably, the IFPs are treated with at least one coupling agent selected from silane coupling agents and phthalate coupling agents, and the addition amount of the IFPs is 0.5-3% of the mass of the IFPs.

More preferably, the silane coupling agent is KH550, KH560 or KH 570.

Preferably, the dispersing lubricant is at least one of liquid paraffin (distillation temperature >300 ℃), white wax (distillation temperature 150 ℃.), polyethylene wax, carboxylated polyethylene wax, oxidized polyethylene wax, high-boiling paraffin wax, microcrystalline paraffin wax, solid paraffin wax, polypropylene wax, stearic acid, calcium stearate, zinc stearate, stearamide, N ' -methylene bis stearamide, N ' -ethylene bis stearamide, and N, N ' -ethylene bis stearamide polar modifiers.

More preferably, the polar modifier of N, N '-ethylene bis stearamide comprises hydroxyethyl ethylene bis stearamide and N, N' -ethylene bis-12-hydroxystearamide.

The dispersed lubricant is non-volatile, non-decomposed and non-carbonized at the melting temperature of the matrix synthetic resin in the application process of the novel functional composite material, and has stable chemical properties; meanwhile, the resin has good compatibility with the selected matrix synthetic resin and IFPs, the melt flowability of the matrix synthetic resin is obviously improved, and the dispersibility of the IFPs in the matrix synthetic resin is improved. The high temperature treatment process is a process of dispersing the effect of the lubricant on the IFPs. Through this process, the IFPs can be sufficiently dispersed due to the dispersing action of the dispersing agent on the IFPs and the mixing shearing action of the high-temperature treatment equipment, and thus, the IFPs can be well dispersed in the matrix synthetic resin. The dispersing lubricant and the combination thereof are reasonably selected, and the dispersing lubricant is nonvolatile, does not decompose or carbonize at the melting temperature of matrix synthetic resin in the application process of the novel functional composite material, and has stable chemical properties; meanwhile, the resin has good compatibility with the selected matrix synthetic resin and IFPs, the melt flowability of the matrix synthetic resin is obviously improved, and the dispersibility of the IFPs in the matrix synthetic resin is improved. During high temperature processing, the molten dispersion lubricant can spread and wet on the surface of IFPs well, and can play a good physical and chemical role on the surface of the IFPs due to the specific groups of the molecules of the dispersion lubricant.

The invention also provides a preparation method of the functional composite material, which comprises the following steps:

the first step is as follows: removing water from the dispersion lubricant, IFPs and the matrix synthetic resin in a drying device; mixing and stirring the dried dispersed lubricant and IFPs uniformly, and then extruding and granulating to obtain IFPs treated by the dispersed lubricant; during this high temperature treatment, the selected dispersing lubricant provides sufficient work and dispersion of the IFPs. After the dispersing lubricant melts at the elevated temperature, it spreads wet on the surfaces of the IFPs. Meanwhile, due to the specific groups of the dispersed lubricant molecules, the dispersed lubricant molecules can play a good physical and chemical role on the surfaces of IFPs.

The second step is that: and adding the dried matrix synthetic resin into the IFPs treated by the dispersed lubricant, mixing, uniformly stirring, and then extruding and granulating to obtain the novel functional composite material. In the second step of the preparation process, the molten matrix synthetic resin is a highly viscous fluid, and it is known that the molecular structure of the matrix synthetic resin is dominated by hydrophobic segments, so that the freely flowable polymer chains have a better interaction with the IFPs treated with the dispersed lubricant obtained in the first step, and the two form an effectively bonded interface structure.

Preferably, the rotation speed of the stirring in the first step and the second step is 30-3000 r/min (preferably 60-300 r/min) and the time is 1-60 min (preferably 5-20 min).

Preferably, the extrusion granulation in the first step and the second step adopts a single-screw extrusion granulator, a double-screw extrusion granulator, a single-screw extrusion granulator matched with banburying, a double-screw extrusion granulator matched with banburying or a two-stage extrusion granulator; the temperature of granulation in the first step is set to be in the range of 80 to 190 ℃. The temperature settings of the different heating zones of the extrusion granulator differ in the first step depending on the dispersion lubricant used. The temperature setting of the different heating zones of the extrusion granulator in the second step varies depending on the matrix synthetic resin used, for example: selecting Polyethylene (PE) and polypropylene (PP) as matrix resins, and setting the temperature within the range of 120-; selecting polyamide 6(PA6) as matrix resin, and setting the temperature within the range of 200-; polyethylene terephthalate (PET) is selected as matrix resin, and the temperature setting range is 240-280 ℃.

The method fully disperses the IFPs through a high-temperature treatment process and two subsequent granulation processes, further improves the dispersion uniformity of the IFPs in the novel functional composite material, and simultaneously unifies the preparation process of the functional composite material with different matrix synthetic resin types.

The synthetic resin of the invention is a high molecular polymer obtained by chemical synthesis of low molecular weight substances, which deforms at a certain temperature and pressure and can recover the original shape after the temperature and the pressure are relieved. In a broad sense, any synthetic high molecular compound that can be used as a processing material for plastic products is called a synthetic resin. For example:

polyolefins: polyethylene (PE), polypropylene (PP), polyvinyl chloride (PVC), and the like;

modified polymers of polyolefins, such as maleic anhydride-modified polyolefins: maleic anhydride-modified polyethylene, maleic anhydride-modified polypropylene, and the like;

polyesters: polyethylene terephthalate (PET), polytrimethylene terephthalate (PTT), polybutylene terephthalate (PBT), polyethylene naphthalate (PEN), and the like;

polyamides: polyamide 6(PA6), polyamide 66(PA66), polyamide 610(PA610), polyamide 1010(PA1010), and the like;

polylactic acid (PLA): polybutylene succinate (PBS);

engineering plastics: polyacrylonitrile-butadiene-styrene plastic (ABS), Polystyrene (PS), Styrene Acrylonitrile (SAN), Polycarbonate (PC), polymethyl methacrylate (PMMA), and the like.

In the present invention, IFPs refer to micro-or nano-scale inorganic oxides or metal simple substances (e.g., TiO) having certain functions (e.g., flame retardancy, antibacterial property, antiviral property, antifungal property, and external ray protection)2ZnO, CuO, Ag metal powder, etc.).

The IFPs are compounded with the matrix synthetic resin, and the IFPs are uniformly dispersed in the matrix synthetic resin to obtain the novel functional composite material. For example: uniformly dispersing IFPs with an antibacterial function in matrix synthetic resin to obtain a new composite material with the antibacterial function; the composite material is a composite carrier of IFPs, such as common antibacterial master batch. The invention takes the preparation method of the novel antibacterial composite material as a key object and explains the uniform preparation method of the novel composite material with similar functionality.

The high-temperature treatment process in the present invention is a process in which the dispersion lubricant acts on the IFPs, and this process allows the dispersion lubricant to sufficiently act on and disperse the IFPs, so that the effect of the dispersion lubricant is maximally exerted. After the subsequent granulation process, the IFPs can be uniformly dispersed in the matrix synthetic resin.

The invention unifies the preparation method of the new functional composite material, and the new functional composite materials of different matrix synthetic resins can be prepared according to the method disclosed by the invention.

The preparation process of the high-dispersity functional composite new material provided by the invention is simple and has no special equipment. And the process is flexible. The IFPs in the invention are replaced by inorganic micro-nano particles such as tourmaline powder particles, jade powder particles, magnesium oxide powder particles, aluminum hydroxide powder particles and the like, and corresponding new composite materials can be obtained.

Drawings

FIG. 1 is a schematic view showing the interaction between a dispersion lubricant and inorganic functional powder particles (IFPs).

Detailed Description

In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.

Example 1

A preparation method of a PE antibacterial composite material comprises the following steps:

the first step is as follows:

firstly, the required raw materials: the lubricant, IFPs and matrix synthetic resin were dispersed, and the water was removed in a drying apparatus.

② mixing at normal temperature. Weighing the dried dispersed lubricant: 2 parts, IFPs: 20 parts of the raw materials are mixed uniformly in a mixing device. Wherein the dispersing lubricant is hydroxyethyl ethylene bis stearamide 1.8 parts, liquid paraffin 0.2 parts (distillation temperature >300 ℃), IFPs nano zinc oxide ZnO powder with average particle diameter of 500nm (without surface modification). The mixing apparatus speed was 150 rpm and the mixing time was 20 minutes. After mixing at room temperature, a "homogeneous mixture of dispersed lubricant and IFPs" is obtained.

And thirdly, high-temperature treatment. The uniform mixture of the dispersion lubricant and the IFPs obtained by the steps is prepared into particles of the IFPs and the dispersion lubricant by the processes of high-temperature melting, screw conveying, extruding, cooling, granulating, drying and the like by using a double-screw extrusion granulator. Wherein the temperatures of the first section, the second section, the third section, the fourth section and the fifth section of the granulator are set as follows: 110 deg.C, 140 deg.C, 150 deg.C.

The second step is that:

after normal temperature mixing and high temperature treatment, the dispersed lubricant is melted and spread and wetted on the surface of the IFPs, the hydrophilic groups interact with the hydroxyl groups on the surface of the IFPs, and the hydrophobic tail faces outwards, and the structural schematic diagram is shown in FIG. 1. Meanwhile, different dispersing lubricants have hydrophobic structures, so that molecular layers of the interaction of the dispersing lubricants are bound on the surfaces of the IFPs. Such a configuration has two benefits. On one hand, the IFPs hinder agglomeration among IFPs due to the steric hindrance, and the IFPs are favorable for efficient dispersion of IFPs particles in matrix synthetic resin. On the other hand, the surface free energy of IFPs is reduced, the interaction between the particles and the matrix synthetic resin is improved, and the interface compatibility of the particles and the matrix synthetic resin is improved.

After high temperature treatment, nano zinc oxide ZnO (2 parts of dispersing lubricant and 20 parts of nano zinc oxide) treated by dispersing lubricant and 78 parts of matrix synthetic resin Polyethylene (PE) subjected to moisture removal by drying equipment are uniformly mixed in mixing equipment. The mixing apparatus speed was 150 rpm and the mixing time was 20 minutes. Then, by using a double-screw extrusion granulator, through the processes of high-temperature melting, screw conveying, extruding, cooling, granulating, drying and the like, particles of nano zinc oxide ZnO dispersed in matrix synthetic resin Polyethylene (PE) can be obtained, namely the novel PE antibacterial composite material. Wherein the temperatures of the first section, the second section, the third section, the fourth section and the fifth section of the granulator are set as follows: 190 deg.C, 210 deg.C.

Example 2

A preparation method of a PA6 antibacterial composite material comprises the following steps:

the first step is as follows:

firstly, the required raw materials: the lubricant, IFPs and matrix synthetic resin were dispersed, and the water was removed in a drying apparatus.

② mixing at normal temperature. Weighing the dried dispersed lubricant: 10 parts, IFPs: and 30 parts of the raw materials are uniformly mixed in a mixing device. Wherein the dispersing lubricant comprises 8 parts of hydroxyethyl ethylene bis stearamide, 1 part of N, N' -ethylene bis stearamide and 1 part of liquid paraffin (distillation temperature)>300 ℃ C.). IFPs is nano TiO2They had an average particle diameter of 200nm (without surface modification). The mixing apparatus speed was 150 rpm and the mixing time was 20 minutes. After mixing at room temperature, a "homogeneous mixture of dispersed lubricant and IFPs" is obtained.

And thirdly, high-temperature treatment. The uniform mixture of the dispersion lubricant and the IFPs obtained by the steps is prepared into particles of the IFPs and the dispersion lubricant by the processes of high-temperature melting, screw conveying, extruding, cooling, granulating, drying and the like by using a double-screw extrusion granulator. Wherein the temperatures of the first section, the second section, the third section, the fourth section and the fifth section of the granulator are set as follows: 110 deg.C, 140 deg.C, 170 deg.C.

The second step is that:

is obtained after high-temperature treatmentNano TiO treated with over-dispersed lubricant2(wherein 10 parts of lubricant and 30 parts of nano titanium dioxide are dispersed), and 60 parts of matrix synthetic resin polyamide 6(PA6) with water removed by a drying device are uniformly mixed in a mixing device. The mixing apparatus speed was 150 rpm and the mixing time was 20 minutes. Then, by using a double-screw extrusion granulator, through the processes of high-temperature melting, screw conveying, extruding, cooling, granulating, drying and the like, particles of nano titanium dioxide dispersed in matrix synthetic resin polyamide 6(PA6) can be obtained, namely the PA6 antibacterial composite new material. Wherein the temperatures of the first section, the second section, the third section, the fourth section and the fifth section of the granulator are set as follows: 230 ℃, 255 ℃, 260 ℃ and 260 ℃.

Example 3

A preparation method of a PBT antibacterial composite material comprises the following steps:

the first step is as follows:

firstly, the required raw materials: the lubricant, IFPs and matrix synthetic resin were dispersed, and the water was removed in a drying apparatus.

② mixing at normal temperature. Weighing the dried dispersed lubricant: 15 parts, IFPs: 50 parts of the raw materials are uniformly mixed in a mixing device. Wherein the dispersing lubricant is 9 parts of hydroxyethyl ethylene bis stearamide, 3 parts of N, N '-ethylene bis-12-hydroxystearamide, 1 part of N, N' -ethylene bis stearamide, 1 part of polyethylene wax and 1 part of liquid paraffin (the distillation temperature is more than 300 ℃). IFPs are nano zinc oxide ZnO, and the average particle size of the IFPs is 100nm (surface modification is carried out by silane coupling agent KH570 with the mass fraction of 3%). The mixing apparatus speed was 150 rpm and the mixing time was 20 minutes. After mixing at room temperature, a "homogeneous mixture of dispersed lubricant and IFPs" is obtained.

And thirdly, high-temperature treatment. "homogeneous mixture of dispersed lubricant and IFPs" obtained by the above procedure: 65 parts of the IFPs and 35 parts of matrix resin are subjected to high-temperature melting, screw conveying, extruding, cooling, granulating, drying and other processes by using a double-screw extrusion granulator to obtain the particles combining the IFPs and the dispersed lubricant. Wherein the temperatures of the first section, the second section, the third section, the fourth section and the fifth section of the granulator are set as follows: 130 deg.C, 150 deg.C, 180 deg.C.

The second step is that:

after high temperature treatment, nano zinc oxide ZnO (15 parts of dispersing lubricant and 50 parts of nano zinc oxide) treated by dispersing lubricant and 35 parts of base synthetic resin polybutylene terephthalate (PBT) subjected to moisture removal by drying equipment are uniformly mixed in mixing equipment. The mixing apparatus speed was 150 rpm and the mixing time was 20 minutes. Then, by utilizing a double-screw extrusion granulator, through the processes of high-temperature melting, screw conveying, extruding, cooling, granulating, drying and the like, particles of nano zinc oxide dispersed in matrix synthetic resin polybutylene terephthalate (PBT) can be obtained, namely the novel PBT antibacterial composite material. Wherein the temperatures of the first section, the second section, the third section, the fourth section and the fifth section of the granulator are set as follows: 240 ℃, 253 ℃, 258 ℃ and 258 ℃.

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