CN108165040B - Composite section prepared by utilizing waste dry film and preparation method thereof - Google Patents
Composite section prepared by utilizing waste dry film and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L101/00—Compositions of unspecified macromolecular compounds
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2272—Ferric oxide (Fe2O3)
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
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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
- 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
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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
- 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 provides a composite section prepared by utilizing waste dry films and a preparation method thereof. The composite section bar comprises the following components in parts by weight: 25-35 parts of dry film fine materials, 35-45 parts of waste circuit board resin powder, 5-20 parts of polyethylene plastic and/or dry wood powder, 5-10 parts of waste glass fiber reinforced plastics and 10-15 parts of auxiliary agents; the dry film fine material is obtained by performing alkali treatment on a waste dry film, and the mass content of colloid components in the dry film fine material is less than or equal to 3%. The composite section with excellent mechanical properties is prepared by resource utilization of the waste dry films, the waste circuit board resin powder and the waste glass fiber reinforced plastics, and has remarkable economic and social benefits.
Description
Technical Field
The invention relates to a composite section, in particular to a composite section prepared by utilizing waste dry films and a preparation method thereof.
Background
The photoresist is a light-sensitive mixed liquid composed of photosensitive resin, sensitizer, solvent and other components. The photosensitive resin in the photoresist can rapidly generate a photocuring reaction in an exposure area after being irradiated by light, so that physical properties such as solubility, affinity and the like are obviously changed, and after being treated by a proper solvent, a soluble part can be removed so as to obtain a required image. Since photoresists have functions of preventing plating and etching, they are widely used in the wiring board industry for the fabrication and transfer of circuit components, solder masks, and dielectric patterns.
A photoresist (generally named dry film) developed by dupont in 1968, which is composed of a polyester film, a photoresist layer, a polyethylene protective film, etc., is widely used in the production process of circuit boards. According to incomplete statistics, the annual waste dry film generated in coastal areas of southeast of China is up to more than 30-50 ten thousand tons; at present, the waste dry film is mostly treated as hazardous waste by incineration. However, since a part of the dry film photoresist may contain a halogen-based photosensitive component, and in addition, the dry film itself contains a large amount of organic colloidal substances, which easily cause generation of highly toxic gases such as dioxin during incineration, there is an urgent need to develop a safe and environment-friendly treatment method.
The continuous increase of the social demand of electric and electronic products promotes the rapid development of the printed circuit board industry, and simultaneously leads to the increasing of waste dry films, waste circuit board resins and other wastes generated in the production and recovery processes of the printed circuit boards, and causes the difficult problems of organic solid wastes, environmental protection disposal and the like. The waste circuit board generated when the electric and electronic products are scrapped usually contains toxic substances such as epoxy resin, brominated flame retardant, heavy metal and the like, and pollutants such as dioxin, fly ash containing heavy metal, garbage leachate and the like can be generated in the traditional treatment modes such as incineration, landfill and the like, so that the environmental pollution is very easy to cause. Therefore, development of a method for recycling the waste dry films and the waste circuit boards is urgently needed.
Disclosure of Invention
The invention provides a composite section prepared by utilizing waste dry films and a preparation method thereof, the method realizes resource utilization of the waste dry films, waste circuit board resin and waste glass fiber reinforced plastics, and the prepared composite section has excellent mechanical properties and has remarkable environmental, economic and social benefits.
The invention provides a composite section prepared by utilizing waste dry films, which comprises the following components in parts by weight: 25-35 parts of dry film fine materials, 35-45 parts of waste circuit board resin powder, 5-20 parts of polyethylene plastic and/or dry wood powder, 5-10 parts of waste glass fiber reinforced plastics and 10-15 parts of auxiliary agents; the dry film fine material is obtained by performing alkali treatment on a waste dry film, and the mass content of colloid components in the dry film fine material is less than or equal to 3%.
In the invention, the dry film is a photoresist produced by DuPont company in America and consists of a polyester film, a photosensitive adhesive layer, a polyethylene protective film and the like; the waste dry film is dry film waste materials which are discarded in the process of producing the circuit board by using the dry film; the dry film fines are obtained by subjecting the waste dry films to an alkali treatment. In the present invention, unless otherwise specified, the contents all refer to mass contents.
The inventor finds that the waste dry film has the defects of high content of colloid components (derived from a photosensitive adhesive layer of the dry film and mainly composed of a polystyrene-butadiene copolymer), difficulty in dispersion and the like when the waste dry film is recycled; the defects can be overcome by carrying out alkali treatment on the waste dry film, so that the resource utilization of the waste dry film is favorably realized. In view of this, the present invention has been completed.
In the invention, the mass content of the colloid component in the dry film fines is less than or equal to 3 percent; specifically, the colloid component is calculated by polystyrene-butadiene copolymer, and the mass content of the colloid component is measured by a Fourier transform infrared spectrometer and a cracking gas chromatography-mass spectrometer; the dry film fine material with the quality requirement (namely the mass content of the colloid component is less than or equal to 3 percent) is beneficial to preparing the composite section with excellent mechanical property. The process conditions for the alkali treatment to form the dry film fines are not critical to the present invention, as long as dry film fines having the above quality requirements are obtained.
Further, the average particle size of the dry film fines is more than 100 mesh, for example, 110-150 mesh. It is understood that the above dry film fines may be obtained by sequentially subjecting the waste dry film to alkali treatment, solid-liquid separation, drying, pulverizing, and sieving.
Furthermore, the dry film fines have a water content of < 1%; specifically, the water content of the dry film fines can be reduced to the above-mentioned suitable range by a conventional manner such as drying, wherein the drying temperature can be controlled to 100-125 ℃ for 30-120 min.
In the present invention, the resin powder of the waste circuit board refers to resin powder obtained by separating most metals from the waste circuit board by physical crushing, multi-stage crushing and sorting techniques. In the invention, the total metal content of the resin powder of the waste circuit board is not more than 0.5 percent, and the average particle size is more than 100 meshes.
The composite section bar of the invention can comprise polyethylene plastic or dried wood powder independently, or can comprise polyethylene plastic and dried wood powder simultaneously. Wherein the granularity of the polyethylene plastic is more than 100 meshes; the granularity of the dried wood powder is more than 100 meshes, and the water content is less than or equal to 0.5 percent.
In the invention, the waste glass fiber reinforced plastics are derived from leftover materials generated in the production and manufacturing field of fan blades and circuit boards, and mainly comprise glass fiber reinforced epoxy resin; specifically, the mass content of the glass fiber in the glass fiber reinforced epoxy resin is about 70%, and the mass content of the epoxy resin is about 30%; in particular, the glass fibers may be alkali-free glass fibers, and further aluminoborosilicate glass fibers having an alkali metal oxide content of 0 to 2%.
In the invention, the auxiliary agent comprises the following components in parts by weight: 3-5 parts of coupling agent, 3-5 parts of colorant, 2-2.5 parts of lubricant and 2-2.5 parts of flame retardant. Specifically, the coupling agent may be selected from one or two of a silane coupling agent and an aluminate; the colorant can be one or two of iron oxide red and rutile type titanium dioxide; the lubricant may be selected from one or both of polyester wax and polyethylene wax; the flame retardant may be one or two selected from zinc borate and aluminum trioxide.
The composite section bar has the compression strength of not less than 50MPa and the bending strength of not less than 30 MPa; the composite section has excellent comprehensive performance.
The composite section bar disclosed by the invention adopts the waste dry films and the waste circuit board resin as main raw materials, the plasticity of the waste dry films is fully utilized, the polyethylene plastics used in the production process of the composite section bar are completely or partially replaced, the using amount of the polyethylene plastics is greatly reduced, the pollution discharge and safety risk brought by the stacking of pollutants such as the waste dry films, the waste circuit boards and the like and the traditional disposal mode are effectively solved, the resource utilization of the waste materials is realized, and the prepared composite section bar has excellent mechanical property.
The invention also provides a preparation method of any one of the composite sections, which comprises the following steps:
1) sequentially carrying out alkali treatment and solid-liquid separation on the waste dry film to obtain dry film filter residue and filtrate;
2) drying, crushing and screening the dry film filter residue to obtain a dry film fine material;
3) mixing 25-35 parts of dry film fine materials, 35-45 parts of waste circuit board resin powder, 5-20 parts of polyethylene plastic and/or dry wood powder, 5-10 parts of waste glass fiber reinforced plastics and 10-15 parts of auxiliary agents, and then carrying out mixing, granulation, extrusion and molding to obtain the composite section.
Specifically, the alkali treatment may be performed with an alkali solution having a concentration of 0.1 to 0.3 mol/L; the alkali solution is not particularly limited, and may be, for example, a NaOH solution. In addition, when the alkali treatment is carried out, the mass ratio of the alkali solution to the waste dry film can be controlled to be (2-3): 1. further, the temperature of the alkali treatment can be controlled to be 85-95 ℃ and the time is 30-120 min. The above-described alkali treatment process readily yields dry film fines having the above-described quality requirements.
Particularly, the filtrate formed by solid-liquid separation can be combined into the alkali solution for alkali treatment, so that the using amount of the alkali solution is reduced, and the cost is further reduced.
The conditions of the drying treatment are not strictly limited as long as the water content of the dry film fines can be reduced to a suitable range, and the water content of the dry film fines can be, for example, less than 1%; specifically, the drying temperature can be controlled at 100-125 ℃ for 30-120 min.
Further, the kneading, granulating, extruding and molding may be carried out in a conventional manner; specifically, the mixing temperature can be controlled to be 75-85 ℃, and the mixing time is 5-10 min; and a double-screw granulator can be adopted for granulation, wherein the granulation temperature is controlled to be 175-185 ℃, the rotating speed of a main machine is controlled to be 75-85r/min, and the feeding rotating speed is controlled to be 30-40 r/min; in addition, a double-screw extruder can be adopted for the extrusion, wherein the extrusion temperature is controlled to be 190-200 ℃, the rotating speed of a main machine is 6-10r/min, and the feeding rotating speed is 9-15 r/min.
The method has simple treatment equipment and low investment cost, can effectively reduce solid waste emission in the production process of the circuit board, thereby solving the problems of pollution emission and safety risk caused by the stockpiling of pollutants such as waste dry films, waste circuit boards and the like and the traditional treatment mode, and can fully utilize the plasticity of a dry film material to completely or partially replace the traditionally used polyethylene plastic, thereby realizing the turning of harm into benefit and changing waste into valuables, and the prepared composite section bar has excellent comprehensive performance and obvious resource environment and economic benefits.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, 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. 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.
The main raw materials adopted by the embodiments of the invention are as follows:
discarding the dry film: the dry film waste material discarded in the production process of the circuit board mainly comprises a polyester film, a photosensitive adhesive layer, a polyethylene protective film and the like;
resin powder of the waste circuit board: the total metal content is not more than 0.5 percent, and the average particle size is more than 100 meshes;
polyethylene plastics: the average particle size is more than 100 meshes;
drying the wood powder: the average particle size is more than 100 meshes, and the water content is not more than 0.5%;
waste glass fiber reinforced plastic: the main components are glass fiber reinforced epoxy resin, wherein the mass content of the glass fiber is about 70 percent, the mass content of the epoxy resin is about 30 percent, and the glass fiber is aluminoborosilicate glass fiber with the content of alkali metal oxide of 0-2 percent.
Silane coupling agent: KH550 (gamma-aminopropyltriethoxysilane).
Example 1
1. Preparation of Dry film fines
And (3) carrying out alkali treatment (alkali boiling) on the waste dry film by adopting 0.1mol/L NaOH solution, wherein the mass ratio of the NaOH solution to the waste dry film is 2:1, the temperature of the alkali treatment is controlled to be 90 ℃, and the time is controlled to be 120min, so as to obtain alkali treatment liquid.
Filtering the alkali treatment solution, collecting filtrate to obtain alkaline filtrate containing a small amount of colloid, and combining the alkaline filtrate into a NaOH solution for recycling; and meanwhile, collecting filter residues to obtain water-containing dry film filter residues, and carrying out ventilation drying on the water-containing dry film filter residues, wherein the drying temperature is controlled at 100 ℃, and the drying time is controlled at 120min to obtain dry film dispersing residues.
And (3) crushing and screening the dry film dispersing slag to obtain dry film fine materials with the average particle size of 120 meshes and the water content of less than 1%.
Detecting the dry film fine materials by adopting a Fourier transform infrared spectrometer and a cracking gas chromatography-mass spectrometer; the results show that: the mass content of the gum component (calculated as polystyrene-butadiene copolymer) in the dry film fines was 2.4%.
2. Preparation of composite profiles
The preparation method comprises the following steps of preparing 45 parts of waste circuit board resin powder, 25 parts of dry film fine materials, 10 parts of polyethylene plastics, 5 parts of waste glass fiber reinforced plastics, 5 parts of silane coupling agents, 5 parts of iron oxide red, 2.5 parts of polyester wax and 2.5 parts of zinc borate.
Fully mixing the waste circuit board resin powder, the dry film fine material, the polyethylene plastic, the waste glass fiber reinforced plastic and the additives (namely the coupling agent, the coloring agent, the lubricating agent and the flame retardant) according to the proportion, then carrying out high-speed mixing, then carrying out granulation by a double-screw granulator, then extruding by a counter-rotating double-screw extruder, and cooling and forming to obtain a composite section; wherein the mixing time is controlled to be 5 minutes, and the mixing temperature is controlled to be 85 ℃; the temperature of the twin-screw granulation is 185 ℃, the rotating speed of the main machine is 85r/min, and the feeding rotating speed is 40 r/min; the temperature of the twin-screw extrusion is 200 ℃, the rotating speed of the main machine is 10r/min, and the feeding rotating speed is 15 r/min.
The composite section prepared in the above way is tested according to the requirements of GB/T245908-2009 Wood Plastic flooring, and the results are shown in Table 1.
Example 2
1. Preparation of Dry film fines
And (3) carrying out alkali treatment (alkali boiling) on the waste dry film by adopting 0.2mol/L NaOH solution, wherein the mass ratio of the NaOH solution to the waste dry film is 2:1, the temperature of the alkali treatment is controlled to be 90 ℃, and the time is controlled to be 60min, so as to obtain alkali treatment liquid.
Filtering the alkali treatment solution, collecting filtrate to obtain alkaline filtrate containing a small amount of colloid, and combining the alkaline filtrate into a NaOH solution for recycling; and meanwhile, collecting filter residues to obtain water-containing dry film filter residues, and carrying out ventilation drying on the water-containing dry film filter residues, wherein the drying temperature is controlled to be 105 ℃, and the drying time is controlled to be 100min, so that dry film dispersing residues are obtained.
And (3) crushing and screening the dry film dispersing slag to obtain a dry film fine material with the average particle size of 130 meshes and the water content of less than 1%.
Detecting the dry film fine material by adopting the method of example 1; the results show that: the mass content of the gum component (calculated by the polystyrene-butadiene copolymer) in the dry film fines was 2.0%.
2. Preparation of composite profiles
Preparing 45 parts of waste circuit board resin powder, 35 parts of dry film fine materials, 5 parts of dry wood powder, 5 parts of waste glass fiber reinforced plastics, 3 parts of silane coupling agent, 3 parts of iron oxide red, 2 parts of polyester wax and 2 parts of zinc borate.
Fully mixing the waste circuit board resin powder, the dry film fines, the dry wood powder, the waste glass fiber reinforced plastics and the additives (namely the coupling agent, the coloring agent, the lubricating agent and the flame retardant) according to the proportion, then carrying out high-speed mixing, then carrying out granulation by a double-screw granulator, then extruding by a counter-rotating double-screw extruder, and cooling and forming to obtain a composite section; wherein the mixing time is controlled to be 5 minutes, and the mixing temperature is controlled to be 80 ℃; the temperature of the twin-screw granulation is 180 ℃, the rotating speed of the main machine is 80r/min, and the feeding rotating speed is 35 r/min; the temperature of the twin-screw extrusion is 195 ℃, the rotating speed of the main machine is 8r/min, and the feeding rotating speed is 12 r/min.
The composite profiles prepared as described above were tested as in example 1 and the results are shown in table 1.
Example 3
1. Preparation of Dry film fines
And (3) carrying out alkali treatment (alkali boiling) on the waste dry film by adopting 0.3mol/L NaOH solution, wherein the mass ratio of the NaOH solution to the waste dry film is 3:1, the temperature of the alkali treatment is controlled to be 90 ℃, and the time is controlled to be 30min, so as to obtain alkali treatment liquid.
Filtering the alkali treatment solution, collecting filtrate to obtain alkaline filtrate containing a small amount of colloid, and combining the alkaline filtrate into a NaOH solution for recycling; and meanwhile, collecting filter residues to obtain water-containing dry film filter residues, and carrying out ventilation drying on the water-containing dry film filter residues, wherein the drying temperature is controlled at 110 ℃, and the drying time is controlled at 80min to obtain dry film dispersing residues.
And (3) crushing and screening the dry film dispersing slag to obtain dry film fine materials with the average particle size of 110 meshes and the water content of less than 1%.
Detecting the dry film fine material by adopting the method of example 1; the results show that: the mass content of the gum component (calculated as polystyrene-butadiene copolymer) in the dry film fines was 2.8%.
2. Preparation of composite profiles
Preparing 35 parts of waste circuit board resin powder, 35 parts of dry film fine materials, 10 parts of dry wood powder, 10 parts of waste glass fiber reinforced plastic, 3 parts of aluminate, 3 parts of rutile titanium dioxide, 2 parts of polyethylene wax and 2 parts of aluminum trioxide.
Fully mixing the waste circuit board resin powder, the dry film fines, the dry wood powder, the waste glass fiber reinforced plastics and the additives (namely the coupling agent, the coloring agent, the lubricating agent and the flame retardant) according to the proportion, then carrying out high-speed mixing, then carrying out granulation by a double-screw granulator, then extruding by a counter-rotating double-screw extruder, and cooling and forming to obtain a composite section; wherein the mixing time is controlled to be 5 minutes, and the mixing temperature is controlled to be 75 ℃; the temperature of the twin-screw granulation is 175 ℃, the rotating speed of the main machine is 75r/min, and the feeding rotating speed is 30 r/min; the temperature of the twin-screw extrusion is 190 ℃, the rotating speed of the main machine is 6r/min, and the feeding rotating speed is 9 r/min.
The composite profiles prepared as described above were tested as in example 1 and the results are shown in table 1.
Example 4
1. Preparation of Dry film fines
And (3) carrying out alkali treatment (alkali boiling) on the waste dry film by adopting 0.2mol/L NaOH solution, wherein the mass ratio of the NaOH solution to the waste dry film is 3:1, the temperature of the alkali treatment is controlled to be 90 ℃, and the time is controlled to be 50min, so as to obtain alkali treatment liquid.
Filtering the alkali treatment solution, collecting filtrate to obtain alkaline filtrate containing a small amount of colloid, and combining the alkaline filtrate into a NaOH solution for recycling; and meanwhile, collecting filter residues to obtain water-containing dry film filter residues, and carrying out ventilation drying on the water-containing dry film filter residues, wherein the drying temperature is controlled to be 115 ℃, and the drying time is 50min, so as to obtain the alkali treatment solution.
Filtering the alkali treatment solution, collecting filtrate to obtain alkaline filtrate containing a small amount of colloid, and combining the alkaline filtrate into a NaOH solution for recycling; and meanwhile, collecting filter residues to obtain dry film dispersing residues containing water, and carrying out ventilation drying on the dry film dispersing residues, wherein the drying temperature is controlled to be 115 ℃, and the drying time is 50min to obtain the dry film dispersing residues.
And (3) crushing and screening the dry film dispersing slag to obtain dry film fine materials with the average particle size of 140 meshes and the water content of less than 1%.
Detecting the dry film fine material by adopting the method of example 1; the results show that: the mass content of the gum component (calculated by the polystyrene-butadiene copolymer) in the dry film fines was 1.0%.
2. Preparation of composite profiles
Preparing raw materials according to 35 parts of waste circuit board resin powder, 30 parts of dry film fine materials, 5 parts of polyethylene plastics, 5 parts of dry wood powder, 10 parts of waste glass fiber reinforced plastics, 5 parts of aluminate, 5 parts of rutile titanium dioxide, 2.5 parts of polyethylene wax and 2.5 parts of aluminum trioxide.
Fully mixing the waste circuit board resin powder, the dry film fine material, the polyethylene plastic, the dry wood powder, the waste glass fiber reinforced plastic and the additives (namely the coupling agent, the coloring agent, the lubricating agent and the flame retardant) according to the proportion, then carrying out high-speed mixing, then carrying out granulation by a double-screw granulator, then extruding by a counter-rotating double-screw extruder, and cooling and forming to obtain a composite section; wherein the mixing time is controlled to be 5 minutes, and the mixing temperature is controlled to be 80 ℃; the temperature of the twin-screw granulation is 185 ℃, the rotating speed of the main machine is 80r/min, and the feeding rotating speed is 35 r/min; the temperature of the twin-screw extrusion is 195 ℃, the rotating speed of the main machine is 8r/min, and the feeding rotating speed is 12 r/min.
The composite profiles prepared as described above were tested as in example 1 and the results are shown in table 1.
Example 5
1. Preparation of Dry film fines
And (3) carrying out alkali treatment (alkali boiling) on the waste dry film by adopting 0.1mol/L NaOH solution, wherein the mass ratio of the NaOH solution to the waste dry film is 2.5:1, the temperature of the alkali treatment is controlled to be 90 ℃, and the time is controlled to be 85min, so as to obtain alkali treatment liquid.
Filtering the alkali treatment solution, collecting filtrate to obtain alkaline filtrate containing a small amount of colloid, and combining the alkaline filtrate into a NaOH solution for recycling; and meanwhile, collecting filter residues to obtain water-containing dry film filter residues, and carrying out ventilation drying on the water-containing dry film filter residues, wherein the drying temperature is controlled to be 120 ℃, and the drying time is controlled to be 35min, so that dry film dispersing residues are obtained.
And (3) crushing and screening the dry film dispersing slag to obtain dry film fine materials with the average particle size of 125 meshes and the water content of less than 1%.
Detecting the dry film fine material by adopting the method of example 1; the results show that: the mass content of the gum component (calculated by the polystyrene-butadiene copolymer) in the dry film fines was 2.2%.
2. Preparation of composite profiles
The preparation method comprises the following steps of preparing 40 parts of waste circuit board resin powder, 30 parts of dry film fine materials, 5 parts of polyethylene plastics, 10 parts of dry wood powder, 5 parts of waste glass fiber reinforced plastics, 1.5 parts of silane coupling agents, 1.5 parts of aluminate, 1.5 parts of iron oxide red, 1.5 parts of rutile titanium dioxide, 1 part of polyester wax, 1 part of polyethylene wax, 1 part of zinc borate and 1 part of aluminum trioxide.
Fully mixing the waste circuit board resin powder, the dry film fine material, the polyethylene plastic, the dry wood powder, the waste glass fiber reinforced plastic and the additives (namely the coupling agent, the coloring agent, the lubricating agent and the flame retardant) according to the proportion, then carrying out high-speed mixing, then carrying out granulation by a double-screw granulator, then extruding by a counter-rotating double-screw extruder, and cooling and forming to obtain a composite section; wherein the mixing time is controlled to be 5 minutes, and the mixing temperature is controlled to be 75 ℃; the temperature of the twin-screw granulation is 175 ℃, the rotating speed of the main machine is 75r/min, and the feeding rotating speed is 30 r/min; the temperature of the twin-screw extrusion is 190 ℃, the rotating speed of the main machine is 6r/min, and the feeding rotating speed is 9 r/min.
The composite profiles prepared as described above were tested as in example 1 and the results are shown in table 1.
Example 6
1. Preparation of Dry film fines
And (3) carrying out alkali treatment (alkali boiling) on the waste dry film by adopting 0.3mol/L NaOH solution, wherein the mass ratio of the NaOH solution to the waste dry film is 2.5:1, the temperature of the alkali treatment is controlled to be 90 ℃, and the time is controlled to be 40min, so as to obtain alkali treatment liquid.
Filtering the alkali treatment solution, collecting filtrate to obtain alkaline filtrate containing a small amount of colloid, and combining the alkaline filtrate into a NaOH solution for recycling; and meanwhile, collecting filter residues to obtain water-containing dry film filter residues, and carrying out ventilation drying on the water-containing dry film filter residues, wherein the drying temperature is controlled to be 125 ℃, and the drying time is controlled to be 30min, so that dry film dispersing residues are obtained.
And (3) crushing and screening the dry film dispersing slag to obtain dry film fine materials with the average particle size of 135 meshes and the water content of less than 1%.
Detecting the dry film fine material by adopting the method of example 1; the results show that: the mass content of the gum component (calculated by the polystyrene-butadiene copolymer) in the dry film fines was 1.6%.
2. Preparation of composite profiles
The preparation method comprises the following steps of preparing 40 parts of waste circuit board resin powder, 25 parts of dry film fine materials, 10 parts of polyethylene plastics, 10 parts of waste glass fiber reinforced plastics, 2.5 parts of silane coupling agents, 2.5 parts of aluminate, 2.5 parts of iron oxide red, 2.5 parts of rutile titanium dioxide, 1 part of polyester wax, 1.5 parts of polyethylene wax, 1 part of zinc borate and 1.5 parts of aluminum trioxide.
Fully mixing the waste circuit board resin powder, the dry film fine material, the polyethylene plastic, the waste glass fiber reinforced plastic and the additives (namely the coupling agent, the coloring agent, the lubricating agent and the flame retardant) according to the proportion, then carrying out high-speed mixing, then carrying out granulation by a double-screw granulator, then extruding by a counter-rotating double-screw extruder, and cooling and forming to obtain a composite section; wherein the mixing time is controlled to be 5 minutes, and the mixing temperature is controlled to be 85 ℃; the temperature of the twin-screw granulation is 185 ℃, the rotating speed of the main machine is 85r/min, and the feeding rotating speed is 40 r/min; the temperature of the twin-screw extrusion is 200 ℃, the rotating speed of the main machine is 10r/min, and the feeding rotating speed is 15 r/min.
The composite profiles prepared as described above were tested as in example 1 and the results are shown in table 1.
Comparative example 1
1. Preparation of Dry film fines
And (3) boiling the waste dry film with water, controlling the boiling temperature to be 90 ℃ and the time to be 120min, and obtaining a boiled liquid.
And filtering the boiled liquid, collecting filter residue, and carrying out ventilation drying on the filter residue, wherein the drying temperature is controlled at 100 ℃, and the drying time is controlled at 120min, so as to obtain the dry film filter residue.
And (3) crushing and screening the dry film filter residue to obtain dry film fine materials with the average particle size of 60 meshes and the water content of less than 1%.
Detecting the dry film fine material by adopting the method of example 1; the results show that: the mass content of the gum component (calculated by the polystyrene-butadiene copolymer) in the dry film fines was 14.0%.
2. Preparation of composite profiles
The preparation method comprises the following steps of preparing 45 parts of waste circuit board resin powder, 25 parts of dry film fine materials, 10 parts of polyethylene plastics, 5 parts of waste glass fiber reinforced plastics, 5 parts of silane coupling agents, 5 parts of iron oxide red, 2.5 parts of polyester wax and 2.5 parts of zinc borate.
Fully mixing the waste circuit board resin powder, the dry film fine material, the polyethylene plastic, the waste glass fiber reinforced plastic and the additives (namely the coupling agent, the coloring agent, the lubricating agent and the flame retardant) according to the proportion, then carrying out high-speed mixing, then carrying out granulation by a double-screw granulator, then extruding by a counter-rotating double-screw extruder, and cooling and forming to obtain a composite section; wherein the mixing time is controlled to be 5 minutes, and the mixing temperature is controlled to be 85 ℃; the temperature of the twin-screw granulation is 185 ℃, the rotating speed of the main machine is 85r/min, and the feeding rotating speed is 40 r/min; the temperature of the twin-screw extrusion is 200 ℃, the rotating speed of the main machine is 10r/min, and the feeding rotating speed is 15 r/min.
The composite profiles prepared as described above were tested according to the method of example 1, respectively, and the results are shown in table 1.
Comparative example 2
1. Preparation of Dry film fines
And (3) carrying out alkali treatment (alkali boiling) on the waste dry film by adopting 0.05mol/L NaOH solution, wherein the mass ratio of the NaOH solution to the waste dry film is 2.5:1, the temperature of the alkali treatment is controlled to be 70 ℃, and the time is controlled to be 150min, so as to obtain alkali treatment liquid.
Filtering the alkali treatment solution to obtain an alkali filtrate and a dry film filter residue containing water; and (3) carrying out ventilation drying on the dry film filter residue containing water, wherein the drying temperature is controlled to be 120 ℃, and the drying time is controlled to be 35min, so as to obtain dry film dispersing residue.
And (3) crushing and screening the dry film dispersing slag to obtain dry film fine materials with the average particle size of 70 meshes and the water content of less than 1%.
Detecting the dry film fine material by adopting the method of example 1; the results show that: the mass content of the gum component (calculated by the polystyrene-butadiene copolymer) in the dry film fines was 10.0%.
2. Preparation of composite profiles
Preparing 45 parts of waste circuit board resin powder, 35 parts of dry film fine materials, 5 parts of dry wood powder, 5 parts of waste glass fiber reinforced plastics, 3 parts of silane coupling agent, 3 parts of iron oxide red, 2 parts of polyester wax and 2 parts of zinc borate.
Fully mixing the waste circuit board resin powder, the dry film fines, the dry wood powder, the waste glass fiber reinforced plastics and the additives (namely the coupling agent, the coloring agent, the lubricating agent and the flame retardant) according to the proportion, then carrying out high-speed mixing, then carrying out granulation by a double-screw granulator, then extruding by a counter-rotating double-screw extruder, and cooling and forming to obtain a composite section; wherein the mixing time is controlled to be 5 minutes, and the mixing temperature is controlled to be 80 ℃; the temperature of the twin-screw granulation is 180 ℃, the rotating speed of the main machine is 80r/min, and the feeding rotating speed is 35 r/min; the temperature of the twin-screw extrusion is 195 ℃, the rotating speed of the main machine is 8r/min, and the feeding rotating speed is 12 r/min.
The composite profiles prepared as described above were tested as in example 1 and the results are shown in table 1.
Comparative example 3
The dry film fines prepared in example 1 were used as starting materials.
Preparing 35 parts of dry film fine material, 10 parts of polyethylene plastic, 5 parts of dry wood powder, 40 parts of waste glass fiber reinforced plastic, 3 parts of silane coupling agent, 3 parts of iron oxide red, 2 parts of polyester wax and 2 parts of zinc borate.
Fully mixing the dry film fine material, the polyethylene plastic, the dried wood powder, the waste glass fiber reinforced plastic and the additives (namely the coupling agent, the coloring agent, the lubricant and the flame retardant) according to the proportion, then carrying out high-speed mixing, then carrying out granulation by a double-screw granulator, then extruding by a counter-rotating double-screw extruder, and cooling and forming to obtain a composite section; wherein the mixing time is controlled to be 5 minutes, and the mixing temperature is controlled to be 85 ℃; the temperature of the twin-screw granulation is 185 ℃, the rotating speed of the main machine is 85r/min, and the feeding rotating speed is 40 r/min; the temperature of the twin-screw extrusion is 200 ℃, the rotating speed of the main machine is 10r/min, and the feeding rotating speed is 15 r/min.
The composite profiles prepared as described above were tested according to the method of example 1, respectively, and the results are shown in table 1.
Comparative example 4
Preparing 45 parts of waste circuit board resin powder, 25 parts of polyethylene plastic, 5 parts of dry wood powder, 15 parts of waste glass fiber reinforced plastic, 3 parts of silane coupling agent, 3 parts of iron oxide red, 2 parts of polyester wax and 2 parts of zinc borate.
Fully mixing the waste circuit board resin powder, the polyethylene plastic, the dried wood powder, the waste glass fiber reinforced plastic and the additives (namely the coupling agent, the coloring agent, the lubricating agent and the flame retardant) according to the proportion, then carrying out high-speed mixing, then carrying out granulation by a double-screw granulator, then extruding by a counter-rotating double-screw extruder, and cooling and forming to obtain a composite section; wherein the mixing time is controlled to be 5 minutes, and the mixing temperature is controlled to be 80 ℃; the temperature of the twin-screw granulation is 180 ℃, the rotating speed of the main machine is 80r/min, and the feeding rotating speed is 35 r/min; the temperature of the twin-screw extrusion is 195 ℃, the rotating speed of the main machine is 8r/min, and the feeding rotating speed is 12 r/min.
The composite profiles prepared as described above were tested as in example 1 and the results are shown in table 1.
TABLE 1 Performance test results for each of the composite profiles
| Composite section bar | Compressive strength/MPa | Flexural Strength/MPa |
| Example 1 | 53.4 | 32.8 |
| Example 2 | 54.6 | 34.5 |
| Example 3 | 51.2 | 31.0 |
| Example 4 | 56.5 | 36.8 |
| Example 5 | 53.8 | 33.0 |
| Example 6 | 54.0 | 32.9 |
| Comparative example 1 | 30.6 | 17.6 |
| Comparative example 2 | 32.5 | 18.3 |
| Comparative example 3 | 46.5 | 28.8 |
| Comparative example 4 | 44.6 | 25.8 |
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (7)
1. The composite section prepared by using the waste dry film is characterized by comprising the following components in parts by weight: 25-35 parts of dry film fine materials, 35-45 parts of waste circuit board resin powder, 5-20 parts of polyethylene plastic and/or dry wood powder, 5-10 parts of waste glass fiber reinforced plastics and 10-15 parts of auxiliary agents; the dry film fine material is obtained by performing alkali treatment, solid-liquid separation, drying, crushing and screening on a waste dry film, wherein the mass content of a colloid component in the dry film fine material is less than or equal to 3%;
performing alkali treatment by using an alkali solution with the concentration of 0.1-0.3mol/L, and controlling the mass ratio of the alkali solution to the waste dry film to be (2-3): 1; the average particle size of the dry film fines is more than 100 meshes.
2. The composite profile according to claim 1, wherein the auxiliary comprises the following components in parts by weight: 3-5 parts of coupling agent, 3-5 parts of colorant, 2-2.5 parts of lubricant and 2-2.5 parts of flame retardant.
3. A process for the preparation of a composite profile according to any one of claims 1 to 2, characterized in that it comprises the following steps:
1) sequentially carrying out alkali treatment and solid-liquid separation on the waste dry film to obtain dry film filter residue and filtrate;
2) drying, crushing and screening the dry film filter residue to obtain a dry film fine material;
3) mixing 25-35 parts of dry film fine materials, 35-45 parts of waste circuit board resin powder, 5-20 parts of polyethylene plastics and/or dry wood powder, 5-10 parts of waste glass fiber reinforced plastics and 10-15 parts of auxiliary agents, and then carrying out mixing, granulation, extrusion and molding to obtain the composite section;
performing alkali treatment by using an alkali solution with the concentration of 0.1-0.3mol/L, and controlling the mass ratio of the alkali solution to the waste dry film to be (2-3): 1; the average particle size of the dry film fine material is more than 100 meshes; controlling the temperature of the alkali treatment to be 85-95 ℃ and the time to be 30-120 min.
4. The method as claimed in claim 3, wherein the drying temperature is controlled to be 100-125 ℃ and the drying time is controlled to be 30-120 min.
5. The method according to claim 3, wherein the temperature of the mixing is controlled to be 75 to 85 ℃ and the time is 5 to 10 min.
6. The preparation method as claimed in claim 3, wherein the granulation is performed by using a twin-screw granulator, wherein the granulation temperature is controlled to be 175-185 ℃, the rotation speed of the main machine is controlled to be 75-85r/min, and the feeding rotation speed is controlled to be 30-40 r/min.
7. The preparation method according to claim 3, wherein the extrusion is performed by using a twin-screw extruder, wherein the extrusion temperature is controlled to be 190-.
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| CN112961509A (en) * | 2021-01-28 | 2021-06-15 | 常州厚德再生资源科技有限公司 | Method for preparing plastic-resin tray by using dry film waste material and resin powder in cooperation with mould pressing |
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| CN1282002A (en) * | 2000-08-28 | 2001-01-31 | 江阴霞客色纺有限公司 | Film release treatment process for photosensitive material |
| CN103709775A (en) * | 2013-12-20 | 2014-04-09 | 黄山美森新材料科技有限公司 | Preparation method of high-strength wood-plastic composite section bar |
| CN105524434A (en) * | 2016-01-19 | 2016-04-27 | 上海第二工业大学 | Organic acid-treated waste printed circuit board non-metallic powder/polyethylene glycol terephthalate composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1282002A (en) * | 2000-08-28 | 2001-01-31 | 江阴霞客色纺有限公司 | Film release treatment process for photosensitive material |
| CN103709775A (en) * | 2013-12-20 | 2014-04-09 | 黄山美森新材料科技有限公司 | Preparation method of high-strength wood-plastic composite section bar |
| CN105524434A (en) * | 2016-01-19 | 2016-04-27 | 上海第二工业大学 | Organic acid-treated waste printed circuit board non-metallic powder/polyethylene glycol terephthalate composite material and preparation method thereof |
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