CN112454721A - Preparation method of cylindrical octabromoether particles - Google Patents

Preparation method of cylindrical octabromoether particles Download PDF

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Publication number
CN112454721A
CN112454721A CN202011365491.1A CN202011365491A CN112454721A CN 112454721 A CN112454721 A CN 112454721A CN 202011365491 A CN202011365491 A CN 202011365491A CN 112454721 A CN112454721 A CN 112454721A
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octabromoether
screw
spraying
silicon carbide
nano silicon
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CN112454721B (en
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王盛海
郭建树
赵震
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Shandong Meite New Material Technology Co ltd
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Shandong Meite New Material Technology Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00—Making granules
    • B29B9/02—Making granules by dividing preformed material
    • B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B05D5/08—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface
    • B05D5/083—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface involving the use of fluoropolymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/05—Filamentary, e.g. strands
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/50—Details of extruders
    • B29C48/505—Screws
    • B29C48/507—Screws characterised by the material or their manufacturing process
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/50—Details of extruders
    • B29C48/505—Screws
    • B29C48/507—Screws characterised by the material or their manufacturing process
    • B29C48/509—Materials, coating or lining therefor
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/12—Powdering or granulating
    • C08J3/126—Polymer particles coated by polymer, e.g. core shell structures
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/12—Powdering or granulating
    • C08J3/128—Polymer particles coated by inorganic and non-macromolecular organic compounds
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/06—Surface hardening
    • C21D1/09—Surface hardening by direct application of electrical or wave energy; by particle radiation

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
  • Medicinal Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Wood Science & Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention relates to a preparation method of cylindrical octabromoether particles. The invention has the beneficial effects that: in the granulation process, the octabromoether is not bonded with a screw in the granulation equipment; effectively avoiding the blockage phenomenon of octabromoether granulation equipment; the operation and maintenance cost of the production device is effectively reduced, and the method can be suitable for large-scale continuous production; the screw hardness of the extruder is 62-67 HRC, and the extruder is strong in durability; the continuous granulation production is 10000h, and the loss of the screw coating of the extruding machine is less than 0.2 percent.

Description

Preparation method of cylindrical octabromoether particles
Technical Field
The invention relates to the field of octabromoether, in particular to a preparation method of cylindrical octabromoether particles.
Background
In recent years, with the rapid development of modern synthetic industry and the improvement of fire-proof safety awareness, the use of flame-retardant materials in various industries is forced by the state through legislation. With the development of the Chinese synthetic material industry and the continuous expansion of the application field, the flame retardant is better applied in various fields of buildings, textiles, plastics, electronic and electric appliances, transportation, aerospace, daily furniture, interior decoration, clothes, food and housing, and the like, and plays a great role.
The plastic industry in China has important structural adjustment, the flame retardant plastic will be increased in the future, and the plastic will be put forward more strict flame retardant requirements, and the proportion of the flame retardant plastic in the plastic will be increased. Tetrabromobisphenol A-bis (2, 3-dibromopropyl) ether, octabromoether for short, is a common brominated flame retardant, is added into materials such as polypropylene, polystyrene and the like and is compounded with antimony compounds for use, so that the materials can obtain excellent flame retardant property. The octabromoether has the bromine content of more than 67 percent, and has a melting point of more than 105 ℃, so the octabromoether has good compatibility with polyolefin materials.
During the production and granulation process of octabromoether, a plodder is generally adopted for granulation. Specifically, the octabromoether product is extruded by the rotation of a screw rod in a strip extruding machine, and is extruded into a strip shape from an extrusion hole of an extrusion plate of the strip extruding machine under the thrust action of the rotation of the screw rod, and then the octabromoether product is cut off to obtain octabromoether particles.
The octabromoether product has a low melting point, is easy to agglomerate under the action of external force and has certain viscosity, so that the conventional octabromoether granulation mode is easy to melt. The applicant finds that in the eight-bromo-ether granulation process, the eight-bromo-ether is bonded with a screw in an extruder, and is an important cause for blockage of granulation equipment. Meanwhile, after the extruder equipment is blocked, manual cleaning is needed, and the cleaning is difficult; impurities are easy to be mixed in the cleaning process; because impurities can not be melted and processed, the quality of the octabromoether particle product is reduced or even does not meet the product quality standard, and the operation and maintenance cost of production is greatly increased.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a preparation method of cylindrical octabromoether particles, which aims to realize the following purposes:
(1) in the eight-bromo-ether granulation process, the eight-bromo-ether is not bonded with a screw in granulation equipment, so that the granulation equipment is prevented from being blocked;
(2) the problems of difficult cleaning, easy impurity mixing, product quality reduction and even scrapping caused by blockage of octabromoether granulation equipment are avoided;
(3) the production, operation and treatment costs of the octabromoether are reduced.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the preparation method of the cylindrical octabromoether particles is characterized by comprising the following steps:
(1) adding water in a predetermined part into the octabromoether product, and uniformly mixing to obtain a mixed material;
(2) conveying the conveyed mixed material into a strip extruding machine according to a preset feeding speed, and extruding and granulating;
(3) and air-cooling the extruded octabromoether particles to form the extruded octabromoether particles.
Further, the water content of the mixed material is 30-35 wt%.
Further, the feeding speed is 300-400 Kg/h.
Further, the air cooling is carried out, and the air volume is 10-2000M3/h。
Furthermore, the bar extruder is a single-screw or double-screw bar extruder;
in the strip extruder, the screw is prepared by firstly carrying out surface treatment on the outer surface of the screw, then carrying out ultrasonic hardening treatment and finally spraying a coating;
the surface treatment comprises the steps of liquid spraying and dipping;
the spray solution is used for preheating the surface of the dried screw rod with the surface impurities removed to 140-160 ℃, and uniformly spraying a predetermined part of spray solution on the surface of the screw rod;
the spraying liquid comprises sodium chloride, zinc nitrate and deionized water;
the sodium chloride: zinc nitrate: the deionized water has a weight ratio of 8-10: 2-3: 90-100;
the spraying amount of the spraying is as follows: 8-20 ml of the water is sprayed on the surface area of each square centimeter.
Further, dipping the screw subjected to liquid spraying into a treating agent with the volume 2 times that of the screw, heating the treating agent to 60-70 ℃, standing for 60-90 min, taking out, and blowing by using hot air at 70 ℃ until the surface of the screw is dried;
the treating agent comprises zirconium nitrate, citric acid, zinc nitrate, diisooctyl sebacate, sodium methallylsulfonate, hydroxymethyl cellulose, ethylenediamine, ethanol and deionized water;
the zirconium nitrate: citric acid: zinc nitrate: diisooctyl sebacate: sodium methallyl sulfonate: hydroxymethyl cellulose: ethylene diamine: ethanol: the deionized water has a weight ratio of 2-3: 3-5: 2-3: 1-2: 2-3: 1-2: 2-3: 10-15: 50-60.
Further, in the ultrasonic hardening, the contact pressure between the ultrasonic cutter head and the surface of the screw is 20-30 MPa, the current value of the ultrasonic generator is 1.5-2.0A, and the rotating linear speed of the outer surface of the screw is 5-12 m/min.
Further, the coating is sprayed, and spraying, curing and forming are carried out;
the spraying step is to uniformly spray a coating agent on the surface of the screw rod after the ultrasonic hardening;
the coating agent comprises perfluoroalkoxy resin, epoxy resin, nano silicon carbide, nano zirconium silicate, manganese powder, nickel powder, silicon nitride, chromium oxide, sodium dodecyl sulfate and methanol;
the perfluoroalkoxy resin: epoxy resin: nano silicon carbide: nano zirconium silicate: manganese powder: nickel powder: silicon nitride: chromium oxide: sodium lauryl sulfate: the weight ratio of methanol is 1: 4-6: 3-5: 3-5: 3-5: 2-3: 3-5: 3-5: 2-3: 35-60 parts of;
and (3) curing, wherein the thickness of the coating after curing is 200-300 mu m.
Further, the nano silicon carbide is silanization modified nano silicon carbide;
the nano silicon carbide is prepared by pickling and removing impurities, then placing the nano silicon carbide into a mixed solution of vinyltrimethoxysilane and acetone, stirring the mixture for 3 hours at 200RPM and drying the mixture;
and (3) removing impurities by acid washing, soaking the nano silicon carbide for 1-2 hours by adopting 2 times of acetic acid with volume of 8%, and leaching the nano silicon carbide by adopting 5 times of deionized water.
Further, the vinyl trimethoxy silane: the weight part ratio of acetone is 1: 15;
the particle size of the nano silicon carbide and the nano zirconium silicate ranges from 100nm to 200 nm;
the particle size of the manganese powder, the nickel powder, the silicon nitride and the chromium oxide ranges from 1 to 2 mu m.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the preparation method of the cylindrical octabromoether particles, in the octabromoether granulation process, the octabromoether is not bonded with a screw in granulation equipment;
(2) the preparation method of the cylindrical octabromoether particles effectively avoids the blockage phenomenon of octabromoether granulation equipment, and the octabromoether particles have stable product quality;
(3) the preparation method of the cylindrical octabromoether particles effectively reduces the operation and maintenance costs of a production device, and can be suitable for large-scale continuous production;
(4) compared with the original preparation method, the preparation method of the cylindrical octabromoether particles has the advantages that the production, operation and maintenance cost is reduced by about 6-9%, and the economic benefit is outstanding;
(5) according to the preparation method of the cylindrical octabromoether particles, the hardness of the screw of the strip extruding machine is improved to 62-67 HRC from the original 46HRC after the strip extruding machine is processed, and the durability is strong;
(6) according to the preparation method of the cylindrical octabromoether particles, provided by the invention, the screw coating of the extruder is wear-resistant, the loss rate is low, the continuous granulation production is carried out for 10000h, and the loss of the coating is lower than 0.2%.
Detailed Description
In order to more clearly understand the technical features, objects, and effects of the present invention, specific embodiments of the present invention will now be described.
Example 1
A preparation method of cylindrical octabromoether particles comprises the following steps:
(1) adding water in a predetermined part into the octabromoether product, and uniformly mixing to obtain a mixed material;
(2) conveying the conveyed mixed material into a strip extruding machine according to a preset feeding speed, and extruding and granulating;
(3) and air-cooling the extruded octabromoether particles to form the extruded octabromoether particles.
The moisture content of the mixed material was 30% wt.
The feed rate was 300 Kg/h.
The air cooling is carried out, and the air volume is 200M3/h。
The bar extruding machine is a double-screw type bar extruding machine.
The screw of the bar extruder comprises a screw shaft and a helical blade.
And a plurality of helical blades which are arranged at equal intervals are arranged on the outer side of the screw shaft.
The screw is made of 45# steel.
The screw is prepared by carrying out surface treatment on the outer surface, then carrying out ultrasonic hardening treatment and finally spraying a coating.
The surface treatment comprises oil removal, water washing, liquid spraying and dipping.
And in the oil removing and water washing steps, firstly, the oil stain, impurities, rust and the like on the surface of the screw are removed by adopting a conventional cleaning agent, and then the surface of the screw is swept by adopting hot air at 60 ℃ until the surface of the screw is dried.
And in the liquid spraying, the surface of the screw is heated to 140 ℃, and the spraying liquid with the preset parts is uniformly sprayed on the surface of the screw.
The spraying liquid comprises sodium chloride, zinc nitrate and deionized water. Dispersing sodium chloride and zinc nitrate into deionized water to obtain the product.
The sodium chloride: zinc nitrate: the weight ratio of deionized water is 8:2: 90.
The spraying amount of the spraying is as follows: 8ml per square centimeter of surface area was sprayed.
And (3) dipping the sprayed screw into a treating agent with the volume 2 times that of the screw, heating the treating agent to 60 ℃, standing for 60min, taking out, and blowing by adopting hot air at 70 ℃ until the surface of the screw is dried.
The treating agent comprises zirconium nitrate, citric acid, zinc nitrate, diisooctyl sebacate, sodium methallyl sulfonate, hydroxymethyl cellulose, ethylenediamine, ethanol and deionized water.
The zirconium nitrate: citric acid: zinc nitrate: diisooctyl sebacate: sodium methallyl sulfonate: hydroxymethyl cellulose: ethylene diamine: ethanol: the weight ratio of the deionized water is 2: 3: 2: 1: 2: 1: 2: 10: 50.
and mixing ethanol and deionized water, adding zirconium nitrate, citric acid and zinc nitrate, uniformly stirring, sequentially adding the rest materials, and stirring at 50RPM for 20min to obtain the treating agent.
And ultrasonic hardening, namely putting the screw subjected to surface treatment into an ultrasonic impact processing device, and performing ultrasonic hardening treatment on the surface of the screw.
The ultrasonic impact processing device is provided with an ultrasonic cutter head, the contact pressure of the ultrasonic cutter head and the surface of the screw is 20MPa, the current value of an ultrasonic generator is 1.5A, and the rotating linear speed of the outer surface of the screw is 5 m/min.
And the coating spraying comprises spraying, curing and forming.
And the spraying step is to uniformly spray a coating agent on the surface of the screw rod after the ultrasonic hardening.
The coating agent comprises perfluoroalkoxy resin, epoxy resin, nano silicon carbide, nano zirconium silicate, manganese powder, nickel powder, silicon nitride, chromium oxide, sodium dodecyl sulfate and methanol.
The perfluoroalkoxy resin: epoxy resin: nano silicon carbide: nano zirconium silicate: manganese powder: nickel powder: silicon nitride: chromium oxide: sodium lauryl sulfate: the weight ratio of methanol is 1: 6: 3: 3: 5: 2: 3: 3: 2: 60.
the perfluoroalkoxy resin had a melt flow index of 2.6 (372 ℃/5.0 kg) and a particle size of 20 μm.
The epoxy value of the epoxy resin is 0.23.
The nano silicon carbide is silanization modified nano silicon carbide. The nano silicon carbide is prepared by pickling nano silicon carbide, removing impurities, putting the nano silicon carbide into a mixed solution of vinyl trimethoxy silane and acetone, stirring the mixture for 3 hours at 200RPM and drying the mixture.
And (3) removing impurities by acid washing, soaking the nano silicon carbide for 1 hour by adopting 2 times of acetic acid with volume of 8%, and then leaching the nano silicon carbide by adopting 5 times of deionized water.
The vinyl trimethoxy silane: the weight ratio of acetone was 1: 15.
The particle size range of the nano silicon carbide and the nano zirconium silicate is 200 nm.
The particle size range of the manganese powder, the nickel powder, the silicon nitride and the chromium oxide is 2 mu m.
The coating agent is prepared by uniformly mixing the perfluoroalkoxy resin, the epoxy resin, the sodium dodecyl sulfate and the methanol, sequentially adding the rest materials, and uniformly mixing.
And (3) curing, namely placing the sprayed screw in a vacuum environment at 400 ℃ for high-temperature curing for 2 h.
And (3) curing, wherein the thickness of the coating after curing is 200 mu m.
And (3) molding, namely placing the solidified screw in a vacuum environment at 30 ℃ and naturally cooling.
In the preparation method of the cylindrical octabromoether particles, in the process of octabromoether granulation, octabromoether does not adhere to a screw in granulation equipment; effectively avoiding the blocking phenomenon of octabromoether granulation equipment, and ensuring stable quality of octabromoether granules; the hardness of the screw of the bar extruder is improved to 62HRC from the original 46HRC after being processed, and the durability is strong; the screw coating of the extruder is wear-resistant and has low loss rate, and the continuous granulation production is carried out for 10000h, and the loss of the coating is 0.16 percent.
Example 2
A preparation method of cylindrical octabromoether particles comprises the following steps:
(1) adding water in a predetermined part into the octabromoether product, and uniformly mixing to obtain a mixed material;
(2) conveying the conveyed mixed material into a strip extruding machine according to a preset feeding speed, and extruding and granulating;
(3) and air-cooling the extruded octabromoether particles to form the extruded octabromoether particles.
The moisture content of the mixture was 32% wt.
The feed rate was 330 Kg/h.
Air cooling with 500M air volume3/h。
The bar extruding machine is a double-screw type bar extruding machine.
The screw of the bar extruder comprises a screw shaft and a helical blade.
And a plurality of helical blades which are arranged at equal intervals are arranged on the outer side of the screw shaft.
The screw is made of 45# steel.
The screw is prepared by carrying out surface treatment on the outer surface, then carrying out ultrasonic hardening treatment and finally spraying a coating.
The surface treatment comprises oil removal, water washing, liquid spraying and dipping.
And in the oil removing and water washing steps, firstly, the oil stain, impurities, rust and the like on the surface of the screw are removed by adopting a conventional cleaning agent, and then the surface of the screw is swept by adopting hot air at 70 ℃ until the surface of the screw is dried.
And in the liquid spraying, the surface of the screw is heated to 150 ℃, and the spraying liquid with the preset parts is uniformly sprayed on the surface of the screw.
The spraying liquid comprises sodium chloride, zinc nitrate and deionized water. Dispersing sodium chloride and zinc nitrate into deionized water to obtain the product.
The sodium chloride: zinc nitrate: the weight ratio of deionized water is 8:3: 90.
The spraying amount of the spraying is as follows: spraying 15ml per square centimeter of surface area.
And (3) dipping the sprayed screw into a treating agent with the volume 2 times that of the screw, heating the treating agent to 70 ℃, standing for 90min, taking out, and blowing by using hot air at 70 ℃ until the surface of the screw is dried.
The treating agent comprises zirconium nitrate, citric acid, zinc nitrate, diisooctyl sebacate, sodium methallyl sulfonate, hydroxymethyl cellulose, ethylenediamine, ethanol and deionized water.
The zirconium nitrate: citric acid: zinc nitrate: diisooctyl sebacate: sodium methallyl sulfonate: hydroxymethyl cellulose: ethylene diamine: ethanol: the weight ratio of the deionized water is 2: 5: 3: 1: 3: 1: 3: 15: 50.
and the treating agent is prepared by mixing ethanol and deionized water, adding zirconium nitrate, citric acid and zinc nitrate, uniformly stirring, sequentially adding the rest materials, and stirring at 100RPM for 30 min.
And ultrasonic hardening, namely putting the screw subjected to surface treatment into an ultrasonic impact processing device, and performing ultrasonic hardening treatment on the surface of the screw.
The ultrasonic impact processing device is provided with an ultrasonic tool bit, the contact pressure of the ultrasonic tool bit and the surface of the screw is 25MPa, the current value of an ultrasonic generator is 1.8A, and the rotating linear speed of the outer surface of the screw is 7 m/min.
And the coating spraying comprises spraying, curing and forming.
And the spraying step is to uniformly spray a coating agent on the surface of the screw rod after the ultrasonic hardening.
The coating agent comprises perfluoroalkoxy resin, epoxy resin, nano silicon carbide, nano zirconium silicate, manganese powder, nickel powder, silicon nitride, chromium oxide, sodium dodecyl sulfate and methanol.
The perfluoroalkoxy resin: epoxy resin: nano silicon carbide: nano zirconium silicate: manganese powder: nickel powder: silicon nitride: chromium oxide: sodium lauryl sulfate: the weight ratio of methanol is 1: 4: 5: 3: 3: 3: 5: 5: 3: 50.
the perfluoroalkoxy resin had a melt flow index of 2.6 (372 ℃/5.0 kg) and a particle size of 20 μm.
The epoxy value of the epoxy resin is 0.28.
The nano silicon carbide is silanization modified nano silicon carbide. The nano silicon carbide is prepared by pickling nano silicon carbide, removing impurities, putting the nano silicon carbide into a mixed solution of vinyl trimethoxy silane and acetone, stirring the mixture for 3 hours at 200RPM and drying the mixture.
And (3) removing impurities by acid washing, soaking the nano silicon carbide for 2 hours by adopting 2 times of acetic acid with volume of 8%, and then leaching the nano silicon carbide by adopting 5 times of deionized water.
The vinyl trimethoxy silane: the weight ratio of acetone was 1: 15.
The particle size of the nano silicon carbide and the nano zirconium silicate is 100 nm.
The particle size of the manganese powder, the nickel powder, the silicon nitride and the chromium oxide is 1 mu m.
The coating agent is prepared by uniformly mixing the perfluoroalkoxy resin, the epoxy resin, the sodium dodecyl sulfate and the methanol, sequentially adding the rest materials, and uniformly mixing.
And (3) curing, namely placing the sprayed screw in a vacuum environment at the temperature of 420 ℃ for high-temperature curing for 2.5 h.
And (3) curing, wherein the thickness of the coating after curing is 280 mu m.
And (3) molding, namely placing the solidified screw in a vacuum environment at 30 ℃ and naturally cooling.
In the preparation method of the cylindrical octabromoether particles, in the process of octabromoether granulation, octabromoether does not adhere to a screw in granulation equipment; effectively avoiding the blocking phenomenon of octabromoether granulation equipment, and ensuring stable quality of octabromoether granules; the hardness of the screw of the bar extruder is improved to 67HRC from the original 46HRC after the re-processing, and the durability is strong; the screw coating of the extruder is wear-resistant and has low loss rate, and the continuous granulation production is carried out for 10000h, and the loss of the coating is 0.09%.
Example 3
A preparation method of cylindrical octabromoether particles comprises the following steps:
(1) adding water in a predetermined part into the octabromoether product, and uniformly mixing to obtain a mixed material;
(2) conveying the conveyed mixed material into a strip extruding machine according to a preset feeding speed, and extruding and granulating;
(3) and air-cooling the extruded octabromoether particles to form the extruded octabromoether particles.
The moisture content of the mixture was 35% wt.
The feed rate was 400 Kg/h.
The air cooling is carried out, and the air volume is 200M3/h。
The bar extruding machine is a double-screw type bar extruding machine.
The screw of the bar extruder comprises a screw shaft and a helical blade.
And a plurality of helical blades which are arranged at equal intervals are arranged on the outer side of the screw shaft.
The screw is made of 45# steel.
The screw is prepared by carrying out surface treatment on the outer surface, then carrying out ultrasonic hardening treatment and finally spraying a coating.
The surface treatment comprises oil removal, water washing, liquid spraying and dipping.
And in the oil removing and water washing steps, firstly, the oil stain, impurities, rust and the like on the surface of the screw are removed by adopting a conventional cleaning agent, and then the surface of the screw is swept by adopting hot air at 70 ℃ until the surface of the screw is dried.
And in the liquid spraying, the surface of the screw is heated to 160 ℃, and the spraying liquid with the preset parts is uniformly sprayed on the surface of the screw.
The spraying liquid comprises sodium chloride, zinc nitrate and deionized water. Dispersing sodium chloride and zinc nitrate into deionized water to obtain the product.
The sodium chloride: zinc nitrate: the weight ratio of deionized water is 10: 3: 90.
The spraying amount of the spraying is as follows: 10ml per square centimeter of surface area was sprayed.
And (3) dipping the sprayed screw into a treating agent with the volume 2 times that of the screw, heating the treating agent to 60 ℃, standing for 90min, taking out, and blowing by adopting hot air at 70 ℃ until the surface of the screw is dried.
The treating agent comprises zirconium nitrate, citric acid, zinc nitrate, diisooctyl sebacate, sodium methallyl sulfonate, hydroxymethyl cellulose, ethylenediamine, ethanol and deionized water.
The zirconium nitrate: citric acid: zinc nitrate: diisooctyl sebacate: sodium methallyl sulfonate: hydroxymethyl cellulose: ethylene diamine: ethanol: the weight ratio of the deionized water is 2: 5: 2: 1: 2: 1: 3: 10: 55.
and mixing ethanol and deionized water, adding zirconium nitrate, citric acid and zinc nitrate, uniformly stirring, sequentially adding the rest materials, and stirring at 80RPM for 30min to obtain the treating agent.
And ultrasonic hardening, namely putting the screw subjected to surface treatment into an ultrasonic impact processing device, and performing ultrasonic hardening treatment on the surface of the screw.
The ultrasonic impact processing device is provided with an ultrasonic tool bit, the contact pressure of the ultrasonic tool bit and the surface of the screw is 20-30 MPa, the current value of an ultrasonic generator is 2.0A, and the rotating linear speed of the outer surface of the screw is 10 m/min.
And the coating spraying comprises spraying, curing and forming.
And the spraying step is to uniformly spray a coating agent on the surface of the screw rod after the ultrasonic hardening.
The coating agent comprises perfluoroalkoxy resin, epoxy resin, nano silicon carbide, nano zirconium silicate, manganese powder, nickel powder, silicon nitride, chromium oxide, sodium dodecyl sulfate and methanol.
The perfluoroalkoxy resin: epoxy resin: nano silicon carbide: nano zirconium silicate: manganese powder: nickel powder: silicon nitride: chromium oxide: sodium lauryl sulfate: the weight ratio of methanol is 1: 5: 3: 5: 5: 3: 3: 5: 2: 60.
the perfluoroalkoxy resin had a melt flow index of 2.6 (372 ℃/5.0 kg) and a particle size of 30 μm.
The epoxy value of the epoxy resin is 0.35.
The nano silicon carbide is silanization modified nano silicon carbide. The nano silicon carbide is prepared by pickling nano silicon carbide, removing impurities, putting the nano silicon carbide into a mixed solution of vinyl trimethoxy silane and acetone, stirring the mixture for 3 hours at 200RPM and drying the mixture.
And (3) removing impurities by acid washing, soaking the nano silicon carbide for 1 hour by adopting 2 times of acetic acid with volume of 8%, and then leaching the nano silicon carbide by adopting 5 times of deionized water.
The vinyl trimethoxy silane: the weight ratio of acetone was 1: 15.
The particle size range of the nano silicon carbide and the nano zirconium silicate is 150 nm.
The particle size range of the manganese powder, the nickel powder, the silicon nitride and the chromium oxide is 2 mu m.
The coating agent is prepared by uniformly mixing the perfluoroalkoxy resin, the epoxy resin, the sodium dodecyl sulfate and the methanol, sequentially adding the rest materials, and uniformly mixing.
And (3) curing, namely placing the sprayed screw in a vacuum environment at the temperature of 420 ℃ for high-temperature curing for 2 h.
And (3) curing, wherein the thickness of the coating after curing is 250 mu m.
And (3) molding, namely placing the solidified screw in a vacuum environment at 30 ℃ and naturally cooling.
In the preparation method of the cylindrical octabromoether particles, in the process of octabromoether granulation, octabromoether does not adhere to a screw in granulation equipment; effectively avoiding the blocking phenomenon of octabromoether granulation equipment, and ensuring stable quality of octabromoether granules; the hardness of the screw of the bar extruder is improved to 65HRC from the original 46HRC after the re-processing, and the durability is strong; the screw coating of the extruder is wear-resistant and has low loss rate, and the continuous granulation production is carried out for 10000h, and the loss of the coating is 0.13 percent.
Comparative example 1
The technical scheme of the embodiment 2 is adopted, and the difference is that the steps of liquid spraying and dipping in the surface treatment are eliminated; the "ultrasonic hardening" step was deleted.
According to the preparation method of the cylindrical octabromoether particles in the comparative example, the screw hardness of the strip extruding machine is 53 HRC; 10000h for continuous granulation production, and the loss of the screw coating of the extruder is 0.31 percent.
Comparative example 2
The technical scheme of the embodiment 2 is adopted, and the difference is that the silanization modified nano silicon carbide adopted in the step of coating spraying is replaced by the commercially available silicon carbide with the same grain size specification.
According to the preparation method of the cylindrical octabromoether particles in the comparative example, the screw hardness of the strip extruding machine is 61 HRC; 10000h for continuous granulation production, and the loss of the screw coating of the extruder is 0.57 percent.
All percentages used in the present invention are mass percentages unless otherwise indicated.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. The preparation method of the cylindrical octabromoether particles is characterized by comprising the following steps:
(1) adding water in a predetermined part into the octabromoether product, and uniformly mixing to obtain a mixed material;
(2) conveying the conveyed mixed material into a strip extruding machine according to a preset feeding speed, and extruding and granulating;
(3) and air-cooling the extruded octabromoether particles to form the extruded octabromoether particles.
2. The method for preparing cylindrical octabromoether particles according to claim 1, wherein the moisture content of the mixed material is 30-35% wt.
3. The method for preparing cylindrical octabromoether particles according to claim 1, wherein the feeding speed is 300 to 400 Kg/h.
4. The method for preparing cylindrical octabromoether particles according to claim 1, wherein the air cooling is carried out, and the air volume is 10-2000M3/h。
5. The method for preparing cylindrical octabromoether particles according to claim 1, wherein the plodder is a single-screw or twin-screw type plodder;
in the strip extruder, the screw is prepared by firstly carrying out surface treatment on the outer surface of the screw, then carrying out ultrasonic hardening treatment and finally spraying a coating;
the surface treatment comprises the steps of liquid spraying and dipping;
the spray solution is used for preheating the surface of the dried screw rod with the surface impurities removed to 140-160 ℃, and uniformly spraying a predetermined part of spray solution on the surface of the screw rod;
the spraying liquid comprises sodium chloride, zinc nitrate and deionized water;
the sodium chloride: zinc nitrate: the deionized water has a weight ratio of 8-10: 2-3: 90-100;
the spraying amount of the spraying is as follows: 8-20 ml of the water is sprayed on the surface area of each square centimeter.
6. The preparation method of the cylindrical octabromoether particles according to claim 5, wherein in the impregnation step, the screw after the liquid spraying is immersed into a treatment agent with 2 times of volume, the treatment agent is heated to 60-70 ℃, is kept stand for 60-90 min and then is taken out, and is blown by hot air at 70 ℃ until the surface of the screw is dried;
the treating agent comprises zirconium nitrate, citric acid, zinc nitrate, diisooctyl sebacate, sodium methallylsulfonate, hydroxymethyl cellulose, ethylenediamine, ethanol and deionized water;
the zirconium nitrate: citric acid: zinc nitrate: diisooctyl sebacate: sodium methallyl sulfonate: hydroxymethyl cellulose: ethylene diamine: ethanol: the deionized water has a weight ratio of 2-3: 3-5: 2-3: 1-2: 2-3: 1-2: 2-3: 10-15: 50-60.
7. The preparation method of cylindrical octabromoether particles according to claim 5, wherein in the ultrasonic hardening, the contact pressure between an ultrasonic tool bit and the surface of the screw is 20-30 MPa, the current value of an ultrasonic generator is 1.5-2.0A, and the linear speed of rotation of the outer surface of the screw is 5-12 m/min.
8. The method for preparing cylindrical octabromoether particles according to claim 5, wherein the coating is sprayed, including spraying, curing, forming;
the spraying step is to uniformly spray a coating agent on the surface of the screw rod after the ultrasonic hardening;
the coating agent comprises perfluoroalkoxy resin, epoxy resin, nano silicon carbide, nano zirconium silicate, manganese powder, nickel powder, silicon nitride, chromium oxide, sodium dodecyl sulfate and methanol;
the perfluoroalkoxy resin: epoxy resin: nano silicon carbide: nano zirconium silicate: manganese powder: nickel powder: silicon nitride: chromium oxide: sodium lauryl sulfate: the weight ratio of methanol is 1: 4-6: 3-5: 3-5: 3-5: 2-3: 3-5: 3-5: 2-3: 35-60 parts of;
and (3) curing, wherein the thickness of the coating after curing is 200-300 mu m.
9. The method for preparing cylindrical octabromoether particles according to claim 8, wherein the nano silicon carbide is silanized and modified;
the nano silicon carbide is prepared by pickling and removing impurities, then placing the nano silicon carbide into a mixed solution of vinyltrimethoxysilane and acetone, stirring the mixture for 3 hours at 200RPM and drying the mixture;
and (3) removing impurities by acid washing, soaking the nano silicon carbide for 1-2 hours by adopting 2 times of acetic acid with volume of 8%, and leaching the nano silicon carbide by adopting 5 times of deionized water.
10. The method of claim 9, wherein the ratio of vinyltrimethoxysilane: the weight part ratio of acetone is 1: 15;
the particle size of the nano silicon carbide and the nano zirconium silicate ranges from 100nm to 200 nm;
the particle size of the manganese powder, the nickel powder, the silicon nitride and the chromium oxide ranges from 1 to 2 mu m.
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