WO2020224182A1 - 一种防喷霜析出的环保型阻燃塑料母料及制备方法 - Google Patents
一种防喷霜析出的环保型阻燃塑料母料及制备方法 Download PDFInfo
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- 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
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/10—Homopolymers or copolymers of propene
- C08J2423/12—Polypropene
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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
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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
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
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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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3477—Six-membered rings
- C08K5/3492—Triazines
- C08K5/34928—Salts
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
Definitions
- the invention relates to the technical field of flame-retardant plastics, in particular to an environment-friendly flame-retardant plastic master batch capable of preventing blooming and precipitation and a preparation method.
- plastics are mainly non-polar materials, and flame retardants are generally fillers or polar melts, when flame retardants are used in plastics, the compatibility of flame retardants with plastics is poor, and it is easy to bloom and precipitate, which not only affects The appearance of the product is glossy, and it will cause the strength of the plastic product to deteriorate.
- Plastic products with higher requirements for flame retardants are generally electrical products, and more flame retardants need to be added. The precipitation of flame retardants seriously affects the appearance quality of plastic products. In addition, with the precipitation of flame retardants, the flame retardant function of plastic products is reduced.
- polypropylene Due to its excellent processability, polypropylene can be used to replace advanced engineering plastics by enhancing its rigidity and strength, and is gradually being applied on a large scale in the fields of automobiles and household appliances.
- polypropylene is easy to process, its flame retardancy becomes a problem.
- polypropylene has a low fire resistance temperature and is flammable.
- the flame retardant is easy to migrate and precipitate in the polypropylene system due to the poor compatibility of the flame retardant with polypropylene.
- the flame retardant often precipitates on the surface of injection molded products due to the influence of heat. Produce silky white strips, affecting the appearance of the product.
- Some insoluble micro-particle flame retardants are easy to migrate to form bloom on the surface of the product, which directly affects the surface finish of the product. According to the prior art, it is mainly to reduce the precipitation of the flame retardant by increasing the interface compatibility of the flame retardant and the resin matrix.
- Chinese Patent Publication No. CN101891952B discloses a non-precipitating flame-retardant masterbatch, which solves the problem of the precipitation of flame retardants by adding modified polyamide as a compatibilizer for the defect of precipitation of brominated flame retardants.
- brominated flame retardants will produce toxic and harmful gases during the production process, pollute the environment, have production safety problems, and are relatively expensive.
- Ammonium polyphosphate is a phosphorus and nitrogen-based special intumescent inorganic flame retardant, which has been used in plastics, coatings and other fields.
- the flame retardant P-N has high content of flame-retardant elements, good thermal stability, high flame-retardant efficiency and lasting flame-retardant performance.
- intumescent flame retardants with APP as the main raw material have become a hot spot in research and development. Therefore, ammonium polyphosphate becomes a better flame retardant.
- Ammonium polyphosphate has lower cost than brominated flame retardants and is environmentally friendly.
- ammonium polyphosphate when used in plastic products, there is a more serious precipitation than brominated flame retardants, and ammonium polyphosphate is sensitive to water. When used in flame retardants for electrical products, there is a risk of deterioration in a humid environment. In addition, ammonium polyphosphate releases a certain amount of small molecules during thermal processing of conventional plastics. Therefore, in order to promote the flame-retardant application of ammonium polyphosphate in the plastics field, it is necessary to solve the problems of heat resistance, water resistance and blooming of ammonium polyphosphate in plastics. However, it is difficult to fundamentally solve the precipitation problem of ammonium polyphosphate by using the existing single compatibilizer technology.
- the present invention proposes an environmentally friendly flame-retardant plastic master batch that prevents blooming and precipitation and its preparation method.
- the present invention provides a preparation method of an environmentally friendly flame-retardant plastic master batch that prevents blooming and precipitation, which is characterized in that the specific preparation method is as follows:
- step (1) Add the composite micropowder to a closed container, fill the closed container with ammonia gas, control the temperature of the container to 35-45°C, and stir at high speed, and spray the aluminum sulfate composite liquid obtained in step (1) into the closed container with a high-pressure spray gun ,
- the surface of the suspended composite powder is in contact with the aluminum sulfate composite liquid, and the ammonia gas gradually dissolves in the water to form a weak alkaline environment, which promotes the formation of aluminum hydroxide coating on the surface of the composite powder; discharge from a closed container and fluidize at 100-120°C
- the bed is dried to obtain a composite modified ammonium polyphosphate flame retardant;
- step (4) The material cooled in step (4) is sent to the twin-screw extruder through the conveying pipeline, and an environmentally friendly flame-retardant plastic masterbatch that prevents blooming and precipitation is obtained through extrusion and granulation.
- Ammonium polyphosphate is an excellent flame retardant.
- the flame retardant mechanism is to generate a strong dehydrating agent for polyphosphoric acid after being dehydrated by heating, which promotes the dehydration of organic surfaces to form carbides, plus the non-volatile phosphorus oxides and polyphosphoric acid produced Covering the surface of the substrate, while containing nitrogen elements, thermal decomposition releases carbon dioxide, nitrogen, ammonia and other gases, these gases are not easy to burn, blocking the supply of oxygen. It is a cheap and excellent environmentally friendly halogen-free flame retardant.
- APP total ammonium polyphosphate
- the ammonium polyphosphate in step (2) is long-chain ammonium polyphosphate with n>500, which is relatively stable at normal plastic processing temperature, but begins to decompose into phosphoric acid and ammonia above 300°C, and further Dehydrated to form polyphosphoric acid or polymetaphosphoric acid, which exhibits excellent flame retardancy.
- Melamine polyphosphate is an additive flame retardant with a wide range of applications. It is generally white, fine powder, and has a decomposition temperature of> 300°C.
- the PN synergy among them shows excellent flame retardancy, and its outstanding The advantages are good thermal stability, insoluble in water, low smoky, and non-hygroscopic. When used in plastics, it has excellent high temperature processing performance. It forms a foamed coke layer during endothermic decomposition and covers the surface of the burning material to isolate the air.
- the vaporized melamine provides an inert gas source and can dilute oxygen. And the concentration of combustible gas produced by the decomposition of high polymer, so as to achieve the purpose of flame retardant. Blended with ammonium polyphosphate shows excellent flame retardancy.
- the melamine phosphate in step (2) is a commercially available melamine polyphosphate with a phosphorus content of more than 14% and a nitrogen content of more than 38%.
- Step (2) The micronizer adopts a conventional micronizer to micronize and composite the commercially available large-particle ammonium polyphosphate and melamine polyphosphate into composite micropowders with a particle size of less than 5 ⁇ m.
- the grinding type miniaturization machine is carefully used.
- the micromachine adopts a vortex jet mill.
- the speed of the high-speed stirring in step (3) is 800-1200 rpm, and it is preferable to fully suspend the composite micropowder so that the atomized aluminum sulfate composite liquid can fully contact.
- the amount of composite micropowder added in the closed container does not exceed 1/3 of the volume of the closed container.
- the closed container is filled with ammonia gas, the ammonia gas environment of the closed container is maintained, and ammonia gas is continuously filled to ensure that the ammonia gas pressure is 0.01 MPa.
- the ammonia gas gradually dissolves in the water and uniformly generates aluminum hydroxide, thereby forming a uniform coating layer on the surface of the ammonium polyphosphate and melamine polyphosphate composite micropowder; different from the direct addition of ammonia, the direct addition of ammonia will cause the rapid and violent formation of aluminum hydroxide , It is difficult to coat the powder uniformly.
- the injection amount of the aluminum sulfate composite liquid in step (3) is controlled to be 0.5-1 times the mass of the composite powder.
- the pressure of the high-pressure spray gun is 0.6-0.8MPa.
- the filler in step (4) is selected from at least one of talc powder, wollastonite powder, montmorillonite, and mica powder.
- the lubricating aid in step (4) is selected from polyethylene wax and stearic acid powder.
- the silicone oil in step (4) is selected from at least one of methyl trifluoropropyl silicone oil, methyl ethoxy silicone oil, methyl silicone oil, and ethyl silicone oil; its excellent hydrophobicity increases the composite modified polyphosphoric acid
- the compatibility of ammonium flame retardant and resin is beneficial to reduce the precipitation of flame retardant.
- the compatibilizer in step (4) is maleic anhydride grafted polypropylene, maleic anhydride grafted polyethylene, maleic anhydride grafted ethylene-octene copolymer, maleic anhydride grafted ethylene-propylene- One of diene copolymers.
- the high-speed stirring speed is 400-900 rpm, and the low-speed stirring speed is 80-100 rpm.
- the twin-screw extruder in step (5) is a counter-rotating twin-screw extruder with a screw diameter of 45 mm and a length-to-diameter ratio of 20:1.
- the screw is set with 5 heating zones from feeding to discharging, the temperature is in order: zone 1 100-120°C, zone 2 150-160°C, zone 3 180-190°C, zone 4 160-170°C, zone 5 130-140 °C; Use air-cooled die surface to cut pellets.
- the short-length-to-length ratio and counter-rotating twin-screw extruder has less shear to the material, which can avoid the premature decomposition of the composite modified ammonium polyphosphate flame retardant caused by high shear.
- the present invention further provides an environmentally friendly flame-retardant plastic master batch prepared by the above method that prevents blooming and precipitation.
- the present invention makes ammonium polyphosphate and melamine polyphosphate composite micronized, and coats the surface of the micronized composite powder to form an aluminum hydroxide coating. While forming the aluminum hydroxide coating film, the silicone powder is formed in the coating film. On the one hand, aluminum hydroxide is coated with ammonium polyphosphate and melamine polyphosphate composite powder, so that the ammonium polyphosphate has good heat resistance.
- the aluminum hydroxide coating increases the moisture resistance of ammonium polyphosphate, and will not be degraded by moisture when used in electrical plastics; It is important that the disperse silicone powder is stably coated on the surface of ammonium polyphosphate through the conversion of aluminum salt into aluminum hydroxide coating to give ammonium polyphosphate excellent hydrophobicity, thereby enhancing the flame retardant in the plastic In particular, the silicone powder has good stability and non-migration. The stable coating of ammonium polyphosphate can effectively prevent its blooming and precipitation.
- the present invention forms an aluminum hydroxide coating on the surface of ammonium polyphosphate and melamine polyphosphate composite micropowder during the process of forming aluminum hydroxide from aluminum salt, and combines the silicone
- the powder is stably coated on the surface of ammonium polyphosphate and melamine polyphosphate composite micropowder. It greatly increases the compatibility of the composite micropowder and the plastic, and effectively inhibits blooming and precipitation; further, the coated aluminum hydroxide is a flame-retardant functional material, which effectively synergizes the flame-retardant function.
- an environmentally-friendly flame-retardant plastic masterbatch capable of preventing blooming and precipitation and a preparation method of the present invention have outstanding features and excellent effects in:
- ammonium polyphosphate and melamine polyphosphate are compounded and micronized, and the surface of the micronized composite powder is coated to form an aluminum hydroxide coating film. While forming the aluminum hydroxide coating film, the silicone powder is formed in the coating film. In the film, aluminum hydroxide is coated with ammonium polyphosphate and melamine polyphosphate composite micropowder, so that ammonium polyphosphate has good heat resistance, makes it easy to be processed in plastic systems by thermoplastics, and reduces the release of small molecules caused by thermal processing.
- the invention is coated with aluminum hydroxide to increase the moisture resistance of ammonium polyphosphate, and will not be degraded by moisture when used in electrical plastics.
- the aluminum salt is converted into aluminum hydroxide coating
- the dispersed silicone powder is stably coated on the surface of ammonium polyphosphate in advance, and the ammonium polyphosphate is given excellent hydrophobicity, thereby enhancing the flame retardant in plastics. Dispersibility and compatibility.
- silicone powder has good stability and non-migration. After stabilizing the coated ammonium polyphosphate, it can effectively prevent its blooming and precipitation.
- the preparation method of the present invention is simple, the process is easy to control, the effect is excellent, and it is suitable for large-scale production.
- the obtained plastic flame-retardant masterbatch is suitable for adding to various plastics to improve the flame retardancy and prevent the blooming and precipitation of flame retardants, especially It has better effect in polypropylene and polyamide.
- Figure 1 Scanning electron micrograph of a test board prepared by using the flame-retardant masterbatch of Example 1 for PP injection molding.
- Figure 2 Low-power scanning electron micrograph of a test board prepared by using the flame-retardant masterbatch of Comparative Example 1 for PP injection molding.
- Figure 3 High-magnification scanning electron micrograph of a test board prepared by using the flame-retardant masterbatch of Comparative Example 1 for PP injection molding.
- Ammonia gas environment and continuously filled with ammonia gas, to ensure that the ammonia gas pressure is 0.01MPa, the ammonia gas gradually dissolves in the water to form a weak alkaline environment, which promotes the aluminum sulfate salt solution on the surface of the composite powder to form an aluminum hydroxide coating layer; put it from a closed container
- the material is dried in a fluidized bed at 100°C to obtain a composite modified ammonium polyphosphate flame retardant; the injection amount of the aluminum sulfate composite liquid is controlled to 0.5 times the quality of the composite powder;
- step (4) The material cooled in step (4) is fed into a counter-rotating twin-screw extruder with a screw diameter of 45 mm and a length-to-diameter ratio of 20:1 through the conveying pipeline.
- the screw sets 5 heating zones from feeding to discharging, the temperature is in order: 120°C in zone 1, 150°C in zone 2, 180°C in zone 3, 160°C in zone 4, and 140°C in zone 5;
- the cold die surface is cut into pellets to obtain an environmentally friendly flame-retardant plastic master batch that prevents blooming and precipitation.
- the flame-retardant plastic master batch obtained in Example 1 and PPK1708 resin were mixed uniformly at a mass ratio of 2:10, and injection molded into a flat test sample, numbered 1#, injection temperature: 200°C in zone 1, 210°C in zone 2, and zone 3 230°C; 240°C in zone 4.
- the obtained test board was placed at 80°C for 24 hours, and the surface of the test board was observed with a scanning electron microscope. As shown in Figure 1, the board surface had good gloss and no precipitates.
- Ammonia gas environment and continuously filled with ammonia gas, to ensure that the ammonia gas pressure is 0.01MPa, the ammonia gas gradually dissolves in the water to form a weak alkaline environment, which promotes the aluminum sulfate salt solution on the surface of the composite powder to form an aluminum hydroxide coating layer; put it from a closed container
- the material is dried in a fluidized bed at 120°C to obtain a composite modified ammonium polyphosphate flame retardant; the injection amount of the aluminum sulfate composite liquid is controlled at 0.5 times the quality of the composite powder;
- step (4) The material cooled in step (4) is fed into a counter-rotating twin-screw extruder with a screw diameter of 45 mm and a length-to-diameter ratio of 20:1 through the conveying pipeline.
- the screw is set with 5 heating zones from feeding to discharging, the temperature is in order: 100°C in zone 1, 150°C in zone 2, 180°C in zone 3, 160°C in zone 4, and 140°C in zone 5;
- the cold die surface is cut into pellets to obtain an environmentally friendly flame-retardant plastic master batch that prevents blooming and precipitation.
- the flame-retardant plastic master batch obtained in Example 2 and PPK1708 resin were mixed uniformly at a mass ratio of 2:10, and injection molded into a flat test sample with a thickness of 16mm, numbered 2#, injection temperature: zone 1 200°C; zone 2 210°C ; Zone 3 230°C; Zone 4 240°C.
- UL 94-2006 test vertical combustion is adopted.
- the instrument uses UL94 horizontal and vertical combustion test box, and the measured flame retardant level reaches V0.
- Ammonia gas environment and continuously filled with ammonia gas, to ensure that the ammonia gas pressure is 0.01MPa, the ammonia gas gradually dissolves in the water to form a weak alkaline environment, which promotes the aluminum sulfate salt solution on the surface of the composite powder to form an aluminum hydroxide coating layer; put it from a closed container
- the material is dried in a fluidized bed at 120°C to obtain a composite modified ammonium polyphosphate flame retardant; the injection amount of the aluminum sulfate composite liquid is controlled at 0.8 times the quality of the composite powder;
- step (4) The material cooled in step (4) is fed into a counter-rotating twin-screw extruder with a screw diameter of 45 mm and a length-to-diameter ratio of 20:1 through the conveying pipeline.
- the screw sets 5 heating zones from feeding to discharging.
- the temperature is in order: 120°C in zone 1, 160°C in zone 2, 190°C in zone 3, 170°C in zone 4, and 140°C in zone 5;
- the cold die surface is cut into pellets to obtain an environmentally friendly flame-retardant plastic master batch that prevents blooming and precipitation.
- Ammonia gas environment and continuously filled with ammonia gas, to ensure that the ammonia gas pressure is 0.01MPa, the ammonia gas gradually dissolves in the water to form a weak alkaline environment, which promotes the aluminum sulfate salt solution on the surface of the composite powder to form an aluminum hydroxide coating layer; put it from a closed container
- the material is dried in a fluidized bed at 100°C to obtain a composite modified ammonium polyphosphate flame retardant; the injection amount of the aluminum sulfate composite liquid is controlled to 0.5 times the quality of the composite powder;
- step (4) The material cooled in step (4) is fed into a counter-rotating twin-screw extruder with a screw diameter of 45 mm and a length-to-diameter ratio of 20:1 through the conveying pipeline.
- the screw sets 5 heating zones from feeding to discharging, the temperature is in order: 120°C in zone 1, 150°C in zone 2, 180°C in zone 3, 160°C in zone 4, and 140°C in zone 5; Cut pellets on the cold die surface to obtain an environmentally friendly flame-retardant plastic master batch.
- Comparative Example 1 did not add silicone powder to the aluminum sulfate solution, but added the silicone powder after the aluminum hydroxide coating was formed, so that a single aluminum hydroxide coating was formed, instead of adding The silicone powder is tightly coated on the surface of the composite powder, which makes the flame retardant easy to bloom and precipitate in the plastic.
- the flame-retardant plastic master batch obtained in Comparative Example 1 and PPK1708 resin were mixed uniformly at a mass ratio of 2:10, and injection molded into a flat test sample, numbered 3#, injection temperature: 200°C in zone 1, 210°C in zone 2, and zone 3 230°C; 240°C in zone 4. Place the obtained test board at 80°C for 24h, and observe the surface of the test board with a scanning electron microscope. As shown in Figure 2, the plate surface has obvious crystal points. Through further magnification observation, as shown in Figure 3, the precipitated surface The crystal point size is close to 5 ⁇ m, which affects the gloss and smoothness of plastic products.
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Abstract
本发明涉及阻燃塑料技术领域,具体涉及一种防喷霜析出的环保型阻燃塑料母料及制备方法。将聚磷酸铵、三聚氰胺聚磷酸盐复合微细化,并在微细化复合微粉表面包覆形成氢氧化铝包膜,在形成氢氧化铝包覆膜的同时将硅酮粉形成在包膜中,然后与填料、润滑助剂、硅油、聚丙烯、相容剂经双螺杆挤出造粒得到一种防喷霜析出的环保型阻燃塑料母料。通过铝盐液转化为氢氧化铝包膜,将分散的硅酮粉预先稳定包覆在聚磷酸铵的表面,赋予聚磷酸铵优异的疏水性,从而增强阻燃剂在塑料中的分散性和相容性,特别的,硅酮粉具有良好的稳定性和非迁移性,稳定包膜聚磷酸铵后可以有效阻止其喷霜析出。
Description
本发明涉及阻燃塑料技术领域,具体涉及一种防喷霜析出的环保型阻燃塑料母料及制备方法。
由于塑料主要为非极性材料,而阻燃剂一般为填料或极性可熔化物,在将阻燃剂用于塑料时阻燃剂与塑料的相容性差,极易喷霜析出,不但影响制品的外观光泽度,而且会导致塑料制品强度劣化。对阻燃剂要求较高的塑料制品一般都是电器产品,需要加入较多的阻燃剂,阻燃剂的析出严重影响塑料制品的外观品质。另外,随着阻燃剂的析出,致使塑料制品阻燃功能降低。
聚丙烯由于具有优异的加工性,通过增强提高刚性和强度,用于替代高级工程塑料,在汽车和家用电器领域逐步大规模化应用。然而在聚丙烯易于加工的同时,其阻燃性成为问题。通常的,聚丙烯耐火温度低、易燃,在加入大量阻燃剂时,由于阻燃剂与聚丙烯的相容性较差,阻燃剂易于在聚丙烯体系中迁移析出。我们在将阻燃剂加入聚丙烯进行注塑加工时,由于受热影响,阻燃剂经常析出在注塑制品表面。产生丝状白条,影响制品的外观。一些非溶性微颗粒阻燃剂易于迁移在制品表面形成喷霜,直接影响制品表面的光洁度。根据现有技术,主要是通常通过增加阻燃剂与树脂基体界面相容性以减轻阻燃剂析出。如中国发明专利公开号CN101891952B公开了一种无析出阻燃母料,针对溴系阻燃剂以析出的缺陷,通过加入改性聚酰胺作为相容剂,解决了阻燃剂析出的问题。然而,随着阻燃剂技术的发展,溴系阻燃剂由于在生产过程中会产生有毒有害气体,污染环境,存在生产安全问题,而且价格较高。
聚磷酸铵(APP)是一种磷、氮系特效膨胀型无机阻燃剂,在塑料、涂料等领域已有应用。该阻燃剂P-N阻燃元素含量高,热稳定性好,阻燃效能高,阻燃性能持久。随着全球阻燃剂朝着环保无卤化方向发展,以APP为主原料的膨胀型阻燃剂已成为研究开发的热点。因此,聚磷酸铵成为较佳的阻燃剂。聚磷酸铵比溴系阻燃剂成本低,而且环保。但在用于塑料制品时存在比溴系阻燃剂更为严重的析出,而且聚磷酸铵对水敏感,在用于电器产品塑料的阻燃剂时,在潮湿环境存在劣化的风险。另外,在常规塑料热加工时聚磷酸铵会释放一定量的小分子。因此,为了推广聚磷酸铵在塑料领域的阻燃应用,必须解决聚磷酸铵在塑料中的耐热、耐水和析出喷霜问题。而采用现有单一的相容剂技术难以根本解决聚磷酸铵的析出问题。
发明内容
针对聚磷酸铵作为塑料阻燃剂存在析出喷霜的缺陷,为了推进聚磷酸铵阻燃剂大剂量用于塑料制品,本发明提出一种防喷霜析出的环保型阻燃塑料母料及的制备方法。通过在聚磷酸铵和三聚氰胺聚磷酸盐复合微粉表面包覆氢氧化铝再进行改性,以增强聚磷酸铵的耐水性和耐热稳定性,并有效防止喷霜析出。
为实现上述目的,本发明采用以下技术方案:
本发明提供一种防喷霜析出的环保型阻燃塑料母料的制备方法,其特征在于,具体制备方法如下:
(1)将硅酮粉与硫酸铝研磨,然后加入去离子水,得到分散硅酮粉的硫酸铝复合液备用;其中硅酮粉、硫酸铝、去离子水的质量比为1∶5∶20;
(2)将聚磷酸铵、三聚氰胺聚磷酸盐以质量比3∶1复合,经微细机处理得到粒径小于5μm的复合微粉;
(3)将复合微粉加入密闭容器,在密闭容器中充氨气,控制容器温度为35-45℃,并高速搅拌,将步骤(1)得到的硫酸铝复合液采用高压喷雾枪喷入密闭容器,悬浮的复合微粉表面与硫酸铝复合液接触,氨气逐步溶解在水中形成弱碱环境,促使复合微粉表面形成氢氧化铝包覆层;从密闭容器放料,在100-120℃的流化床干燥,得到复合改性聚磷酸铵阻燃剂;
(4)将40-50重量份复合改性聚磷酸铵阻燃剂、5-10重量份填料、0.5-1重量份润滑助剂、0.1-0.3重量份硅油加入高速混合机,在100-120℃高速搅拌处理15-20min,然后加入15-20重量份聚丙烯、5-10重量份相容剂低速搅拌混合3-5min,混合均匀,放料进入冷混机,低速搅拌冷却;
(5)经输送管路,将步骤(4)冷却的物料送入双螺杆挤出机,经挤出造粒得到一种防喷霜析出的环保型阻燃塑料母料。
聚磷酸铵(APP)是一种优异的阻燃剂,阻燃机理是受热脱水后生成聚磷酸强脱水剂,促使有机物表面脱水生成碳化物,加之生成的非挥发性磷的氧化物及聚磷酸对基材表面进行覆盖,同时含有氮元素,受热分解释放出二氧化碳、氮气、氨气等气体,这些气体不易燃烧,阻断了氧的供应。是一种廉价的优异的环保无卤阻燃剂。年费清单发罗总聚磷酸铵(APP)的结构通式为(NH4)
(n+2)PnO
(3n+1),当n=10-20,易水溶;n=20-100,水难溶,但对水敏感。
优选的,步骤(2)所述聚磷酸铵选用n>500的长链聚磷酸铵,其在常规塑料加工温度时较稳定,但在300℃以上开始分解成磷酸和氨,高于300℃进一步脱水形成聚磷酸或聚偏磷酸,表现优异的阻燃性。
三聚氰胺聚磷酸盐(MPP)是一种应用范围很广添加型阻燃剂,一般为白色、微细粉体,分解温度>300℃,其中的P-N协同性表现出优异的阻燃性,其突出的优点是热稳定性好,不溶于水,发烟性小,不吸湿。用于塑料时具有优异的耐高温加工性能,在吸热分解时生成泡沫状的焦碳层,覆盖在燃烧物的表面,起到隔绝空气的作用,汽化的三聚氰胺提供惰性气源,可稀释氧气和因高聚物分解而产生的可燃气体浓度,从而达到阻燃目的。配合聚磷酸铵表现优异的阻燃性。
优选的,步骤(2)所述三聚氰胺磷酸盐选用市售磷含量大于14%,氮含量大于38%的三聚氰胺聚磷酸盐。
步骤(2)所述微细机采用常规微细化机,将市售的大粒径聚磷酸铵、三聚氰胺聚磷酸盐微细化复合处理为粒径小于5μm的复合微粉。为了防止微细化处理时高温导致物料变性、团聚,谨慎采用研磨类微细化机。优选的,所述微细机采用涡旋气流粉碎机。
优选的,步骤(3)所述高速搅拌转速为800-1200rpm,较佳的使复合微粉充分悬浮,以便于雾化的硫酸铝复合液充分接触。在实际操作时,为了保证复合微粉充分悬浮,复合微粉在密闭容器的加入量不超过密闭容器容量的1/3。
优选的,步骤(3)在密闭容器中充氨气,维持密闭容器氨气环境,并不断充入氨气,保证氨气压力在0.01MPa,在雾化的硫酸铝复合液喷入时,氨气逐步溶解于水中,并均匀生成氢氧化铝,从而在聚磷酸铵、三聚氰胺聚磷酸盐复合微粉表面形成均匀的包覆层;不同于直接加氨水,直接加氨水会导致剧烈快速生成氢氧化铝,难以均匀的包覆微粉。
进一步优选的,步骤(3)所述硫酸铝复合液的喷入量控制在复合微粉质量的0.5-1倍。为了较佳的保证在复合微粉表面均匀形成氢氧化铝包覆层,高压喷雾枪压力为0.6-0.8MPa。
优选的,步骤(4)所述填料选用滑石粉、硅灰石粉、蒙脱土、云母粉中的至少一种。
优选的,步骤(4)所述润滑助剂选用聚乙烯蜡、硬脂酸粉中的一种。
优选的,步骤(4)所述硅油选用甲基三氟丙基硅油、甲基乙氧基硅油、甲基硅油、乙基硅油中的至少一种;其优异的疏水性增加复合改性聚磷酸铵阻燃剂与树脂的相容性,有利于降低阻燃剂的析出。
优选的,步骤(4)所述相容剂为马来酸酐接枝聚丙烯、马来酸酐接枝聚乙烯、马来酸酐接枝乙烯-辛烯共聚物、马来酸酐接枝乙烯-丙烯-二烯烃共聚物中的一种。
优选的,步骤(4)所述高速搅拌转速为400-900rpm,所述低速搅拌转速为80-100rpm。
优选的,步骤(5)所述双螺杆挤出机选用螺杆直径45mm、长径比20∶1的短长经比异向双螺杆挤出机。螺杆由进料到出料设置5个加热区,温度依次为:1区100-120℃、2区150-160℃、3区180-190℃、4区160-170℃、5区130-140℃;采用风冷模面切粒。短长经比、异向旋转的双螺杆挤出机对物料剪切较小,可以避免高剪切造成的复合改性聚磷酸铵阻燃剂提前分解。
本发明进一步提供由上述方法制备得到的一种防喷霜析出的环保型阻燃塑料母料。为了解决聚磷酸铵在塑料中作为阻燃剂存在喷霜析出的缺陷,本发明将聚磷酸铵、三聚氰胺聚磷酸盐复合微细化,并在微细化复合微粉表面包覆形成氢氧化铝包膜,在形成氢氧化铝包覆膜的同时将硅酮粉形成在包膜中,一方面,氢氧化铝包覆聚磷酸铵、三聚氰胺聚磷酸盐复合微粉,使得聚磷酸铵具有良好的耐热性,使其易于在塑料体系热塑加工,降低热加工造成的小分子释放;另一方面,通过氢氧化铝包覆,使得聚磷酸铵耐潮性能增加,不会在用于电器塑料时受潮劣化;更为重要的是,通过铝盐转化为氢氧化铝包膜,将分散的硅酮粉预先稳定包覆在聚磷酸铵的表面,赋予聚磷酸铵优异的疏水性,从而增强阻燃剂在塑料中的分散性和相容性,特别的,硅酮粉具有良好的稳定性和非迁移性,稳定包膜聚磷酸铵后可以有效阻止其喷霜析出。
相比于直接加入硅酮粉改性聚磷酸铵,本发明在铝盐形成氢氧化铝的过程中,在聚磷酸铵、三聚氰胺聚磷酸盐复合微粉表面形成氢氧化铝包膜,并将硅酮粉稳定包覆在聚磷酸铵、三聚氰胺聚磷酸盐复合微粉 表面。大幅增加了复合微粉与塑料的相容性,并有效抑制喷霜析出;进一步的所包覆的氢氧化铝为阻燃功能材料,有效协同阻燃功能的发挥。
本发明一种防喷霜析出的环保型阻燃塑料母料及制备方法,与现有技术相比,突出的特点和优异的效果体现在:
1、本发明将聚磷酸铵、三聚氰胺聚磷酸盐复合微细化,并在微细化复合微粉表面包覆形成氢氧化铝包膜,在形成氢氧化铝包覆膜的同时将硅酮粉形成在包膜中,氢氧化铝包覆聚磷酸铵、三聚氰胺聚磷酸盐复合微粉,使得聚磷酸铵具有良好的耐热性,使其易于在塑料体系热塑加工,降低热加工造成的小分子释放。
2、本发明通过氢氧化铝包覆,使得聚磷酸铵耐潮性能增加,不会在用于电器塑料时受潮劣化。
3、本发明通过铝盐转化为氢氧化铝包膜,将分散的硅酮粉预先稳定包覆在聚磷酸铵的表面,赋予聚磷酸铵优异的疏水性,从而增强阻燃剂在塑料中的分散性和相容性,特别的,硅酮粉具有良好的稳定性和非迁移性,稳定包膜聚磷酸铵后可以有效阻止其喷霜析出。
4、本发明制备方法简单,过程易控,效果优异,适合于规模化生产,得到的塑料阻燃母料适合于在各种塑料中加入提高阻燃性,防止阻燃剂喷霜析出,尤其在聚丙烯、聚酰胺中使用效果更佳。
附图1:实施例1阻燃母料用于PP注塑制备的测试板扫描电镜照片。
附图2:对比例1阻燃母料用于PP注塑制备的测试板的低倍扫描电镜照片。
附图3:对比例1阻燃母料用于PP注塑制备的测试板的高倍扫描电镜照片。
以下通过具体实施方式对本发明作进一步的详细说明,但不应将此理解为本发明的范围仅限于以下的实例。在不脱离本发明上述方法思想的情况下,根据本领域普通技术知识和惯用手段做出的各种替换或变更,均应包含在本发明的范围内。
实施例1
(1)将硅酮粉与硫酸铝研磨,然后加入去离子水,得到分散硅酮粉的硫酸铝复合液备用;其中硅酮粉、硫酸铝、去离子水的质量比为1∶5∶20;
(2)将n>500的长链聚磷酸铵、市售磷含量大于14%,氮含量大于38%的三聚氰胺聚磷酸盐以质量比3∶1复合,经涡旋气流粉碎机处理得到粒径小于5μm的复合微粉;
(3)将复合微粉加入密闭容器,保证复合微粉在密闭容器的加入量不超过密闭容器容量的1/3,在密闭容器中充氨气,控制容器温度为45℃,并以800rpm的高速搅拌,较佳的使复合微粉充分悬浮,将步骤(1)得到的硫酸铝复合液采用高压喷雾枪,压力为0.6MPa喷入密闭容器,悬浮的复合微粉表面与硫酸铝 复合液接触,维持密闭容器氨气环境,并不断充入氨气,保证氨气压力在0.01MPa,氨气逐步溶解在水中形成弱碱环境,促使复合微粉表面硫酸铝盐液形成氢氧化铝包覆层;从密闭容器放料,在100℃的流化床干燥,得到复合改性聚磷酸铵阻燃剂;硫酸铝复合液的喷入量控制在复合微粉质量的0.5倍;
(4)将40重量份复合改性聚磷酸铵阻燃剂、5重量份滑石粉、0.5重量份聚乙烯蜡、0.1重量份甲基三氟丙基硅油加入高速混合机,在100℃、搅拌转速400rpm高速搅拌处理15min,然后加入15重量份聚丙烯、50重量份相容剂马来酸酐接枝聚丙烯以80rpm低速搅拌混合3min,混合均匀,放料进入冷混机,低速搅拌冷却至室温;
(5)经输送管路,将步骤(4)冷却的物料送入螺杆直径45mm、长径比20∶1的短长经比异向双螺杆挤出机。螺杆由进料到出料设置5个加热区,温度依次为:1区120℃、2区150℃、3区180℃、4区160℃、5区140℃;经挤出造粒,采用风冷模面切粒,得到一种防喷霜析出的环保型阻燃塑料母料。
将实施例1得到的阻燃塑料母粒料与PPK1708树脂以质量比2∶10混合均匀,注塑为平板测试样,编号为1#,注塑温度:1区200℃;2区210℃;3区230℃;4区240℃。将得到的测试板在80℃条件下放置24h,利用扫面电镜观察测试板表面,如附图1所示,板面光泽较好,无析出物。
实施例2
(1)将硅酮粉与硫酸铝研磨,然后加入去离子水,得到分散硅酮粉的硫酸铝复合液备用;其中硅酮粉、硫酸铝、去离子水的质量比为1∶5∶20;
(2)将n>500的长链聚磷酸铵、市售磷含量大于14%,氮含量大于38%的三聚氰胺聚磷酸盐以质量比3∶1复合,经涡旋气流粉碎机处理得到粒径小于5μm的复合微粉;
(3)将复合微粉加入密闭容器,保证复合微粉在密闭容器的加入量不超过密闭容器容量的1/3,在密闭容器中充氨气,控制容器温度为35℃,并以1200rpm的高速搅拌,较佳的使复合微粉充分悬浮,将步骤(1)得到的硫酸铝复合液采用高压喷雾枪,压力为0.8MPa喷入密闭容器,悬浮的复合微粉表面与硫酸铝复合液接触,维持密闭容器氨气环境,并不断充入氨气,保证氨气压力在0.01MPa,氨气逐步溶解在水中形成弱碱环境,促使复合微粉表面硫酸铝盐液形成氢氧化铝包覆层;从密闭容器放料,在120℃的流化床干燥,得到复合改性聚磷酸铵阻燃剂;硫酸铝复合液的喷入量控制在复合微粉质量的0.5倍;
(4)将50重量份复合改性聚磷酸铵阻燃剂、10重量份硅灰石粉、1重量份硬脂酸、0.2重量份甲基硅油加入高速混合机,在120℃、搅拌转速800rpm高速搅拌处理20min,然后加入20重量份聚丙烯、10重量份相容剂马来酸酐接枝聚乙烯以100rpm低速搅拌混合5min,混合均匀,放料进入冷混机,低速搅拌冷却;
(5)经输送管路,将步骤(4)冷却的物料送入螺杆直径45mm、长径比20∶1的短长经比异向双螺杆挤出机。螺杆由进料到出料设置5个加热区,温度依次为:1区100℃、2区150℃、3区180℃、4区160℃、 5区140℃;经挤出造粒,采用风冷模面切粒,得到一种防喷霜析出的环保型阻燃塑料母料。
将实施例2得到的阻燃塑料母粒料与PPK1708树脂以质量比2∶10混合均匀,注塑为厚度16mm的平板测试样,编号为2#,注塑温度:1区200℃;2区210℃;3区230℃;4区240℃。按UL 94-2006测试,采用垂直燃烧。仪器采用UL94水平垂直燃烧试验箱,测得阻燃级别达到V0级。
实施例3
(1)将硅酮粉与硫酸铝研磨,然后加入去离子水,得到分散硅酮粉的硫酸铝复合液备用;其中硅酮粉、硫酸铝、去离子水的质量比为1∶5∶20;
(2)将n>500的长链聚磷酸铵、市售磷含量大于14%,氮含量大于38%的三聚氰胺聚磷酸盐以质量比3∶1复合,经涡旋气流粉碎机处理得到粒径小于5μm的复合微粉;
(3)将复合微粉加入密闭容器,保证复合微粉在密闭容器的加入量不超过密闭容器容量的1/3,在密闭容器中充氨气,控制容器温度为45℃,并以1200rpm的高速搅拌,较佳的使复合微粉充分悬浮,将步骤(1)得到的硫酸铝复合液采用高压喷雾枪,压力为0.8MPa喷入密闭容器,悬浮的复合微粉表面与硫酸铝复合液接触,维持密闭容器氨气环境,并不断充入氨气,保证氨气压力在0.01MPa,氨气逐步溶解在水中形成弱碱环境,促使复合微粉表面硫酸铝盐液形成氢氧化铝包覆层;从密闭容器放料,在120℃的流化床干燥,得到复合改性聚磷酸铵阻燃剂;硫酸铝复合液的喷入量控制在复合微粉质量的0.8倍;
(4)将50重量份复合改性聚磷酸铵阻燃剂、5重量份云母粉、0.5重量份聚乙烯蜡、0.3重量份甲基乙氧基硅油加入高速混合机,在100℃、搅拌转速900rpm高速搅拌处理20min,然后加入15重量份聚丙烯、5重量份相容剂马来酸酐接枝乙烯-辛烯共聚物以80rpm低速搅拌混合5min,混合均匀,放料进入冷混机,低速搅拌冷却;
(5)经输送管路,将步骤(4)冷却的物料送入螺杆直径45mm、长径比20∶1的短长经比异向双螺杆挤出机。螺杆由进料到出料设置5个加热区,温度依次为:1区120℃、2区160℃、3区190℃、4区170℃、5区140℃;经挤出造粒,采用风冷模面切粒,得到一种防喷霜析出的环保型阻燃塑料母料。
对比例1
(1)将硫酸铝加入去离子水,得到硫酸铝复合液备用;其中硫酸铝、去离子水的质量比为5∶20;
(2)将n>500的长链聚磷酸铵、市售磷含量大于14%,氮含量大于38%的三聚氰胺聚磷酸盐以质量比3∶1复合,经涡旋气流粉碎机处理得到粒径小于5μm的复合微粉;
(3)将复合微粉加入密闭容器,保证复合微粉在密闭容器的加入量不超过密闭容器容量的1/3,在密闭容器中充氨气,控制容器温度为45℃,并以800rpm的高速搅拌,较佳的使复合微粉充分悬浮,将步骤(1)得到的硫酸铝复合液采用高压喷雾枪,压力为0.6MPa喷入密闭容器,悬浮的复合微粉表面与硫酸铝复合液接触,维持密闭容器氨气环境,并不断充入氨气,保证氨气压力在0.01MPa,氨气逐步溶解在水中形 成弱碱环境,促使复合微粉表面硫酸铝盐液形成氢氧化铝包覆层;从密闭容器放料,在100℃的流化床干燥,得到复合改性聚磷酸铵阻燃剂;硫酸铝复合液的喷入量控制在复合微粉质量的0.5倍;
(4)将40重量份复合改性聚磷酸铵阻燃剂、1重量份硅酮粉、5重量份滑石粉、0.5重量份聚乙烯蜡、0.1重量份甲基三氟丙基硅油加入高速混合机,在100℃、搅拌转速400rpm高速搅拌处理15min,然后加入15重量份聚丙烯、50重量份相容剂马来酸酐接枝聚丙烯以80rpm低速搅拌混合3min,混合均匀,放料进入冷混机,低速搅拌冷却至室温;
(5)经输送管路,将步骤(4)冷却的物料送入螺杆直径45mm、长径比20∶1的短长经比异向双螺杆挤出机。螺杆由进料到出料设置5个加热区,温度依次为:1区120℃、2区150℃、3区180℃、4区160℃、5区140℃;经挤出造粒,采用风冷模面切粒,得到一种环保型阻燃塑料母料。
相比于实施例1,对比例1没有在硫酸铝液中加入硅酮粉,而是形成氢氧化铝包膜后再加入硅酮粉,使得形成了单一的氢氧化铝包膜,而没有将硅酮粉紧密包覆在复合微粉表面,使得阻燃剂在塑料中容易喷霜析出。
将对比例1得到的阻燃塑料母粒料与PPK1708树脂以质量比2∶10混合均匀,注塑为平板测试样,编号为3#,注塑温度:1区200℃;2区210℃;3区230℃;4区240℃。将得到的测试板在80℃条件下放置24h,利用扫面电镜观察测试板表面,如附图2所示,板面具有明显析出的晶点,通过进一步放大观察,如附图3,析出的晶点大小接近5μm,响塑料制品的光泽度和光滑度。
Claims (10)
- 一种防喷霜析出的环保型阻燃塑料母料的制备方法,其特征在于,具体制备方法如下:(1)将硅酮粉与硫酸铝研磨,然后加入去离子水,得到分散硅酮粉的硫酸铝复合液备用;其中硅酮粉、硫酸铝、去离子水的质量比为1∶5∶20;(2)将聚磷酸铵、三聚氰胺聚磷酸盐以质量比3∶1复合,经微细机处理得到粒径小于5μm的复合微粉;(3)将复合微粉加入密闭容器,在密闭容器中充氨气,控制容器温度为35-45℃,并高速搅拌,将步骤(1)得到的硫酸铝复合液采用高压喷雾枪喷入密闭容器,悬浮的复合微粉表面与硫酸铝复合液接触,氨气逐步溶解在水中形成弱碱环境,促使复合微粉表面形成氢氧化铝包覆层;从密闭容器放料,在100-120℃的流化床干燥,得到复合改性聚磷酸铵阻燃剂;(4)将40-50重量份复合改性聚磷酸铵阻燃剂、5-10重量份填料、0.5-1重量份润滑助剂、0.1-0.3重量份硅油加入高速混合机,在100-120℃高速搅拌处理15-20min,然后加入15-20重量份聚丙烯、5-10重量份相容剂低速搅拌混合3-5min,混合均匀,放料进入冷混机,低速搅拌冷却;(5)经输送管路,将步骤(4)冷却的物料送入双螺杆挤出机,经挤出造粒得到一种防喷霜析出的环保型阻燃塑料母料。
- 根据权利要求1所述一种防喷霜析出的环保型阻燃塑料母料的制备方法,其特征在于:聚磷酸铵的结构通式为(NH4) (n+2)PnO (3n+1),步骤(2)所述聚磷酸铵选用n>500的长链聚磷酸铵。
- 根据权利要求1所述一种防喷霜析出的环保型阻燃塑料母料的制备方法,其特征在于:步骤(2)所述三聚氰胺磷酸盐选用市售磷含量大于14%,氮含量大于 38%的三聚氰胺聚磷酸盐。
- 根据权利要求1所述一种防喷霜析出的环保型阻燃塑料母料的制备方法,其特征在于:步骤(2)所述微细机采用涡旋气流粉碎机。
- 根据权利要求1所述一种防喷霜析出的环保型阻燃塑料母料的制备方法,其特征在于:步骤(3)所述高速搅拌转速为800-1200rpm,复合微粉在密闭容器的加入量不超过密闭容器容量的1/3。
- 根据权利要求1所述一种防喷霜析出的环保型阻燃塑料母料的制备方法,其特征在于:步骤(3)在密闭容器中充氨气,维持密闭容器氨气环境,并不断充入氨气,保证氨气压力在0.01MPa;所述高压喷雾枪压力为0.6-0.8MPa。进一步优选的,步骤(3)所述硫酸铝复合液的喷入量控制在复合微粉质量的0.5-1倍。为了较佳的保证在复合微粉表面均匀形成氢氧化铝包覆层,高压喷雾枪压力为0.6-0.8MPa。
- 根据权利要求1所述一种防喷霜析出的环保型阻燃塑料母料的制备方法,其特征在于:步骤(4)所述填料选用滑石粉、硅灰石粉、蒙脱土、云母粉中的至少一种;所述润滑助剂选用聚乙烯蜡、硬脂酸粉中的一种;所述硅油选用甲基三氟丙基硅油、甲基乙氧基硅油、甲基硅油、乙基硅油中的至少一种;所述相容剂为马来酸酐接枝聚丙烯、马来酸酐接枝聚乙烯、马来酸酐接枝乙烯-辛烯共聚物、马来酸酐接枝乙烯-丙烯-二烯烃共聚物中的一种。
- 根据权利要求1所述一种防喷霜析出的环保型阻燃塑料母料的制备方法,其特征在于:步骤(4)所述高速搅拌转速为400-900rpm,所述低速搅拌转速为80-100rpm。
- 根据权利要求1所述一种防喷霜析出的环保型阻燃塑料母料的制备方法,其特 征在于:步骤(5)所述双螺杆挤出机选用螺杆直径45mm、长径比20∶1的短长经比双螺杆挤出机;螺杆由进料到出料设置5个加热区,温度依次为:1区100-120℃、2区150-160℃、3区180-190℃、4区160-170℃、5区130-140℃;采用风冷模面切粒。
- 一种防喷霜析出的环保型阻燃塑料母料,其特征在于:由权利要求1-9任一项所述方法制备得到。
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