CN112457570A - Preparation method of halogen-free environment-friendly flame-retardant master batch for long glass fiber reinforced polypropylene composite material - Google Patents

Preparation method of halogen-free environment-friendly flame-retardant master batch for long glass fiber reinforced polypropylene composite material Download PDF

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Publication number
CN112457570A
CN112457570A CN202011269967.1A CN202011269967A CN112457570A CN 112457570 A CN112457570 A CN 112457570A CN 202011269967 A CN202011269967 A CN 202011269967A CN 112457570 A CN112457570 A CN 112457570A
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glass fiber
fiber reinforced
halogen
flame retardant
master batch
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吴建国
刘渊
陈荣
闻辉
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Jiangsu Jitri Advanced Polymer Materials Research Institute Co Ltd
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Jiangsu Jitri Advanced Polymer Materials Research Institute Co Ltd
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    • 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
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
    • C08J5/08—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials glass fibres
    • 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
    • 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
    • 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
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • 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
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C08K3/041—Carbon nanotubes
    • 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
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C08K3/042—Graphene or derivatives, e.g. graphene oxides
    • 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
    • C08K3/34—Silicon-containing compounds
    • C08K3/346—Clay
    • 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
    • C08K5/3442—Heterocyclic compounds having nitrogen in the ring having two nitrogen atoms in the ring
    • C08K5/3462—Six-membered rings
    • 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
    • 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
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/14—Glass
    • 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

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
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Abstract

The invention provides a preparation method of a halogen-free environment-friendly flame-retardant master batch for a long glass fiber reinforced polypropylene composite material, which comprises the steps of sequentially adding 400ml of dimethylformamide solution and 50g of polypropylene oxide wax into a three-neck flask and fully stirring to obtain microencapsulated modified piperazine pyrophosphate and melamine polyphosphate compound flame retardant powder; taking polypropylene powder as a carrier in 50 mass percent, respectively adding microencapsulated modified piperazine pyrophosphate and melamine polyphosphate compound powder flame retardant in 40-48.8 mass percent, flame retardant synergist in 1-8 mass percent, compound antioxidant in 0.1-1.0 mass percent and lubricant in 0.1-1.0 mass percent, and melting and granulating the mixture by a double-screw extruder to obtain the environment-friendly flame-retardant master batch for glass fiber reinforced polypropylene. On the basis of compounding of the halogen-free flame retardant, the third component, namely the nano material is introduced, so that the flame retardant efficiency is greatly improved, the using amount of the flame retardant can be reduced from 20% to 16-18%, the phenomenon of low-fall is obviously reduced, and the mechanical property is better.

Description

Preparation method of halogen-free environment-friendly flame-retardant master batch for long glass fiber reinforced polypropylene composite material
Technical Field
The invention relates to the field of long glass fiber reinforced polypropylene composite material preparation, and particularly relates to a preparation method of a halogen-free environment-friendly flame-retardant master batch for a long glass fiber reinforced polypropylene composite material.
Background
In the preparation process of the long glass fiber reinforced polypropylene composite material, the long glass fiber reinforced polypropylene composite material has high processing temperature and long heating time, the flame retardant is easy to decompose and lose efficacy under heating, the flame retardant is inconvenient to be directly added, and the long glass fiber reinforced polypropylene composite material particles and the flame-retardant master batches are generally uniformly mixed and then are subjected to injection molding or compression molding.
In addition, the halogen-free flame retardant used for the glass fiber reinforced polypropylene has few varieties, and the halogen-free environment-friendly flame retardant is a hydrophilic polar material, the polypropylene is a hydrophobic non-polar material, the compatibility of the halogen-free environment-friendly flame retardant and the polypropylene is poor, and the halogen-free environment-friendly flame retardant added into the polypropylene can bring negative effects on mechanical properties no matter whether the flame retardant mainly comprises ammonium polyphosphate, piperazine pyrophosphate, melamine polyphosphate and the like.
Disclosure of Invention
The invention provides a preparation method of a halogen-free environment-friendly flame-retardant master batch for a long glass fiber reinforced polypropylene composite material, which aims to solve at least one technical problem.
In order to solve the above problems, as an aspect of the present invention, a method for preparing a halogen-free environment-friendly flame retardant master batch for a long glass fiber reinforced polypropylene composite material is provided, which comprises the following steps:
step 1, placing a 1000ml three-neck flask into a water bath for fixing, adjusting the temperature of the water bath to 65 ℃, sequentially adding 400ml of dimethylformamide solution and 50g of polypropylene oxide wax into the three-neck flask, and fully stirring;
step 2, after the oxidized polypropylene wax is completely dissolved in the dimethylformamide, adding 150g of flame retardant powder compounded by piperazine pyrophosphate and melamine polyphosphate into the solution, and continuously stirring for 30 min;
step 3, taking out the mixture in the three-neck flask, putting the mixture into a vacuum oven at 80 ℃, drying to remove a dimethylformamide solvent, and crushing the mixture by using an airflow type ultramicro-powder machine to obtain microencapsulated modified piperazine pyrophosphate and melamine polyphosphate compound flame retardant powder;
and 4, taking polypropylene powder as a carrier with the mass percent of 50%, respectively adding 40-48.8% of microencapsulated modified pyrophosphoric piperazine and melamine polyphosphate compound powder flame retardant with the mass percent, 1-8% of any flame retardant synergist in organic montmorillonite, carbon nano tube, graphene and other nano materials with the mass percent of 0.1-1.0%, and 0.1-1.0% of lubricant with the mass percent of 0.1-1.0%, and melting and granulating by using a double-screw extruder to obtain the environment-friendly flame retardant master batch for the glass fiber reinforced polypropylene.
Preferably, the oxidized polypropylene wax has a molecular weight of 3000-10000.
Preferably, the mass percentage of the piperazine pyrophosphate to the melamine polyphosphate is 5: 1 to 1: 5.
preferably, the polypropylene powder is homo-or co-polymerized, MFR: 20-200g/10 min.
Preferably, the compound antioxidant is one or two of antioxidant 1010, antioxidant 1098, antioxidant 168 and the like.
Preferably, the lubricant is one or two of calcium stearate, mesoacid amide and the like.
Preferably, the flame retardant synergist is any one of organic montmorillonite, carbon nanotube, graphene and other nano materials.
On the basis of halogen-free flame retardant compounding (compounding of piperazine pyrophosphate and melamine polyphosphate), a third component, namely a nano material (flame retardant synergist), is introduced, so that the flame retardant efficiency is greatly improved, the flame retardant dosage can be reduced from 20% to 16-18%, the droop phenomenon is obviously reduced, and the mechanical property is better.
Detailed Description
The following detailed description of embodiments of the invention, but the invention can be practiced in many different ways, as defined and covered by the claims.
The halogen-free environment-friendly flame-retardant master batch for the long glass fiber reinforced polypropylene composite material is prepared by the following steps:
firstly, placing a 1000ml three-neck flask in a water bath kettle for fixing, and adjusting the temperature of the water bath kettle to 65 ℃; at the temperature, 400ml of dimethylformamide solution and 50g of polypropylene oxide wax (molecular weight 3000-10000) are added into a three-neck flask in sequence and fully stirred; after the oxidized polypropylene wax is completely dissolved in l dimethyl formamide, 150g of traditional piperazine pyrophosphate and melamine polyphosphate compound flame retardant powder (the ratio of piperazine pyrophosphate to melamine polyphosphate is 5/1-1/5 by mass percent) is added into the solution, the mixture is continuously stirred for 30min, then the mixture in a three-neck flask is taken out, the mixture is put into a vacuum oven at 80 ℃ to be dried to remove the dimethyl formamide solvent, and the mixture is crushed by an airflow type ultramicro powder machine to obtain the microencapsulated modified piperazine pyrophosphate and melamine polyphosphate compound flame retardant powder.
Then, taking polypropylene powder (homopolymerization or copolymerization, MFR: 20-200g/10min) as 50 percent of carrier (mass percent), respectively adding 40-48.8 percent of microencapsulated modified piperazine pyrophosphate and melamine polyphosphate compound powder flame retardant, 1-8 percent of any one flame retardant synergist in nano materials such as organic montmorillonite, carbon nano tube and graphene, 0.1-1.0 percent of one or any two compound antioxidants such as antioxidant 1010, antioxidant 1098 and antioxidant 168, and 0.1-1.0 percent of one or any two lubricants such as calcium stearate and mesoacid amide, and melting and granulating by a double-screw extruder to obtain the environment-friendly flame-retardant master batch for glass fiber reinforced polypropylene.
In the technical scheme, the surface modification treatment is carried out on the halogen-free environment-friendly flame retardant, so that the modifier and the flame retardant form hydrogen bond medium-coated microcapsules, the compatibility of the microcapsule and polypropylene is improved, the flame retardant property of the polypropylene is improved, the negative influence of the microcapsule on the mechanical property of the long glass fiber reinforced polypropylene composite material is reduced as much as possible, and the flame retardant efficiency of the microcapsule is improved; carbonyl and hydroxyl on the molecular chain of the polypropylene oxide wax can be combined with piperazine pyrophosphate and-C ═ O and-N-H on melamine polyphosphate to form hydrogen bonds, and the polypropylene wax microcapsule is used for coating the piperazine pyrophosphate and the melamine polyphosphate, so that the polypropylene wax microcapsule has improved compatibility with polypropylene.
According to the invention, on the basis of compounding piperazine pyrophosphate and melamine polyphosphate halogen-free flame retardant, a third component, namely a nano material, is introduced as a flame retardant synergist, so that the flame retardant efficiency is greatly improved, the flame retardant dosage can be reduced from 20% to 16-18%, the sag phenomenon is obviously reduced, and the mechanical property is better.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. 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 (7)

1. The preparation method of the halogen-free environment-friendly flame-retardant master batch for the long glass fiber reinforced polypropylene composite material is characterized by comprising the following steps of:
step 1, placing a 1000ml three-neck flask into a water bath for fixing, adjusting the temperature of the water bath to 65 ℃, sequentially adding 400ml of dimethylformamide solution and 50g of polypropylene oxide wax into the three-neck flask, and fully stirring;
step 2, after the oxidized polypropylene wax is completely dissolved in the dimethylformamide, adding 150g of flame retardant powder compounded by piperazine pyrophosphate and melamine polyphosphate into the solution, and continuously stirring for 30 min;
step 3, taking out the mixture in the three-neck flask, putting the mixture into a vacuum oven at 80 ℃, drying to remove a dimethylformamide solvent, and crushing the mixture by using an airflow type ultramicro-powder machine to obtain microencapsulated modified piperazine pyrophosphate and melamine polyphosphate compound flame retardant powder;
and 4, taking polypropylene powder as a carrier with the mass percent of 50%, respectively adding microencapsulated modified piperazine pyrophosphate and melamine polyphosphate compound powder flame retardant with the mass percent of 40-48.8%, flame retardant synergist with the mass percent of 1-8%, compound antioxidant with the mass percent of 0.1-1.0% and lubricant with the mass percent of 0.1-1.0%, and melting and granulating by a double-screw extruder to obtain the environment-friendly flame-retardant master batch for the glass fiber reinforced polypropylene.
2. The method for preparing the halogen-free environment-friendly flame-retardant master batch for the long glass fiber reinforced polypropylene composite material as claimed in claim 1, wherein the molecular weight of the oxidized polypropylene wax is 3000-10000.
3. The preparation method of the halogen-free environment-friendly flame-retardant master batch for the long glass fiber reinforced polypropylene composite material as claimed in claim 1, wherein the mass percentage of the piperazine pyrophosphate and the melamine polyphosphate is 5/1-1/5.
4. The preparation method of the halogen-free environment-friendly flame-retardant master batch for the long glass fiber reinforced polypropylene composite material according to claim 1, wherein the polypropylene powder is homopolymerized or copolymerized, and the MFR: 20-200g/10 min.
5. The preparation method of the halogen-free environment-friendly flame-retardant master batch for the long glass fiber reinforced polypropylene composite material according to claim 1, wherein the antioxidant is one or two of an antioxidant 1010, an antioxidant 1098, an antioxidant 168 and the like.
6. The preparation method of the halogen-free environment-friendly flame-retardant master batch for the long glass fiber reinforced polypropylene composite material according to claim 1, wherein the lubricant is one or two of calcium stearate, mesoacid amide and the like.
7. The preparation method of the halogen-free environment-friendly flame retardant master batch for the long glass fiber reinforced polypropylene composite material according to claim 1, wherein the flame retardant synergist is any one of organic montmorillonite, carbon nanotube, graphene and other nano materials.
CN202011269967.1A 2020-11-13 2020-11-13 Preparation method of halogen-free environment-friendly flame-retardant master batch for long glass fiber reinforced polypropylene composite material Pending CN112457570A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114031844A (en) * 2021-10-25 2022-02-11 浙江旭森非卤消烟阻燃剂有限公司 Halogen-free flame-retardant master batch for continuous long glass fiber reinforced polypropylene and preparation method thereof
CN114181431A (en) * 2021-12-21 2022-03-15 包头稀土研究院 Flame retardant, preparation method and application thereof and polyolefin composition

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Publication number Priority date Publication date Assignee Title
CN1712444A (en) * 2005-07-12 2005-12-28 南京航空航天大学 Non-halogen fire-retardant polypropylene and production thereof
CN102134352A (en) * 2011-05-09 2011-07-27 中山大学 Expansion type flame-retardant polypropylene composite material and preparation method thereof
CN103589052A (en) * 2012-08-14 2014-02-19 滁州格美特科技有限公司 Water-resistant flame-retardant polypropylene composite material and preparation method thereof
CN104086884A (en) * 2014-07-03 2014-10-08 合肥杰事杰新材料股份有限公司 Flame retardant polypropylene material and preparation method thereof
CN104629095A (en) * 2015-03-04 2015-05-20 南京炫胜塑料科技股份有限公司 Environment-friendly composite flame retardant and polypropylene flame-retardant composition
CN110577717A (en) * 2019-08-30 2019-12-17 东莞毅工工程塑料有限公司 scratch-resistant flame-retardant PP (polypropylene) modified material and preparation method thereof
CN111484670A (en) * 2019-12-20 2020-08-04 四川鑫达企业集团有限公司 Halogen-free flame-retardant low-floating-fiber reinforced polypropylene composite material and preparation method thereof
CN111690207A (en) * 2020-07-30 2020-09-22 安徽集虹材料科技有限公司 Production method of halogen-free flame-retardant master batch

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1712444A (en) * 2005-07-12 2005-12-28 南京航空航天大学 Non-halogen fire-retardant polypropylene and production thereof
CN102134352A (en) * 2011-05-09 2011-07-27 中山大学 Expansion type flame-retardant polypropylene composite material and preparation method thereof
CN103589052A (en) * 2012-08-14 2014-02-19 滁州格美特科技有限公司 Water-resistant flame-retardant polypropylene composite material and preparation method thereof
CN104086884A (en) * 2014-07-03 2014-10-08 合肥杰事杰新材料股份有限公司 Flame retardant polypropylene material and preparation method thereof
CN104629095A (en) * 2015-03-04 2015-05-20 南京炫胜塑料科技股份有限公司 Environment-friendly composite flame retardant and polypropylene flame-retardant composition
CN110577717A (en) * 2019-08-30 2019-12-17 东莞毅工工程塑料有限公司 scratch-resistant flame-retardant PP (polypropylene) modified material and preparation method thereof
CN111484670A (en) * 2019-12-20 2020-08-04 四川鑫达企业集团有限公司 Halogen-free flame-retardant low-floating-fiber reinforced polypropylene composite material and preparation method thereof
CN111690207A (en) * 2020-07-30 2020-09-22 安徽集虹材料科技有限公司 Production method of halogen-free flame-retardant master batch

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114031844A (en) * 2021-10-25 2022-02-11 浙江旭森非卤消烟阻燃剂有限公司 Halogen-free flame-retardant master batch for continuous long glass fiber reinforced polypropylene and preparation method thereof
CN114031844B (en) * 2021-10-25 2023-10-03 浙江旭森阻燃剂股份有限公司 Halogen-free flame-retardant master batch for continuous long glass fiber reinforced polypropylene and preparation method thereof
CN114181431A (en) * 2021-12-21 2022-03-15 包头稀土研究院 Flame retardant, preparation method and application thereof and polyolefin composition
CN114181431B (en) * 2021-12-21 2023-08-15 包头稀土研究院 Flame retardant, preparation method and application thereof and polyolefin composition

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