CN112322029B - Halogen-free flame-retardant nylon material and preparation method and application thereof - Google Patents
Halogen-free flame-retardant nylon material and preparation method and application thereof Download PDFInfo
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- CN112322029B CN112322029B CN202011298794.6A CN202011298794A CN112322029B CN 112322029 B CN112322029 B CN 112322029B CN 202011298794 A CN202011298794 A CN 202011298794A CN 112322029 B CN112322029 B CN 112322029B
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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
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
- C08K5/5313—Phosphinic compounds, e.g. R2=P(:O)OR'
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
- C08J3/122—Pulverisation by spraying
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- 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
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- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
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Abstract
The invention discloses a halogen-free flame-retardant nylon material and a preparation method and application thereof, wherein the preparation raw materials of the halogen-free flame-retardant nylon material comprise nylon powder, organic aluminum phosphate, amine polyphosphate and an auxiliary agent; d of the nylon powder 10 20 to 50 μm, D 50 Is 50-90 mu m, and the D of the organic aluminum phosphate 50 D in the nylon powder 10 And D 50 D of said amine polyphosphate 50 Not more than 10 μm. The invention reasonably sets the grain diameters of the nylon powder, the flame retardant organic aluminum phosphate and the amine polyphosphate to ensure that the main flame retardant organic aluminum phosphate has the grain diameter D 50 Control in nylon powder D 10 And D 50 While adding auxiliary flame retardant amine polyphosphate D 50 The limit is below 10 mu m, which is beneficial to the uniform dispersion of the flame retardant between the nylon powder, improves the contact area of the flame retardant and the nylon powder, effectively wraps the nylon molecules in the combustion process of the flame retardant, and effectively improves the flame retardant efficiency.
Description
Technical Field
The invention relates to the technical field of additive manufacturing materials, in particular to a halogen-free flame-retardant nylon material and a preparation method and application thereof.
Background
The Selective Laser Sintering (SLS) technology is a typical 3D printing technology, and it applies a layered manufacturing concept and utilizes a discrete-stacking principle to stack materials layer by layer to manufacture a new manufacturing technology of a solid object, which embodies the close combination of an information network technology, an advanced material technology and a digital manufacturing technology, and is an important component of intelligent manufacturing. Through rapid development for many years, the SLS technology has been widely applied to various fields such as automobiles, household appliances, aerospace, medical biology and the like, and is one of the more mature 3D printing technologies applied at present.
The nylon powder is used as a typical thermoplastic semi-crystalline polymer material, has excellent mechanical property, good thermal property and low melt viscosity, is very suitable for being used as a forming material of an SLS (selective laser sintering) process, can be used for preparing a sintered part with high density and high strength after SLS sintering, and is a mainstream consumable material of an SLS 3D printing technology at present. However, since nylon has a low oxygen index, a high combustion speed and a severe dripping during combustion, and flame is easily dispersed to cause secondary ignition, the application of nylon materials (such as automobiles and aerospace) with strict safety requirements is greatly limited, and a flame-retardant nylon material suitable for SLS 3D printing needs to be developed.
Disclosure of Invention
The present invention has been made to solve at least one of the above-mentioned problems occurring in the prior art. Therefore, the invention provides the halogen-free flame-retardant nylon material which is good in powder fluidity and high in flame-retardant efficiency.
The invention also provides a preparation method and application of the halogen-free flame-retardant nylon material.
The technical scheme adopted by the invention is as follows:
the first aspect of the invention provides a halogen-free flame-retardant nylon material, which is prepared from raw materials including nylon powder, organic aluminum phosphate, amine polyphosphate and an auxiliary agent; d of the nylon powder 10 20 to 50 μm, D 50 Is 50-90 mu m, and the D of the organic aluminum phosphate 50 D in the nylon powder 10 And D 50 D of said amine polyphosphates 50 Not more than 10 μm.
The halogen-free flame-retardant nylon material according to the first aspect of the invention has at least the following beneficial effects:
the traditional process for preparing the flame-retardant nylon plastic generally adopts the flame retardant with smaller particle size, and all raw materials are melted and stirred in the preparation process, so that the flame retardant and the nylon powder can be uniformly dispersed even if the particle size of the flame retardant and the nylon powder is extremely small. However,the nylon material used for 3D printing is powder, all raw materials of the nylon material are simply mixed and cannot be melted and stirred, only the nylon material which enters the printing process and is acted by laser can be melted, and the nylon material which is not acted by the laser is always kept in a powder state, so if the nylon powder and the flame retardant with small particle size are adopted, agglomeration is easy to generate, the flame retardant is difficult to uniformly disperse, and the flame retardant performance of a printed product is reduced. The invention reasonably sets the grain diameters of the nylon powder, the organic aluminum phosphate serving as the flame retardant and the amine polyphosphate to ensure that the D of the organic aluminum phosphate serving as the main flame retardant is D 50 D controlled in nylon powder 10 And D 50 While adding auxiliary flame retardant amine polyphosphate D 50 The limit is below 10 mu m, which is beneficial to the uniform dispersion of the flame retardant between the nylon powder, improves the contact area of the flame retardant and the nylon powder, effectively wraps the nylon molecules in the combustion process of the flame retardant, and effectively improves the flame retardant efficiency.
By compounding two flame retardants of organic aluminum phosphate and amine polyphosphate, the flame retardant efficiency of the material is improved, and the dosage of the flame retardant is greatly reduced. Because the organic aluminum phosphate and the amine polyphosphate have good compatibility with nylon, the mechanical property of the nylon is maintained to the maximum extent.
According to a preferred embodiment of the invention, the nylon powder has a maximum particle size of < 200 μm.
According to a preferred embodiment of the invention, D of the organophosphate is 50 20-70 μm, D of said amine polyphosphate 50 Is 2-10 μm.
According to a preferred embodiment of the invention, the nylon powder has a maximum particle size of < 150 μm, D 50 D of the organic aluminum phosphate is 50-70 mu m 50 20-50 μm, D of said amine polyphosphate 50 Is 2-5 μm.
According to a preferred embodiment of the invention, the auxiliary agent comprises an antioxidant and a powder flow auxiliary agent, and the halogen-free flame-retardant nylon material comprises the following preparation raw materials in percentage by mass:
50 to 90 percent of nylon powder
1 to 25 percent of organic aluminum phosphate
1 to 25 percent of amine polyphosphate
0.1 to 1 percent of antioxidant
0.1 to 1 percent of powder flow additive.
According to a more preferred embodiment of the invention, the halogen-free flame retardant nylon material comprises the following preparation raw materials in percentage by mass:
50 to 80 percent of nylon powder
10 to 25 percent of organic aluminum phosphate
5 to 20 percent of amine polyphosphate
0.1 to 1 percent of antioxidant
0.1 to 1 percent of powder flow additive.
According to a preferred embodiment of the present invention, the nylon powder comprises any one or more of nylon 12, nylon 11, nylon 1012, nylon 1010, and nylon 610.
According to a preferred embodiment of the invention, the aluminum organophosphate comprises at least one of aluminum diethylphosphinate, aluminum tris (diethylphosphinate).
According to a preferred embodiment of the present invention, the amine polyphosphate comprises at least one of melamine phosphate and melamine polyphosphate.
According to a preferred embodiment of the present invention, the antioxidant is selected from general antioxidants, and as an example, the antioxidant is selected from one or two of antioxidant 1098 and antioxidant 168, preferably a combination of antioxidant 1098 and antioxidant 168.
According to a more preferred embodiment of the present invention, the mass ratio of the antioxidant 1098 to the antioxidant 168 is (1 to 3): 1.
according to a preferred embodiment of the present invention, the powder flow aid is selected from at least one of fumed silica and nano titania.
The second aspect of the invention provides a preparation method of the halogen-free flame retardant nylon material, which comprises the following steps:
dispersing nylon powder, organic aluminum phosphate, amine polyphosphate and an auxiliary agent in a solvent, stirring, and then carrying out spray drying to obtain the halogen-free flame-retardant nylon material.
The solvent can be a volatile organic solvent, such as ethanol.
The hot air inlet temperature adopted when spray drying is carried out is 180-200 ℃, and 185 ℃ is preferred.
According to the invention, the nylon powder and the flame retardant are fully, uniformly and effectively dispersed in a solvent dispersion mode, so that the risk of agglomeration of the flame retardant is avoided, spray drying is carried out subsequently, the air inlet temperature is controlled to be close to the melting point of the nylon powder, and the flame retardant is more closely attached to the periphery of nylon particles under the action of the surface tension of the nylon powder, so that the uniform dispersion state is maintained.
The third aspect of the invention is to provide the application of the halogen-free flame retardant nylon material in 3D printing.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The starting materials, reagents or apparatus used in the examples were obtained from conventional commercial sources unless otherwise specified. Unless otherwise indicated, the testing or testing methods are conventional in the art.
Example 1
Preparing corresponding dry preparation materials according to the following components of 80 parts of nylon powder, 15 parts of diethyl aluminum hypophosphite, 5 parts of melamine phosphate, 0.5 part of antioxidant 1098 and 168 combination (mass ratio is 1). Wherein the maximum particle diameter of the nylon powder is 102 mu m, D 50 58 μm, D 10 Is 29 μm; d of aluminium diethylphosphinate 50 38 μm, D of melamine phosphate 50 Is 5 μm.
And then the ingredients are put into an enamel kettle and dispersed in an ethanol solvent, after the ingredients are fully and uniformly stirred, spray drying is carried out, and the hot air inlet temperature is controlled at 185 ℃, so that the finished product of the halogen-free flame-retardant nylon powder is obtained.
Example 2
70 parts of nylon powder, 20 parts of diethyl aluminum hypophosphite and 10 parts of melamine phosphate0.5 part of antioxidant 1098 and 168 (mass ratio is 2. Wherein the maximum particle diameter of the nylon powder is 102 mu m, D 50 Is 58 μm, D 10 Is 29 μm; d of diethyl aluminum hypophosphite 50 38 μm, D of melamine phosphate 50 Is 5 μm.
And then the ingredients are put into an enamel kettle and dispersed in an ethanol solvent, after the ingredients are fully and uniformly stirred, spray drying is carried out, and the hot air inlet temperature is controlled at 185 ℃, so that the finished product of the halogen-free flame-retardant nylon powder is obtained.
Example 3
Preparing corresponding drying preparation materials according to the following components and mass ratio of 60 parts of nylon powder, 25 parts of diethyl aluminum hypophosphite, 15 parts of melamine phosphate, 0.5 part of antioxidant 1098 and 168 combination (mass ratio is 3). Wherein the maximum particle diameter of the nylon powder is 102 mu m, D 50 58 μm, D 10 Is 29 μm; d of aluminium diethylphosphinate 50 38 μm, D of melamine phosphate 50 Is 5 μm.
And then the ingredients are put into an enamel kettle and dispersed in an ethanol solvent, after the ingredients are fully and uniformly stirred, spray drying is carried out, and the hot air inlet temperature is controlled at 185 ℃, so that the finished product of the halogen-free flame-retardant nylon powder is obtained.
Comparative example 1
The main difference between this comparative example and example 1 is that: diethyl aluminum hypophosphite was used as a single flame retardant.
Specifically, according to the following components in parts by weight of 80 parts of nylon powder, 20 parts of diethyl aluminum hypophosphite, 0.5 part of antioxidant 1098 and 168 combination (mass ratio is 1). Wherein the maximum particle diameter of the nylon powder is 102 mu m, D 50 58 μm, D 10 Is 29 μm; d of aluminium diethylphosphinate 50 And was 38 μm.
And then the ingredients are put into an enamel kettle and dispersed in an ethanol solvent, after the ingredients are fully and uniformly stirred, spray drying is carried out, and the hot air inlet temperature is controlled at 185 ℃, so that the finished product of the halogen-free flame-retardant nylon powder is obtained.
Comparative example 2
The main difference between this comparative example and example 2 is that: diethyl aluminum hypophosphite was used as a single flame retardant.
Specifically, according to the following components in parts by mass ratio of 70 parts of nylon powder, 30 parts of diethyl aluminum hypophosphite, 0.5 part of antioxidant 1098 and 168 combination (mass ratio is 2). Wherein the maximum particle diameter of the nylon powder is 102 μm, D 50 58 μm, D10 29 μm; d of diethyl aluminum hypophosphite 50 And was 38 μm.
And then the ingredients are put into an enamel kettle and dispersed in an ethanol solvent, after the ingredients are fully and uniformly stirred, spray drying is carried out, and the hot air inlet temperature is controlled at 185 ℃, so that the finished product of the halogen-free flame-retardant nylon powder is obtained.
Comparative example 3
The main difference between this comparative example and example 2 is that: a single flame retardant melamine phosphate was used.
Specifically, according to the following components and mass ratio, 70 parts of nylon powder, 30 parts of melamine phosphate, 0.5 part of antioxidant 1098 and 168 composition (mass ratio is 2). Wherein the maximum particle diameter of the nylon powder is 102 μm, D 50 Is 58 μm, D 10 Is 29 μm; d of melamine phosphate 50 Is 5 μm.
And then the ingredients are put into an enamel kettle and dispersed in an ethanol solvent, after the ingredients are fully and uniformly stirred, spray drying is carried out, and the hot air inlet temperature is controlled at 185 ℃, so that the finished product of the halogen-free flame-retardant nylon powder is obtained.
Comparative example 4
The main difference between this comparative example and example 2 is that: d of diethyl aluminum hypophosphite with melamine phosphate 50 The same values were 5 μm.
Specifically, according to the following components and mass ratio of 70 parts of nylon powder, 20 parts of diethyl aluminum hypophosphite, 10 parts of melamine phosphate, 0.5 part of antioxidant 1098 and 168 (mass ratio is 2 50 Is 58 μm, D 10 D of 29 μm aluminum diethylhypophosphite with melamine phosphate 50 Is 5 μm.
And then the ingredients are put into an enamel kettle and dispersed in an ethanol solvent, after the ingredients are fully and uniformly stirred, spray drying is carried out, and the hot air inlet temperature is controlled at 185 ℃, so that the finished product of the halogen-free flame-retardant nylon powder is obtained.
Comparative example 5
The main difference between this comparative example and example 2 is that: d of diethyl aluminum hypophosphite with melamine phosphate 50 All are 80 μm.
Specifically, according to the following components and mass ratio of 70 parts of nylon powder, 20 parts of diethyl aluminum hypophosphite, 10 parts of melamine phosphate, 0.5 part of antioxidant 1098 and 168 combination (mass ratio is 2: 1), and 0.2 part of nano titanium dioxide, preparing corresponding drying preparation materials, wherein the maximum particle size of the nylon powder is 102 mu m, and the maximum particle size D is D 50 58 μm, D 10 D of 29 μm aluminum diethylhypophosphite and melamine phosphate 50 And 80 μm.
And then the ingredients are put into an enamel kettle and dispersed in an ethanol solvent, after the ingredients are fully and uniformly stirred, spray drying is carried out, and the hot air inlet temperature is controlled at 185 ℃, so that the finished product of the halogen-free flame-retardant nylon powder is obtained.
The halogen-free flame-retardant nylon materials of the above embodiments and comparative examples are used for SLS 3D printing, standard sample strips for UL94 flame-retardant test are sintered, the thickness of the sample strips is 1mm and 2mm respectively, the UL94 standard is adopted for carrying out the combustion test, and the flame-retardant test results are shown in the following table, wherein V0 and V2 are UL94 flame-retardant grades.
| Thickness of sample strip | 1mm | 2mm |
| Example 1 | V2 | V0 |
| Example 2 | V2 | V0 |
| Example 3 | V2 | V0 |
| Comparative example 1 | V2 | V2 |
| Comparative example 2 | V2 | V2 |
| Comparative example 3 | V2 | V2 |
| Comparative example 4 | V2 | V2 |
| Comparative example 5 | V2 | V2 |
The test results reflect that the flame retardant effect of the sample strips printed by SLS 3D using the halogen-free flame retardant nylon material of embodiments 1-3 can reach UL 94V 0 grade when the sample strips are 2mm thick (the UL94 flame retardant grade is gradually increased from HB, V2, V1 to V0, and the UL 94V 0 grade is the highest grade flame retardant grade). In contrast, when diethyl aluminum hypophosphite or melamine aluminum phosphate is used alone as a flame retardant (comparative examples 1 to 3), or nylon powder, diethyl aluminum hypophosphite and melamine aluminum phosphate are arranged according to a particle size combination different from that of examples 1 to 3, the flame retardant effect of a sample strip with the thickness of 2mm only reaches UL 94V 2 level, and cannot reach UL 94V 0 level, which shows that the flame retardant performance of the halogen-free flame retardant nylon material can be effectively improved by compounding diethyl aluminum hypophosphite or melamine aluminum phosphate, and meanwhile, the nylon powder, diethyl aluminum hypophosphite and melamine aluminum phosphate are distributed according to specific particle sizes, so that the halogen-free flame retardant nylon material is suitable for SLS 3D printing.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. A halogen-free flame-retardant nylon material is characterized in that: the halogen-free flame-retardant nylon material comprises the following preparation raw materials in percentage by mass: 50-80% of nylon powder, 10-25% of organic aluminum phosphate, 5-20% of amine polyphosphate, 0.1-1% of antioxidant and 0.1-1% of powder flow assistant; d of the nylon powder 10 20 to 50 μm, D 50 50 to 90 mu m, D of the organic aluminum phosphate 50 D in the nylon powder 10 And D 50 D of said amine polyphosphates 50 Not more than 10 μm; and dispersing the nylon powder, the organic aluminum phosphate, the amine polyphosphate, the antioxidant and the powder flow aid in a solvent, stirring, and performing spray drying to obtain the halogen-free flame-retardant nylon material.
2. The halogen-free flame retardant nylon material of claim 1, wherein: the maximum particle size of the nylon powder is less than 200 mu m.
3. The halogen-free flame retardant nylon material according to claim 2,the method is characterized in that: d of the organophosphate 50 20 to 70 mu m, D of the amine polyphosphate 50 2 to 10 μm.
4. The halogen-free flame retardant nylon material of claim 3, wherein: the maximum particle diameter of the nylon powder is less than 150 mu m, D 50 50 to 70 mu m, D of the organic aluminum phosphate 50 20 to 50 mu m, D of the amine polyphosphate 50 Is 2 to 5 mu m.
5. The halogen-free flame retardant nylon material according to claim 1 or 2, characterized in that: the nylon powder comprises at least one of nylon 12, nylon 11, nylon 1012, nylon 1010 and nylon 610.
6. The halogen-free flame retardant nylon material according to claim 1 or 2, characterized in that: the aluminum organophosphate comprises at least one of aluminum diethylphosphinate and aluminum tris (diethylphosphinate).
7. The halogen-free flame retardant nylon material according to claim 1 or 2, characterized in that: the amine polyphosphate comprises at least one of melamine phosphate and melamine polyphosphate.
8. The preparation method of the halogen-free flame retardant nylon material of any one of claims 1 to 7, which is characterized in that: the method comprises the following steps:
dispersing nylon powder, organic aluminum phosphate, amine polyphosphate, an antioxidant and a powder flow aid in a solvent, stirring, and then carrying out spray drying to obtain the halogen-free flame-retardant nylon material.
9. The use of the halogen-free flame-retardant nylon material according to any one of claims 1 to 7 in 3D printing.
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| DE10256097A1 (en) * | 2002-12-02 | 2004-06-17 | Eos Gmbh Electro Optical Systems | Plastic powder for laser sintering |
| CN100358939C (en) * | 2005-11-11 | 2008-01-02 | 淄博广通化工有限责任公司 | Method for preparing powder of nylon |
| CN102585290B (en) * | 2012-03-14 | 2013-04-17 | 济南泰星精细化工有限公司 | Method for preparing melamine cyanurate with large particle size and wide distribution |
| CN106854359A (en) * | 2016-11-24 | 2017-06-16 | 广东美塑塑料科技有限公司 | Inexpensive high heat-resistant halogen-free flame-retardant reinforced plastic PA66 composition and preparation method thereof |
| CN106987116A (en) * | 2017-04-28 | 2017-07-28 | 湖南华曙高科技有限责任公司 | Halogen-free flame-retardant nylon material for selective laser sintering and preparation method thereof |
| FR3071840B1 (en) * | 2017-10-04 | 2019-10-11 | Arkema France | THERMOPLASTIC POWDER COMPOSITION AND REINFORCED 3-DIMENSIONAL OBJECT MANUFACTURED BY 3D PRINTING OF SUCH A COMPOSITION |
| WO2019195689A1 (en) * | 2018-04-06 | 2019-10-10 | E. I. Du Pont De Nemours And Company | Additive manufacturing compositions |
| FR3093945B1 (en) * | 2019-03-18 | 2023-10-27 | Arkema France | FLAME-RETARDANT POLYAMIDES AND COPOLYAMIDES FOR 3D PRINTING |
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