CN115477838A - Polyether type TPU halogen-free flame retardant master batch and preparation method thereof - Google Patents
Polyether type TPU halogen-free flame retardant master batch and preparation method thereof Download PDFInfo
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- 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
- C08J3/20—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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2475/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2475/04—Polyurethanes
- C08J2475/08—Polyurethanes from polyethers
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- 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
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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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- 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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Abstract
The invention discloses a polyether type TPU halogen-free flame retardant master batch and a preparation method thereof, wherein the polyether type TPU halogen-free flame retardant master batch comprises the following components in percentage by mass: 36-48% of TPU, 50-60% of halogen-free flame retardant, 0.3-0.5% of anti-dripping agent, 0.2-0.5% of antioxidant, 1-2% of lubricant and 0.5-1% of white mineral oil, wherein the flame retardant grade of the polyether TPU added with the flame retardant master batch reaches UL94V-0, the tensile strength of the polyether TPU can reach more than 20Mpa, and dripping can not occur.
Description
Technical Field
The invention belongs to the technical field of flame-retardant TPU (thermoplastic polyurethane) master batches, and particularly relates to a polyether type halogen-free flame-retardant master batch for TPU and a preparation method thereof.
Background
The TPU (polyether urethane elastomer) has the advantages of better chemical corrosion resistance, weather resistance, hydrolytic stability, electrical insulation and the like, and is widely applied to the fields of automobiles, building materials, cable sheaths, sports mountaineering shoe materials, multifunctional films and the like.
However, the polyether TPU material is extremely easy to burn, the Oxygen Index (OI) is only about 18%, and the polyether TPU material is accompanied by dense smoke and releases a large amount of harmful gas during burning, and meanwhile, the phenomenon of serious dripping exists. The existing flame-retardant TPU usually adopts a brominated flame retardant, but has the problem of environmental protection, or adopts magnesium hydroxide and aluminum hydroxide, the addition amount of which is more than 60 percent can meet the flame-retardant requirement, but the mechanical property is obviously reduced after flame retardation. Taking tensile strength as an example, the tensile strength of pure polyether type TPU is 30-40 MPa generally, after a common flame retardant is adopted, the tensile strength is rapidly reduced to about 10MPa or even below, and the strength of the cable generally needs to reach 20MPa.
Disclosure of Invention
Therefore, it is necessary to provide a polyether type TPU halogen-free flame retardant master batch with good flame retardance and capable of avoiding obvious reduction of mechanical properties and aiming at the problem that the mechanical properties of a common flame retardant TPU material are obviously reduced after flame retardance, and a preparation method thereof.
The halogen-free flame-retardant master batch for the polyether TPU comprises the following components in percentage by mass:
36 to 48 percent of polyether type TPU and 50 to 60 percent of halogen-free flame retardant
0.3 to 0.5 percent of anti-dripping agent and 0.2 to 0.5 percent of antioxidant
1 to 2 percent of lubricant and 0.5 to 1 percent of white mineral oil.
In one embodiment, the halogen-free flame retardant is a compound consisting of aluminum hypophosphite, melamine cyanurate, and a macromolecular triazine char-forming agent.
In one embodiment, the mass ratio of the aluminum hypophosphite, the melamine cyanurate and the macromolecular triazine charring agent in the compound is 3.
In one embodiment, the mass ratio of aluminum hypophosphite, melamine cyanurate, and the macromolecular triazine char-forming agent in the formulation is preferably 3.
In one embodiment, the macromolecular triazine charring agent is synthesized by using cyanuric chloride, ethylamine and piperazine as raw materials, or cyanuric chloride, diphenylamine and ethylenediamine as raw materials, or cyanuric chloride, piperazine and cage-shaped phosphate as raw materials.
In one embodiment, the anti-drip agent is polytetrafluoroethylene.
In one embodiment, the antioxidant is one or more of pentaerythritol tetrakis [ methyl- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], 1,3, 5-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) isocyanurate, 1,3, 5-tris (4-tert-butyl-3-hydroxy-2, 6-dimethylbenzyl) -1,3, 5-triazine-2, 4,6- (1H, 3H, 5H) -trione, tris (2, 4-di-tert-butylphenyl) phosphite (antioxidant 168), bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite (antioxidant THP-24), distearyl thiodipropionate.
In one embodiment, the lubricant is one or more of calcium stearate, zinc stearate, polyethylene wax, and N, N' -ethylene bis stearamide.
The preparation method of the halogen-free flame retardant master batch for preparing the polyether TPU is characterized by comprising the following steps:
weighing the polyether TPU, the halogen-free flame retardant, the anti-dripping agent, the antioxidant, the lubricant and the white mineral oil according to the mass percentage, uniformly stirring the polyether TPU and the white mineral oil in a high-speed mixer, then adding the halogen-free flame retardant, the anti-dripping agent, the antioxidant and the lubricant, uniformly mixing, adding the mixture into a double-screw machine for extrusion granulation, wherein the processing temperature is 160-180 ℃, drying the granulated master batch, cooling and packaging to obtain the flame-retardant master batch.
Compared with the prior art, the polyether type TPU halogen-free flame retardant master batch and the preparation method thereof have the beneficial effects that:
1. the preparation method comprises the following steps of selecting a macromolecular triazine charring agent in a halogen-free flame retardant, and compounding the macromolecular triazine charring agent with aluminum hypophosphite and melamine cyanurate according to the mass ratio of 3;
2. the reason is that the macromolecule triazine charring agent has the bonding of the triazine ring and the piperazine ring structure, and has better charring performance than polyol charring agents such as pentaerythritol or micromolecule triazine charring agents.
3. The flame-retardant master batch prepared can avoid the problems of uneven dispersion, dust pollution and the like caused by directly adding the flame retardant, is favorable for direct injection molding of manufacturers without extrusion equipment, simplifies the processing process and improves the production efficiency.
Detailed Description
The present invention will be described in detail with reference to the following embodiments in order to make the aforementioned objects, features and advantages of the invention more comprehensible. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
The halogen-free flame-retardant master batch for the polyether TPU comprises the following components in percentage by mass:
36 to 48 percent of polyether TPU and 50 to 60 percent of halogen-free flame retardant
0.3 to 0.5 percent of anti-dripping agent and 0.2 to 0.5 percent of antioxidant
1 to 2 percent of lubricant and 0.5 to 1 percent of white mineral oil.
Example 1
This example evaluates the effect of different mass ratios of Aluminum Hypophosphite (AHP), melamine Cyanurate (MCA) and a macromolecular triazine char former (as exemplified by ETPC) on flame retardancy of polyether TPUs. When the halogen-free flame retardant is a compound consisting of aluminum hypophosphite, melamine cyanurate and a macromolecular triazine charring agent according to the mass ratio of 3.
The polyether type TPU halogen-free flame retardant material is prepared from the following raw materials in percentage by mass: 72% of polyether type TPU, 27% of halogen-free flame retardant, 0.3% of anti-dripping agent, 0.2% of antioxidant and 0.5% of lubricant, wherein the halogen-free flame retardant is a compound of aluminum hypophosphite, melamine cyanurate and macromolecular triazine charring agent (ETPC), the compound is compounded according to the mass ratio in the table 1, the anti-dripping agent is polytetrafluoroethylene, the antioxidant is tetra [ methyl- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester (antioxidant 1010), and the lubricant is N, N' -Ethylene Bis Stearamide (EBS).
Weighing polyether type TPU, halogen-free flame retardant, anti-dripping agent, antioxidant and lubricant according to the mass percent of the raw materials, uniformly stirring the polyether type TPU, the halogen-free flame retardant, the anti-dripping agent, the antioxidant and the lubricant in a high-speed mixer, adding the mixture into a double-screw machine for extrusion granulation, controlling the processing temperature to be 160-180 ℃, drying the granulated particles, and performing UL94 vertical combustion test and limited oxygen index test by injection molding into a standard sample strip. The test results are shown in Table 1.
Table 1:
as can be seen from the results in Table 1, the oxygen index of the halogen-free flame retardant without ETPC or with ETPC only is very low, and the vertical burning UL-94 is not graded. As the addition amount of ETPC is increased, the oxygen index is increased, and UL-94 reaches V-0 grade from a stepless grade. When AHP MCA: ETPC =3:1: at 1.5, the average burn time was the shortest, the oxygen index was the highest, the LOI was 31.5, and the vertical burn UL-94 was V-0. As the amount of ETPC added continues to increase, the average burn time gradually increases, the oxygen index gradually decreases, and the vertical burn UL-94 becomes V-1 grade.
Example 2
This example evaluates the effect of the number of halogen-free flame retardant additives on the flame retardancy of polyether TPU.
The polyether type TPU halogen-free flame retardant material is prepared from the following raw materials in percentage by mass: 69-80% of polyether type TPU, 0.3% of anti-dripping agent, 0.2% of antioxidant and 0.5% of lubricant, wherein the halogen-free flame retardant is a compound of aluminum hypophosphite, melamine cyanurate and a macromolecular triazine charring agent (ETPC) according to the mass ratio of 3:1:1.5, compounding, wherein the anti-dripping agent is polytetrafluoroethylene, the antioxidant is tetra [ methyl- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester (antioxidant 1010), and the lubricant is N, N' -Ethylene Bis Stearamide (EBS).
Weighing polyether type TPU, halogen-free flame retardant, anti-dripping agent, antioxidant and lubricant according to the mass percent of the raw materials, uniformly stirring the polyether type TPU, the halogen-free flame retardant, the anti-dripping agent, the antioxidant and the lubricant in a high-speed mixer, adding the mixture into a double-screw machine for extrusion granulation, controlling the processing temperature to be 160-180 ℃, drying the granulated particles, and performing UL94 vertical combustion test and limited oxygen index test by injection molding into a standard sample strip. The test results are shown in Table 2.
Table 2:
as can be seen from the results in Table 2, the more the amount of the halogen-free flame retardant added, the shorter the average combustion time, the larger the oxygen index gradually, and the vertical combustion UL-94 from V-2 level to V-0 level. 27 percent of halogen-free flame retardant is added, the LOI is 31.5, and the vertical burning UL-94 is V-0 grade. When the addition amount of the halogen-free flame retardant is increased, the oxygen index is not increased much, but the mechanical property of the material is reduced and the material cost is increased. Therefore, 27% of the halogen-free flame retardant is properly added into the polyether TPU.
Example 3
The polyether type halogen-free flame retardant master batch for the TPU is prepared from the following raw materials in percentage by mass: 36.5% of polyether type TPU, 60% of halogen-free flame retardant, 0.3% of anti-dripping agent, 0.2% of antioxidant, 2% of lubricant, 1% of white mineral oil, wherein the halogen-free flame retardant is a compound of aluminum hypophosphite, melamine cyanurate and a macromolecular triazine charring agent (ETPC), the mass ratio of the anti-dripping agent to the anti-dripping agent is 3. Aluminum hypophosphite and melamine cyanurate are frequently compounded in the market at present, 8% -16% of the aluminum hypophosphite and melamine cyanurate are added into polyester TPU to reach UL94V-0, but more than 45% of the aluminum hypophosphite and melamine cyanurate are added into polyether TPU to reach UL 94V-0. Aluminum hypophosphite, melamine cyanurate and a macromolecular triazine charring agent are compounded to serve as a halogen-free flame retardant, and the mass ratio of the halogen-free flame retardant to the melamine cyanurate to the macromolecular triazine charring agent is 3:1:1.5, the total addition mass fraction of the flame retardant reaches UL94V-0 only by 27 percent.
Weighing polyether type TPU, halogen-free flame retardant, anti-dripping agent, antioxidant, lubricant and white mineral oil according to the mass percentage of each raw material in the embodiment 3, firstly stirring the polyether type TPU and the white mineral oil uniformly in a high-speed mixer, then adding the halogen-free flame retardant, the anti-dripping agent, the antioxidant and the lubricant into the mixer to be mixed uniformly, adding the mixture into a double screw machine to extrude and granulate, controlling the processing temperature between 160 ℃ and 180 ℃, drying, cooling and packaging the granulated master batch to obtain the flame-retardant master batch.
Example 4
The polyether type halogen-free flame retardant master batch for the TPU is prepared from the following raw materials in percentage by mass: 47.5% of polyether type TPU, 50% of halogen-free flame retardant, 0.5% of anti-dripping agent, 0.5% of antioxidant, 1% of lubricant, 0.5% of white mineral oil, wherein the halogen-free flame retardant is a compound of aluminum hypophosphite, melamine cyanurate and a macromolecular triazine charring agent (PTCA), the mass ratio of the anti-dripping agent to the flame retardant is 3.
Weighing the polyether TPU, the halogen-free flame retardant, the anti-dripping agent, the antioxidant, the lubricant and the white mineral oil according to the mass percentage of the raw materials in the embodiment 4, firstly stirring the polyether TPU and the white mineral oil uniformly in a high-speed mixer, then adding the halogen-free flame retardant, the anti-dripping agent, the antioxidant and the lubricant, uniformly mixing, adding the mixture into a double-screw machine for extrusion granulation, controlling the processing temperature to be 160-180 ℃, drying, cooling and packaging the granulated master batch to obtain the flame-retardant master batch.
Example 5
The polyether type halogen-free flame retardant master batch for the TPU is prepared from the following raw materials in percentage by mass: 42% of polyether type TPU, 55% of halogen-free flame retardant, 0.4% of anti-dripping agent, 0.4% of antioxidant, 1.5% of lubricant, 0.7% of white mineral oil, wherein the halogen-free flame retardant is a compound of aluminum hypophosphite, melamine cyanurate and a macromolecular triazine charring agent (PEPAC), the mass ratio of the anti-dripping agent to the antioxidant is 3:1, the lubricant is zinc stearate.
Weighing the polyether TPU, the halogen-free flame retardant, the anti-dripping agent, the antioxidant, the lubricant and the white mineral oil according to the mass percentage of the raw materials in the embodiment 5, firstly stirring the polyether TPU and the white mineral oil uniformly in a high-speed mixer, then adding the halogen-free flame retardant, the anti-dripping agent, the antioxidant and the lubricant, uniformly mixing, adding the mixture into a double-screw machine for extrusion granulation, controlling the processing temperature to be 160-180 ℃, drying, cooling and packaging the granulated master batch to obtain the flame-retardant master batch.
Comparative example 1
The preparation method is characterized by comprising the following raw materials in percentage by mass: 99% of polyether type TPU, 0.3% of anti-dripping agent, 0.2% of antioxidant and 0.5% of lubricant, wherein the anti-dripping agent is polytetrafluoroethylene, the antioxidant is antioxidant 1010, and the lubricant is EBS.
Weighing TPU, anti-dripping agent, antioxidant and lubricant according to the mass percent of the raw materials in the comparative example 1, uniformly stirring in a high-speed mixer, then extruding and granulating in a double-screw extruder, controlling the processing temperature to be between 160 and 180 ℃, drying and cooling the granules formed by granulation for later use.
Comparative example 2
The polyether type halogen-free flame retardant master batch for the TPU is prepared from the following raw materials in percentage by mass: 36.5% of polyether type TPU, 60% of halogen-free flame retardant, 0.3% of anti-dripping agent, 0.2% of antioxidant, 2% of lubricant, 1% of white mineral oil, and the halogen-free flame retardant is a compound of aluminum hypophosphite and melamine cyanurate, wherein the mass ratio of the flame retardant to the white mineral oil is 2.
Weighing the polyether TPU, the halogen-free flame retardant, the anti-dripping agent, the antioxidant, the lubricant and the white mineral oil according to the mass percent of the raw materials in the comparative example 2, stirring the polyether TPU and the white mineral oil uniformly in a high-speed mixer, then adding the halogen-free flame retardant, the anti-dripping agent, the antioxidant and the lubricant, mixing uniformly, adding the mixture into a double screw machine for extrusion granulation, controlling the processing temperature to be between 160 and 180 ℃, drying and cooling the granulated master batch for later use.
The master batches of examples 3 to 5 and comparative examples 1 to 2 were injection-molded with polyether TPU, respectively, in the mass percentages given in Table 3, and the injection-molded standard sample bars were tested, the test results of which are given in Table 3.
Table 3:
the vertical burning test standard in each of the above examples was ASTM D3801, and the tensile strength and elongation at break were tested in accordance with ASTM D412; the limiting oxygen index test standard is ASTM D2863; the Shore A hardness is tested according to GB/T531-1999.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is specific and detailed, but not to be understood as limiting the scope of the invention. It should be noted that various changes and modifications can be made by those skilled in the art without departing from the spirit of the invention, and these changes and modifications are all within the scope of the invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (9)
1. The halogen-free flame-retardant master batch for the polyether TPU is characterized by comprising the following components in percentage by mass:
36 to 48 percent of polyether type TPU and 50 to 60 percent of halogen-free flame retardant
0.3 to 0.5 percent of anti-dripping agent and 0.2 to 0.5 percent of antioxidant
1 to 2 percent of lubricant and 0.5 to 1 percent of white mineral oil.
2. The halogen-free flame retardant masterbatch for polyether TPU according to claim 1, wherein the halogen-free flame retardant is a compound consisting of aluminum hypophosphite, melamine cyanurate, and a macromolecular triazine charring agent.
3. The halogen-free flame-retardant masterbatch for polyether TPU according to claim 2, wherein the mass ratio of aluminum hypophosphite, melamine cyanurate and macromolecular triazine charring agent in the compound is 3.
4. The halogen-free flame retardant masterbatch for polyether type TPU according to claim 2, wherein the mass ratio of aluminum hypophosphite, melamine cyanurate and macromolecular triazine charring agent in the compound is 3.
5. The polyether type halogen-free flame retardant masterbatch for TPU according to claim 2, wherein the macromolecular triazine char-forming agent is synthesized from cyanuric chloride, ethylamine and piperazine, or from cyanuric chloride, diphenylamine and ethylenediamine, or from cyanuric chloride, piperazine and caged phosphate.
6. The halogen-free flame retardant masterbatch for polyether TPU according to claim 1, wherein the anti-dripping agent is polytetrafluoroethylene.
7. The halogen-free flame retardant masterbatch for polyether type TPU according to claim 1, wherein the antioxidant is one or more of pentaerythritol tetrakis [ methyl- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], 1,3, 5-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) isocyanurate, 1,3, 5-tris (4-tert-butyl-3-hydroxy-2, 6-dimethylbenzyl) -1,3, 5-triazine-2, 4,6- (1H, 3H, 5H) -trione, tris (2, 4-di-tert-butylphenyl) phosphite (antioxidant 168), bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite (antioxidant THP-24), distearyl thiodipropionate.
8. The halogen-free flame retardant masterbatch for polyether type TPU according to claim 1, wherein the lubricant is one or more of calcium stearate, zinc stearate, polyethylene wax, and N, N' -ethylene bis stearamide.
9. A preparation method for preparing the halogen-free flame retardant master batch for the polyether TPU of claim 1, which is characterized by comprising the following steps:
weighing the polyether TPU, the halogen-free flame retardant, the anti-dripping agent, the antioxidant, the lubricant and the white mineral oil according to the mass percent of claim 1, uniformly stirring the polyether TPU and the white mineral oil in a high-speed mixer, then adding the halogen-free flame retardant, the anti-dripping agent, the antioxidant and the lubricant, uniformly mixing, adding the mixture into a double-screw machine, extruding and granulating, wherein the processing temperature is 160-180 ℃, drying, cooling and packaging the granulated master batch to obtain the flame-retardant master batch.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103333336A (en) * | 2013-06-04 | 2013-10-02 | 合肥安聚达新材料科技有限公司 | Preparation method of novel hyperbranched triazine char forming agent |
| CN104693782A (en) * | 2015-03-18 | 2015-06-10 | 苏州安鸿泰新材料有限公司 | Halogen-free flame retardant polyether thermoplastic polyurethane elastomer and preparation method thereof |
| CN106939095A (en) * | 2017-03-31 | 2017-07-11 | 江苏坤宇集团有限公司 | Flame-retardant compounds based on three piperazine triazine carbon forming agents |
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- 2021-05-31 CN CN202110600031.0A patent/CN115477838A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103333336A (en) * | 2013-06-04 | 2013-10-02 | 合肥安聚达新材料科技有限公司 | Preparation method of novel hyperbranched triazine char forming agent |
| CN104693782A (en) * | 2015-03-18 | 2015-06-10 | 苏州安鸿泰新材料有限公司 | Halogen-free flame retardant polyether thermoplastic polyurethane elastomer and preparation method thereof |
| CN106939095A (en) * | 2017-03-31 | 2017-07-11 | 江苏坤宇集团有限公司 | Flame-retardant compounds based on three piperazine triazine carbon forming agents |
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| Title |
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