CN113912938B - Ultraviolet aging resistant flame-retardant polypropylene material and preparation method thereof - Google Patents
Ultraviolet aging resistant flame-retardant polypropylene material and preparation method thereof Download PDFInfo
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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
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- C08K5/00—Use of organic ingredients
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- 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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- C08L2201/02—Flame or fire retardant/resistant
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Abstract
The invention discloses an anti-ultraviolet aging flame-retardant polypropylene material and a preparation method thereof, wherein the anti-ultraviolet aging flame-retardant polypropylene material is prepared from homo-polypropylene, melamine hydrobromide, hypophosphorous acid rare earth salt, a flame-retardant synergist and a lubricant in a mass ratio of 96-98.25: 0.3-1.5:0.2-1: 0.25-0.5: 1. The invention utilizes the characteristics of rare earth salt, can lead the polypropylene material to have certain flame retardance and certain ultraviolet light aging resistance, effectively overcomes the defects of poor heat resistance, invalidation of light stabilizer and the like of the halogen flame retardant, greatly expands the application range and application prospect of the halogen flame retardant and the polypropylene material, and simultaneously has obvious advantages when preparing non-woven fabrics and fibers due to extremely low usage amount.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to an ultraviolet aging resistant flame-retardant polypropylene material and a preparation method thereof.
Background
Polypropylene (PP) as a general thermoplastic has the advantages of high crystallinity, regular structure, good heat resistance and the like. However, the Limiting Oxygen Index (LOI) of the pure PP resin is very low, which is only about 18%, and the ultraviolet aging resistance is relatively poor. PP can produce a large amount of smoke and toxic gas in the combustion process, and has great threat to the life health of people. And meanwhile, PP has great influence on the service performance under long-term ultraviolet irradiation. Therefore, the polypropylene is subjected to ultraviolet aging resistance and flame retardant modification, and the polypropylene has important significance for expanding the application field and protecting the life health of people.
At present, the flame retardants used in polypropylene are mainly halogen flame retardants, phosphorus flame retardants, intumescent flame retardants, metal hydroxides, and the like. However, phosphorus flame retardants, intumescent flame retardants, and metal hydroxides have the disadvantages of large addition amount and relatively high cost, and have adverse effects on the mechanical properties of the materials, so that the application of the phosphorus flame retardants, intumescent flame retardants, and metal hydroxides is limited. The halogen flame retardant occupies an important position in the flame-retardant polypropylene market due to the advantages of proper price, high flame-retardant efficiency and the like. With the enhancement of environmental awareness and the perfection of relevant laws and regulations, the low halogenation of flame retardant materials becomes a trend. Therefore, the selection of a proper synergistic flame retardant to reduce the addition amount of the halogen flame retardant is crucial to the application and development of the halogen flame retardant.
On the other hand, polypropylene is easily degraded by auto-photo-oxidation (aging) and cannot be used due to the influence of light and heat in the natural environment, and the weather resistance of polypropylene is improved by adding light stabilizers and antioxidants. The method is simple and feasible, and is the most practical and widely applied method at present. However, the brominated flame retardant and the traditional HALS light stabilizer have antagonism when irradiated by ultraviolet light, and mainly HBr generated by the brominated flame retardant under the action of the ultraviolet light reacts with the alkaline HALS to cause the light stabilizer to lose efficacy.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide an ultraviolet aging resistant flame-retardant polypropylene material.
The invention also aims to provide a preparation method of the ultraviolet aging resistant flame-retardant polypropylene material.
The technical scheme of the invention is as follows:
an anti-ultraviolet aging flame-retardant polypropylene material is prepared from homopolymerized polypropylene, melamine hydrobromide, hypophosphorous acid rare earth salt, flame-retardant synergist and lubricant in a mass ratio of 96-98.25: 0.3-1.5:0.2-1: 0.25-0.5:1,
the rare earth hypophosphite is cerium hypophosphite, lanthanum hypophosphite, alkyl cerium hypophosphite, phenyl lanthanum hypophosphite or phenyl cerium hypophosphite;
the flame retardant synergist is phosphotungstic acid metal salt or organic synergist, and the structural formula of the organic synergist is
R 1 To R 4 Are respectively and independently C1-C6 alkyl, X is alkyl, halogen, amino or sulfonic group, and Y is alkyl, halogen, amino or sulfonic group.
In a preferred embodiment of the present invention, the rare earth hypophosphite is cerium hypophosphite, cerium phenyl hypophosphite, lanthanum phenyl hypophosphite or lanthanum tert-butyl hypophosphite.
Further preferably, the rare earth hypophosphite is cerium hypophosphite.
In a preferred embodiment of the present invention, the metal phosphotungstate is sodium phosphotungstate or calcium phosphotungstate.
In a preferred embodiment of the invention, the organic synergist is 2, 3-dimethyl-2, 3-diphenylbutane.
In a preferred embodiment of the invention, the lubricant is EBS.
In a preferred embodiment of the present invention, the rare earth hypophosphite is cerium hypophosphite, cerium phenyl hypophosphite, lanthanum phenyl hypophosphite or lanthanum tert-butyl hypophosphite, the metal phosphotungstate is sodium phosphotungstate or calcium phosphotungstate, the organic synergist is 2, 3-dimethyl-2, 3-diphenylbutane, and the lubricant is EBS.
Further preferably, the rare earth hypophosphite is cerium hypophosphite.
The preparation method of the ultraviolet aging resistant flame-retardant polypropylene material comprises the following steps:
(1) Adding the homopolymerized polypropylene, melamine hydrobromide, hypophosphorous acid rare earth salt, the flame retardant synergist and the lubricant into a tellurion mixer to be fully mixed;
(2) And (2) melting, mixing, extruding and granulating the material obtained in the step (1) through a double-screw extruder to obtain the material.
In a preferred embodiment of the invention, the twin-screw extruder has a rotational speed of 180 to 200rpm and an extrusion temperature of 190 to 210 ℃.
The invention has the beneficial effects that:
1. according to the invention, stable ultraviolet aging resistant and flame retardant PP (polypropylene) compound is obtained by utilizing the ultraviolet aging resistant and synergistic flame retardant property of the rare earth hypophosphite, the rare earth hypophosphite has a unique effect in coordination with MHB flame retardant, the defects of relatively high addition amount of a halogen flame retardant and the like are effectively overcome, a high flame retardant grade can be obtained by extremely low addition amount, the addition amount of the halogen flame retardant meets the Rohs regulation requirements of European Union, the total halogen content is less than 1500ppm, and the PP compound is more environment-friendly.
2. The hypophosphorous acid rare earth salt has the ultraviolet aging resistance effect, and has better thermal stability compared with an anti-aging auxiliary agent such as a light stabilizer; the halogen flame retardant and the traditional HALS light stabilizer can generate antagonism when being irradiated by ultraviolet light, so that the light stabilizer can lose efficacy, the defect is overcome by using the hypophosphorous acid rare earth salt, and the application range of the halogen flame retardant and the polypropylene can be greatly expanded.
3. The invention is applied to the fields of building materials, electronic appliances and the like, and can provide more durable and more efficient ultraviolet aging resistance and flame retardant effect.
Detailed Description
The technical solution of the present invention is further illustrated and described by the following detailed description.
The melt flow rate of the homo-polypropylene in the following examples was 2.0 to 20.0g/10min, and the isotactic index was 97.0. + -. 0.5%.
Example 1:
96.25 parts of homo-polypropylene, 1.5 parts of MHB (CAS number: 29305-12-2), 1 part of cerium hypophosphite, 0.25 part of 2, 3-dimethyl-2, 3-diphenylbutane and 1 part of lubricant EBS are weighed and added into a high-speed mixer to be mixed for 5min.
And melting, mixing, extruding, granulating, drying and injection molding the obtained mixture by a double-screw extruder (the rotating speed is 200rpm, and the extrusion temperature from the feeding section to a die head is 165 ℃, 180 ℃, 190 ℃, 200 ℃, 210 ℃, 205 ℃, 210 ℃ and 210 ℃ in sequence) to obtain the ultraviolet aging resistant flame retardant polypropylene material.
Example 2:
96.75 parts of homo-polypropylene, 1.2 parts of MHB, 0.8 part of cerium hypophosphite, 0.25 part of 2, 3-dimethyl-2, 3-diphenylbutane and 1 part of lubricant EBS are weighed and added into a high-speed mixer to be mixed for 5min.
The preparation method is the same as example 1.
Example 3:
97.75 parts of homo-polypropylene, 0.6 part of MHB, 0.4 part of cerium hypophosphite, 0.25 part of 2, 3-dimethyl-2, 3-diphenylbutane and 1 part of lubricant EBS are weighed and added into a high-speed mixer to be mixed for 5min.
The preparation method is the same as example 1.
Example 4:
98.25 parts of homo-polypropylene, 0.3 part of MHB, 0.2 part of cerium hypophosphite, 0.25 part of 2, 3-dimethyl-2, 3-diphenylbutane and 1 part of lubricant EBS are weighed and added into a high-speed mixer to be mixed for 5min.
The preparation method is the same as example 1.
Example 5:
96.25 parts of homopolymerized polypropylene, 1.5 parts of MHB, 1 part of cerium hypophosphite, 0.25 part of sodium phosphotungstate and 1 part of lubricant EBS are weighed and added into a high-speed mixer to be mixed for 5min.
The preparation method is the same as example 1.
Example 6:
96.75 parts of homo-polypropylene, 1.2 parts of MHB, 0.8 part of cerium hypophosphite, 0.25 part of calcium phosphotungstate and 1 part of lubricant EBS are weighed and added into a high-speed mixer to be mixed for 5min.
The preparation method is the same as example 1.
Example 7:
97.5 parts of homo-polypropylene, 0.6 part of MHB, 0.4 part of cerium hypophosphite, 0.5 part of 2, 3-dimethyl-2, 3-diphenylbutane and 1 part of lubricant EBS are weighed and added into a high-speed mixer to be mixed for 5min.
The preparation method is the same as example 1.
Example 8:
98 parts of homo-polypropylene, 0.3 part of MHB, 0.2 part of cerium hypophosphite, 0.5 part of 2, 3-dimethyl-2, 3-diphenylbutane and 1 part of lubricant EBS are weighed and added into a high-speed mixer to be mixed for 5min.
The preparation method is the same as example 1.
Example 9
97.5 parts of homo-polypropylene, 0.6 part of MHB, 0.4 part of lanthanum hypophosphite, 0.5 part of 2, 3-dimethyl-2, 3-diphenylbutane and 1 part of lubricant EBS are weighed and added into a high-speed mixer to be mixed for 5min.
The preparation method is the same as example 1.
Example 10
97.5 parts of homo-polypropylene, 0.6 part of MHB, 0.4 part of cerium phenylphosphinate, 0.5 part of 2, 3-dimethyl-2, 3-dibrominated phenylbutane and 1 part of lubricant EBS are weighed and added into a high-speed mixer to be mixed for 5min.
The preparation method is the same as example 1.
Example 11
97.5 parts of homo-polypropylene, 0.6 part of MHB, 0.4 part of lanthanum phenylphosphinate, 0.5 part of 2, 3-diethyl-2, 3-diphenylaminooctane and 1 part of lubricant EBS are weighed and added into a high-speed mixer to be mixed for 5min.
The preparation method is the same as example 1.
Example 12
97.5 parts of homo-polypropylene, 0.6 part of MHB, 0.4 part of cerium methyl hypophosphite, 0.5 part of 2, 3-dimethyl-2, 3-ditolyl butane and 1 part of lubricant EBS are weighed and added into a high-speed mixer to be mixed for 5min.
The preparation method is the same as example 1.
Example 13
98 parts of homo-polypropylene, 0.3 part of MHB, 0.2 part of lanthanum tert-butylphosphinate, 0.5 part of 2, 3-dimethyl-2, 3-di (benzenesulfonic acid) based hexane and 1 part of lubricant EBS were weighed and mixed in a high-speed mixer for 5min.
The preparation method is the same as example 1.
Comparative example 1:
96.25 parts of homo-polypropylene, 1.5 parts of MHB, 1 part of aluminum hypophosphite, 0.25 part of 2, 3-dimethyl-2, 3-diphenylbutane and 1 part of lubricant EBS are weighed and added into a high-speed mixer to be mixed for 5min.
The preparation method is the same as example 1.
Comparative example 2:
98.25 parts of homo-polypropylene, 0.3 part of MHB, 0.2 part of aluminum hypophosphite, 0.25 part of 2, 3-dimethyl-2, 3-diphenylbutane and 1 part of lubricant EBS are weighed and added into a high-speed mixer to be mixed for 5min.
The preparation method is the same as example 1.
Comparative example 3:
96.25 parts of homo-polypropylene, 2.5 parts of MHB, 0.25 part of 2, 3-dimethyl-2, 3-diphenylbutane and 1 part of lubricant EBS are weighed and added into a high-speed mixer to be mixed for 5min.
The preparation method is the same as example 1.
Comparative example 4:
96.25 parts of homo-polypropylene, 2.75 parts of MHB and 1 part of lubricant EBS are weighed and added into a high-speed mixer to be mixed for 5min.
The preparation method is the same as example 1.
Comparative example 5:
96.25 parts of homo-polypropylene, 1.65 parts of MHB, 1.1 parts of cerium hypophosphite and 1 part of lubricant EBS are weighed and added into a high-speed mixer to be mixed for 5min.
The preparation method is the same as example 1.
Comparative example 6:
96.25 parts of homo-polypropylene, 2.5 parts of cerium hypophosphite, 0.25 part of 2,3= dimethyl-2, 3-diphenylbutane and 1 part of lubricant EBS are weighed and added into a high-speed mixer to be mixed for 5min.
The preparation method is the same as example 1.
Comparative example 7:
96.25 parts of homopolymerized polypropylene, 2.75 parts of cerium hypophosphite and 1 part of lubricant EBS are weighed and added into a high-speed mixer to be mixed for 5min.
The preparation method is the same as example 1.
The technical effects of the above examples and comparative examples are shown in tables 1 to 4 below:
TABLE 1
* ff is the total time of the first flame combustion, the second flame combustion and the flameless combustion of 5 specimens;
* The above UL-94 test samples all produced droplets and ignited absorbent cotton.
* The aging test is to carry out the flame retardant performance test after aging the sample strips in a thermal oxidation aging box for 168 hours at 150 ℃.
The above table 1 shows that the flame retardant effect is optimized only by the co-participation of MHB, cerium hypophosphite and the flame retardant synergist.
TABLE 2
TABLE 3
* The change delta YI of the yellow index is measured after irradiation at 340nm, 168h and 50-60 ℃.
* The melt index of the homopolymeric PP was 3.2g/min.
It can be seen from tables 2 and 3 that when the total addition amount of the flame retardant is 2.75%, the hypophosphorous acid rare earth salt synergistic MHB flame-retardant PP before aging and the comparative aluminum hypophosphite synergistic MHB flame-retardant PP have almost the same flame-retardant grade and mechanical property, but the hypophosphorous acid rare earth salt has better mechanical property and flame-retardant property compared with the aluminum hypophosphite synergistic MHB after artificial accelerated aging, which indicates that the hypophosphorous acid rare earth salt plays the roles of ultraviolet aging resistance and MHB flame retardance.
TABLE 4
As can be seen from Table 4, when the addition amount of the flame retardant is reduced, the flame retardant effects of the rare earth hypophosphite and the MHB flame-retardant PP are obviously different from the flame retardant effects of the comparative aluminum hypophosphite and the MHB flame-retardant PP before and after aging, and the fact that the rare earth hypophosphite can achieve better flame retardant and ultraviolet aging resistant effects at an extremely low addition amount compared with the traditional metal hypophosphite is shown.
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims.
Claims (9)
1. An ultraviolet aging resistant flame-retardant polypropylene material is characterized in that: the flame retardant is prepared from homo-polypropylene, melamine hydrobromide, hypophosphorous acid rare earth salt, a flame retardant synergist and a lubricant according to a mass ratio of 96-98.25: 0.3-1.5,
the rare earth hypophosphite is cerium hypophosphite, lanthanum hypophosphite, alkyl cerium hypophosphite, phenyl lanthanum hypophosphite or phenyl cerium hypophosphite;
the flame retardant synergist is phosphotungstate metal salt or organic synergist, the phosphotungstate metal salt is sodium phosphotungstate or calcium phosphotungstate, and the structural formula of the organic synergist is
，R 1 To R 4 Are respectively and independently C1-C6 alkyl, X is alkyl, halogen, amino or sulfonic group, and Y is alkyl, halogen, amino or sulfonic group.
2. The ultraviolet aging resistant and flame retardant polypropylene material of claim 1, wherein: the rare earth hypophosphite is cerium hypophosphite, phenyl cerium hypophosphite, lanthanum hypophosphite, phenyl lanthanum hypophosphite or tert-butyl lanthanum hypophosphite.
3. The ultraviolet aging resistant and flame retardant polypropylene material of claim 2, wherein: the rare earth hypophosphite is cerium hypophosphite.
4. The ultraviolet aging resistant and flame retardant polypropylene material of claim 1, wherein: the organic synergist is 2, 3-dimethyl-2, 3-diphenyl butane.
5. The ultraviolet aging resistant and flame retardant polypropylene material of claim 1, wherein: the lubricant is EBS.
6. The ultraviolet aging resistant and flame retardant polypropylene material of claim 1, wherein: the rare earth hypophosphite is cerium hypophosphite, cerium phenyl hypophosphite, lanthanum phenyl hypophosphite or tert-butyl lanthanum hypophosphite, the metal phosphotungstate is sodium phosphotungstate or calcium phosphotungstate, the organic synergist is 2, 3-dimethyl-2, 3-diphenylbutane, and the lubricant is EBS.
7. The ultraviolet aging resistant and flame retardant polypropylene material of claim 6, wherein: the rare earth hypophosphite is cerium hypophosphite.
8. The preparation method of the ultraviolet aging resistant flame retardant polypropylene material of any one of claims 1 to 7, wherein the preparation method comprises the following steps: the method comprises the following steps:
(1) Adding the homo-polypropylene, melamine hydrobromide, hypophosphorous acid rare earth salt, flame retardant synergist and lubricant into a high-speed mixer, and fully mixing;
(2) And (2) melting, mixing, extruding and granulating the material obtained in the step (1) through a double-screw extruder to obtain the material.
9. The method of claim 8, wherein: the rotating speed of the double-screw extruder is 180-200rpm, and the extrusion temperature is 190-210 ℃.
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