CN112111094A - Resin-coated diethyl aluminum hypophosphite flame-retardant low-density polyethylene and preparation method thereof - Google Patents
Resin-coated diethyl aluminum hypophosphite flame-retardant low-density polyethylene and preparation method thereof Download PDFInfo
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
- C08G8/10—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with phenol
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- 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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Abstract
The invention belongs to the field of high polymer materials, and particularly relates to resin-coated diethyl aluminum hypophosphite (PF @ ADP) flame-retardant low-density polyethylene and a preparation method thereof. The flame-retardant low-density polyethylene comprises the following components in percentage by mass: low density polyethylene: 70% -80%, PF @ ADP: 20 to 30 percent. And melting and blending PF @ MADP and low-density polyethylene in an internal mixer to obtain the resin-coated diethyl aluminum hypophosphite flame-retardant low-density polyethylene. The Limit Oxygen Index (LOI) of the intumescent flame-retardant low-density polyethylene can reach 31.3 when the addition amount of PF @ ADP (PF: 30% and ADP: 70%) is 30%, and the flame-retardant grade reaches UL94-V0, so that the intumescent flame-retardant low-density polyethylene has wide application prospect.
Description
Technical Field
The invention belongs to the field of high polymer materials, and particularly discloses resin-coated diethyl aluminum hypophosphite flame-retardant low-density polyethylene and a preparation method thereof.
Background
Low Density Polyethylene (LDPE) is a thermoplastic resin material polymerized from ethylene monomers, has the characteristics of excellent electrical insulation property, chemical corrosion resistance, easy processability and the like, and is widely applied to the production of cables, building materials, plastic films and the like. However, LDPE is flammable (oxygen index is only about 17%), with severe melting, dripping and flaming phenomena during combustion and release of toxic and harmful gases. Therefore, it is important to improve the application safety of LDPE by flame retardant modification.
The flame retardant researched for LDPE flame retardation mainly comprises halogen flame retardants and halogen-free flame retardants, wherein the halogen flame retardants are most widely used and have high flame retardation efficiency, but the halogen flame retardants can generate a large amount of toxic smoke while being flame-retardant, so that people can easily smoke and suffocate the toxic smoke when inhaling the toxic smoke, and the halogen flame retardants are not environment-friendly. The development of a safe, environment-friendly and high-performance halogen-free flame retardant system suitable for LDPE becomes one of the research hotspots.
The literature reports that the halogen-free flame retardant applied to LDPE comprises metal hydroxide, phosphorus flame retardant and the like. The metal hydroxide mainly comprises magnesium hydroxide and aluminum hydroxide, and has the advantages of wide and easily available source, low price, environmental protection, high safety and smoke suppression. However, the addition amount of the material reaches 40-60% when the material is used, and the mechanical property and the processing property of the material are seriously damaged. The phosphorus flame retardant mainly comprises an organic phosphorus flame retardant and an inorganic phosphorus flame retardant, wherein the organic phosphorus flame retardant is considered to be one of the most promising flame retardants for replacing halogen flame retardants, particularly alkyl hypophosphite, has high flame retardant efficiency and small influence on the mechanical properties of materials, and does not contain P-O-C bonds in a molecular structure, thereby being beneficial to improving the hydrolysis resistance. Diethyl aluminum hypophosphite (ADP) is taken as a representative of alkyl hypophosphite, and has the characteristics of low toxicity, high efficiency, good color, low smoke density during combustion, good thermal stability and the like, so that the diethyl aluminum hypophosphite is widely concerned at home and abroad. However, the diethyl aluminum hypophosphite is rarely reported in LDPE flame retardance, because diethyl aluminum hypophosphite is an inorganic metal flame retardant and cannot be well compatible in low-density polyethylene, meanwhile, the binding force of ADP and LDPE is different, certain internal stress is easily caused, the flame retardant particles are distributed in an LDPE matrix to destroy the binding capacity, the interface is debonded when a force is applied, and the mechanical property is reduced.
Disclosure of Invention
The invention aims to provide phenolic resin (PF) stably coated diethyl aluminum hypophosphite flame-retardant low-density polyethylene and a preparation method thereof, which can improve the flame retardant property of the low-density polyethylene and the compatibility of a flame retardant and LDPE, thereby reducing the deterioration of mechanical properties.
The flame-retardant low-density polyethylene provided by the invention comprises the following components in percentage by mass: low Density Polyethylene (LDPE): 70% -80%; flame retardant PF @ ADP: 20% -30%;
further, the flame-retardant low-density polyethylene comprises the following components in percentage by mass: low Density Polyethylene (LDPE): 70%, flame retardant PF @ ADP: 30%, Low Density Polyethylene (LDPE): 75%, flame retardant PF @ ADP: 25%, Low Density Polyethylene (LDPE): 80%, flame retardant PF @ ADP: 20 percent.
The invention adopts an emulsion polymerization method to prepare the PF @ ADP flame retardant, and the PF @ ADP flame retardant and the LDPE are subjected to melt blending to prepare the PF stably-coated ADP flame-retardant LDPE. The oxygen index of the product can meet the requirement of a flame-retardant material, and the degradation of the mechanical property of the material is reduced.
(1) Preparation method of PF @ ADP flame retardant
(a) Respectively weighing phenol and formaldehyde solution according to the mass ratio of 4:5, adding the phenol and formaldehyde solution into a three-neck flask, heating the three-neck flask to 60 ℃, adjusting the pH to 8.0-9.0 by using 10% sodium hydroxide solution, heating the three-neck flask to 75 ℃ for reaction for 2.0h, adjusting the pH to 7.0 by using acetic acid solution to obtain brown viscous liquid, namely PF prepolymer, adding 180mL of distilled water, and cooling the liquid for later use.
(b) Weighing ADP powder, filling the ADP powder into a three-necked bottle with a stirring and condensing device, adding a proper amount of ethanol, dispersing for 20min, adding the prepolymer, adjusting the pH to 3.0-4.0 by using 10% of dilute hydrochloric acid, reacting for 2.0h at 80 ℃, adjusting to be neutral by using 10% of NaOH solution, filtering, washing, putting the PF @ ADP subjected to dehydration treatment into a drying box, drying for 3.0h at 135 ℃, completely crosslinking and curing the PF, and crushing and grinding to obtain a resin-coated diethyl aluminum hypophosphite product.
Wherein, the fineness of ADP is 1-5 μm, the phosphorus content in ADP is 23% -24%, and the aluminum content is 6% -7%.
The ADP content in the resin-coated diethyl aluminum hypophosphite is 60-75%.
(2) Preparation of flame-retardant LDPE
Dried LDPE (70% -90%), PF @ ADP (10% -30%) were prepared in mass%. Setting the internal mixing temperature of the internal mixer to 145-155 ℃, slowly pouring LDPE into the internal mixer from a feeding port after the temperature is stable, slowly adding the mixture of PF @ ADP, fully extruding and shearing under the action of a double rotor, and fully mixing the LDPE and the PF @ ADP flame retardant. And (3) operating for 10-15min, sequentially opening the two movable plates of the internal mixer, and sampling to obtain the diethyl aluminum hypophosphite coated flame-retardant low-density polyethylene.
Has the advantages that:
1. the invention adopts in-situ coated diethyl aluminum hypophosphite, and provides a solution for the problem of halogen-free flame retardance of the low-density polyethylene.
2. The resin-coated diethyl aluminum hypophosphite disclosed by the invention not only has a good flame retardant effect on low-density polyethylene, but also is beneficial to improving the compatibility between a flame retardant and LDPE (low-density polyethylene), so that the degradation of mechanical properties is reduced, and the application influence on LDPE is small.
Drawings
FIG. 1 is an infrared spectrum of ADP and PF @ ADP.
Figures 2 and 3 are SEM images of ADP and PF @ ADP, respectively.
FIG. 4 is a TG plot of LDPE, LDPE mixed with ADP (comparative example 1) and LDPE mixed with PF @ ADP (example 2).
FIG. 5 is a plot of the luminous flux for smoke density testing of LDPE, LDPE mixed with ADP (comparative example 1) and LDPE mixed with PF @ ADP (example 2).
Detailed Description
The present invention is further described below with reference to examples, but is not limited thereto.
Example 1
The diethyl aluminum hypophosphite coated flame-retardant low-density polyethylene consists of the following components in percentage by mass: LDPE (Low-Density polyethylene): 80%, PF @ ADP (PF: 25%, ADP: 75%): 20 percent. The preparation process comprises the following steps:
(1) 33.7g of phenol and 44mL of formaldehyde solution are respectively weighed and added into a three-neck flask to be heated to 60 ℃, the pH value is adjusted to 8.0-9.0, the mixture is uniformly stirred at 1000rpm to react for 2.0h, the pH value is adjusted to be neutral to obtain brown viscous liquid, 23.1g of brown viscous liquid is weighed and is added into 50mL of distilled water to be cooled for standby (PF prepolymer).
(2) Weighing 45g of ADP, adding into a three-necked bottle, adding 225mL of ethanol, dispersing for 20min, adding the PF prepolymer in the step (1), adjusting the pH value to 3.0-4.0, and heating to 80 ℃ for reaction for 2.0 h.
(3) The pH was adjusted to neutral, and the resulting suspension was centrifuged at 8000rpm for 3min, then washed with distilled water, and repeated twice.
(4) The centrifuged material was dried in an oven at 135 ℃ for 3.0h, and the dried sample was ground to prepare a PF @ ADP flame retardant.
(5) Putting the flame retardant and the low-density polyethylene into a 60 ℃ oven for 12.0h, drying and dehydrating,
(6) the banburying temperature of the banbury mixer is set to 150 ℃, and after the temperature is stable, the feeding is started.
(7) Firstly, pouring dried LDPE into an internal mixer from a charging opening, adding dried ADP, fully extruding and shearing the ADP under the action of a double rotor, and fully mixing the LDPE and the intumescent flame retardant; and after running for 15min, sequentially opening two movable plates of the internal mixer, and sampling to obtain the LDPE/ADP material.
FIG. 1 is an infrared spectrum of ADP and PF @ ADP. It can be seen that 2880cm-1And 2958cm-1is-CH3The absorption peak of (1). 1460cm-1And 1371cm-1is-CH3And (3) absorption peak due to C-H bending vibration in (1). 1150cm-1Is the absorption peak of P ═ O stretching vibration, 1078cm-1Is the absorption peak of the stretching vibration of P-O. At the same time, 1230cm-1Is the P-C tensile shock absorption peak. Further, the internal stretching vibration absorption peaks of the benzene rings C ═ C appeared at 1512cm respectively-1And 1613cm-1To (3). 1371cm-1The peak is an O-H bending vibration peak, and the peak intensity is improved. At the same time, 1005cm-1Has an enhanced absorption peak at 756cm-1A new absorption peak appeared due to the 1, 2, 4 substituents in the phenyl ring and the 1, 2 substituents in the phenyl ring, indicating that PF is coated with ADP.
Fig. 2 and 3 are SEM images of ADP and PF @ ADP, respectively, and it can be seen that ADP particles are ellipsoidal, have a relatively rough surface, have a particle size of less than 5 μm, and have a slightly increased particle size and a smooth and dense surface after being coated with a phenolic resin, indicating that PF @ ADP was successfully prepared.
The properties of the example material are shown in table 1.
Example 2
The diethyl aluminum hypophosphite coated flame-retardant low-density polyethylene consists of the following components in percentage by mass: LDPE (Low-Density polyethylene): 80%, PF @ ADP (PF: 30%, ADP: 70%): 20 percent. The preparation process comprises the following steps:
(1) 33.7g of phenol and 44mL of formaldehyde solution are respectively weighed and added into a three-neck flask to be heated to 60 ℃, the pH value is adjusted to 8.0-9.0, the mixture is uniformly reacted for 2.0h under the stirring of 1000rpm, the pH value is adjusted to be neutral to obtain brown viscous liquid, and 27.7g of brown viscous liquid is weighed and added into 50mL of distilled water to be cooled for standby.
(2) Weighing 42g of ADP, adding into a three-necked bottle, adding 210mL of ethanol, dispersing for 20min, adding the PF prepolymer in the step (1), adjusting the pH value to 3.0-4.0, and heating to 80 ℃ for reaction for 2.0 h.
(3) The pH was adjusted to neutral, and the resulting suspension was centrifuged at 8000rpm for 3min, then washed with distilled water, and repeated twice.
(4) The centrifuged material was dried in an oven at 135 ℃ for 3.0h, and the dried sample was ground to prepare a PF @ ADP flame retardant.
(5) The drying and banburying steps of example 1 are repeated for the weighed LDPE and PF @ ADP to obtain the LDPE/PF @ ADP material.
FIG. 4 is a TG plot of LDPE, LDPE mixed with ADP (comparative example 1) and LDPE mixed with PF @ ADP (example 2). The ADP coated by PF can improve the thermal stability of the LDPE composite material to a certain extent.
FIG. 5 is a plot of the luminous flux for smoke density testing of LDPE, LDPE mixed with ADP (comparative example 1) and LDPE mixed with PF @ ADP (example 2). The ADP can effectively inhibit the smoke release amount of the LDPE composite material after being coated by PF.
The properties of the example materials are shown in Table 1
Example 3
The diethyl aluminum hypophosphite coated flame-retardant low-density polyethylene consists of the following components in percentage by mass: LDPE (Low-Density polyethylene): 80%, PF @ ADP (PF: 40%, ADP: 60%): 20 percent. The preparation process comprises the following steps:
(1) 33.7g of phenol and 44mL of formaldehyde solution are respectively weighed and added into a three-neck flask to be heated to 60 ℃, the pH value is adjusted to 8.0-9.0, the mixture is uniformly reacted for 2.0h under the stirring of 1000rpm, the pH value is adjusted to be neutral to obtain brown viscous liquid, and 36.9g of brown viscous liquid is weighed and added into 70mL of distilled water to be cooled for standby.
(2) Weighing 36g of ADP, adding into a three-necked bottle, adding 180mL of ethanol, dispersing for 20min, adding the PF prepolymer in the step (1), adjusting the pH value to 3.0-4.0, and heating to 80 ℃ for reaction for 2.0 h.
(3) The pH was adjusted to neutral, and the resulting suspension was centrifuged at 8000rpm for 3min, then washed with distilled water, and repeated twice.
(4) Drying the centrifuged substance in an oven at 135 ℃ for 3.0h, grinding the dried sample, and preparing the PF @ ADP flame retardant
(5) The drying and banburying steps of example 1 are repeated for the weighed LDPE and PF @ ADP to obtain the LDPE/PF @ ADP material.
Example 4
The diethyl aluminum hypophosphite coated flame-retardant low-density polyethylene consists of the following components in percentage by mass: LDPE (Low-Density polyethylene): 75%, PF @ ADP (PF: 30%, ADP: 70%): 25 percent. The preparation process comprises the following steps:
the procedure for making PF @ ADP flame retardant was the same as in example 2.
(2) And repeating the drying and banburying steps in the example 1 on the weighed LDPE and PF @ ADP to obtain the LDPE/PF @ ADP material.
Example 5
The diethyl aluminum hypophosphite coated flame-retardant low-density polyethylene consists of the following components in percentage by mass: LDPE (Low-Density polyethylene): 70%, PF @ ADP (PF: 30%, ADP: 70%): 30 percent. The preparation process comprises the following steps:
(1) 33.7g of phenol and 44mL of formaldehyde solution are respectively weighed and added into a three-neck flask to be heated to 60 ℃, the pH value is adjusted to 8.0-9.0, the mixture is uniformly reacted for 2.0h under the stirring of 1000rpm, the pH value is adjusted to be neutral to obtain brown viscous liquid, and 27.7g of brown viscous liquid is weighed and added into 50mL of distilled water to be cooled for standby.
(2) 42g of ADP is weighed and added into a three-necked bottle, 210mL of ethanol is added, dispersion is carried out for 20min, the PF prepolymer is added, the pH is adjusted to 3.0-4.0, and the mixture is heated to 80 ℃ for reaction for 2.0 h.
(3) The pH was adjusted to neutral, and the resulting suspension was centrifuged at 8000rpm for 3min, then washed with distilled water, and repeated twice.
(4) Drying the centrifuged substance in an oven at 135 ℃ for 3.0h, grinding the dried sample, and preparing the PF @ ADP flame retardant
(5) And repeating the drying and banburying steps in the example 1 on the weighed LDPE and PF @ ADP to obtain the LDPE/PF @ ADP material.
Comparative example 1
The flame-retardant low-density polyethylene comprises the following raw materials in percentage by mass: LDPE (Low-Density polyethylene): 80%, ADP: 20 percent. The preparation process comprises the following steps:
(1) placing the two materials in a drying oven at 60 ℃ for 12.0h, drying to remove water,
(2) the banburying temperature of the banbury mixer is set to 150 ℃, and after the temperature is stable, the feeding is started.
(3) Firstly, pouring the dried LDPE into an internal mixer from a feeding port, then adding the dried ADP, fully extruding and shearing the ADP under the action of a double rotor, and fully mixing the LDPE and the intumescent flame retardant.
(4) And after running for 15min, sequentially opening two movable plates of the internal mixer, and sampling to obtain the LDPE/ADP material.
The properties of the example materials are shown in Table 1
Table 1 examples 1-5 table of properties of flame retardant polymer materials
As can be seen from Table 1, the resin-coated diethyl aluminum hypophosphite can improve the flame retardant property of the material to a certain extent, and the flame retardant property has the tendency of increasing first and then decreasing along with the increase of the addition amount of PF, when PF @ ADP (30% of PF and 70% of ADP): when the addition amount reaches 30%, the Limiting Oxygen Index (LOI) reaches 31.3, and the vertical combustion grade can reach V-0. The results of tensile strength and elongation at break show that the coating of the phenolic resin can effectively improve the compatibility of ADP and LDPE, and has positive effect on the improvement of mechanical properties. Thermogravimetric (TG) results show that the coating of the phenolic resin can improve the residue mass ratio of the flame-retardant composite material at 700 ℃, and the thermal stability of the flame-retardant LDPE is improved. The smoke density test result shows that the addition of PF @ ADP can reduce the smoke release amount of the flame-retardant LDPE composite material.
Claims (6)
1. The resin-coated aluminum diethylphosphinate flame-retardant low-density polyethylene is characterized by comprising the following components in percentage by mass: low Density Polyethylene (LDPE): 70% -80%; flame retardant PF @ ADP: 20% -30%, wherein the content of phosphorus in ADP is 23% -24%, the content of aluminum in ADP is 6% -7%, and D95≤5μm。
2. The resin-coated aluminum diethylphosphinate flame retardant low density polyethylene of claim 1, wherein the flame retardant low density polyethylene comprises, in mass percent: low Density Polyethylene (LDPE): 70%, flame retardant PF @ ADP: 30%, Low Density Polyethylene (LDPE): 75%, flame retardant PF @ ADP: 25%, Low Density Polyethylene (LDPE): 80%, flame retardant PF @ ADP: 20 percent.
3. The preparation method of the resin-coated diethyl aluminum hypophosphite flame-retardant low-density polyethylene is characterized by comprising the following steps:
(1) preparing a flame retardant PF @ ADP by adopting an emulsion polymerization method;
(2) slowly pouring the dried LDPE into an internal mixer from a feeding port, then slowly adding the dried PF @ ADP, fully extruding the mixture under the action of a double rotor, and shearing to fully mix the LDPE and the PF @ ADP combustion agent;
(3) and (4) running for 10-15min, and sampling to obtain the resin-coated diethyl aluminum hypophosphite flame-retardant low-density polyethylene.
4. The preparation method of the resin-coated diethyl aluminum hypophosphite flame-retardant low density polyethylene as claimed in claim 3, wherein the preparation method of the flame retardant PF @ ADP in the step (1) comprises the following steps:
(a) mixing phenol and formaldehyde solution according to the mass ratio of 4:5, heating to 60 ℃, adjusting the pH to 8.0-9.0 by using alkaline solution, heating to 75 ℃ for reaction for 2.0h, adjusting the pH to 7.0 to obtain PF prepolymer, and adding distilled water for cooling for later use;
(b) dispersing ADP in an ethanol solution, adding the PF prepolymer, adjusting the pH value to 3.0-4.0, reacting at 80 ℃ for 2.0h, adjusting the pH value to be neutral, filtering, washing, putting the dehydrated PF @ ADP into a drying oven, drying at 135 ℃ for 3.0h to completely crosslink and solidify the PF, and crushing and grinding to obtain the PF @ ADP.
5. The method for preparing resin-coated diethyl aluminum hypophosphite flame-retardant low density polyethylene as claimed in claim 4, wherein the ADP content in the PF @ ADP prepared in step (b) is 60% -75%.
6. The method for preparing the resin-coated aluminum diethylphosphinate flame-retardant low-density polyethylene as claimed in claim 3, wherein the banburying temperature of the internal mixer in the step (2) is 145-155 ℃.
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| CN112898666A (en) * | 2021-01-27 | 2021-06-04 | 常州大学 | Modified semi-siloxane synergistic intumescent flame-retardant low-density polyethylene and preparation method thereof |
| CN113136052A (en) * | 2021-04-01 | 2021-07-20 | 浙江新化化工股份有限公司 | Flame-retardant composition, plastic, and preparation method and application thereof |
| CN114591557A (en) * | 2022-04-21 | 2022-06-07 | 北方民族大学 | Flame-retardant low-density polyethylene composite material and preparation method thereof |
| CN114591557B (en) * | 2022-04-21 | 2023-06-16 | 北方民族大学 | Flame-retardant low-density polyethylene composite material and preparation method thereof |
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