CN110862575A - Composite intumescent flame retardant, flame-retardant high impact polystyrene material and preparation method thereof - Google Patents
Composite intumescent flame retardant, flame-retardant high impact polystyrene material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a composite intumescent flame retardant, a flame-retardant high impact polystyrene material and a preparation method thereof. The composite intumescent flame retardant consists of 97.67-99.67 wt% of intumescent flame retardant and 0.33-2.33 wt% of nano layered double metal CoAl hydroxide; the flame-retardant high impact polystyrene material consists of high impact polystyrene and the composite intumescent flame retardant in a mass ratio of 70: 30. The flame-retardant high impact polystyrene material disclosed by the invention is simple in formula, halogen-free and environment-friendly, the flame retardant property and the mechanical property of the flame-retardant high impact polystyrene are obviously improved, the molten drop phenomenon is obviously improved, a continuous and compact carbon layer is generated after combustion, and the heat insulation and oxygen isolation effects are achieved.
Description
Technical Field
The invention belongs to the technical field of high impact polystyrene materials, and relates to a composite intumescent flame retardant, a flame-retardant high impact polystyrene material and a preparation method thereof.
Background
Polystyrene is one of five common plastics. The high impact polystyrene is an improved polystyrene product, has high impact resistance, good processability and dimensional stability, and is a polymer material with wide application. However, high impact polystyrene is easily combustible, LOI is only about 18%, and the melt dripping phenomenon is serious, so that the application of the high impact polystyrene in the fields of food packaging, electronic and electric appliances, military materials and the like is greatly limited. Therefore, the research on the flame-retardant high impact polystyrene material has very important significance.
The Intumescent Flame Retardant (IFR) mainly comprises three parts, namely an acid source (ammonium polyphosphate (APP) and the like), a carbon source (PER and the like) and an air source (melamine and the like). Is one of the most popular flame retardant systems currently applied to high impact polystyrene, has the advantages of no halogen, high efficiency, low toxicity and the like, and has wide application fields. However, compared with halogen flame retardants, IFR has a large smoke yield and a relatively low flame retardant efficiency, and often needs to be added in a large amount to meet the flame retardant requirement, which leads to a great reduction in the mechanical properties of the composite material.
Disclosure of Invention
The invention aims to provide a composite intumescent flame retardant, a flame-retardant high impact polystyrene material containing the composite intumescent flame retardant and a preparation method thereof. The invention utilizes CoAl-LDH to improve the compatibility of IFR and high impact polystyrene, the flame retardant system is halogen-free, efficient, green and environment-friendly, and the flame retardant property of the high impact polystyrene material is obviously improved.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a composite intumescent flame retardant comprises 97.67-99.67 wt% of Intumescent Flame Retardant (IFR) and 0.33-2.33 wt% of nano-layered double-metal CoAl hydroxide (CoAl-LDH).
Preferably, the intumescent flame retardant consists of ammonium polyphosphate and pentaerythritol in a mass ratio of 3: 1.
Preferably, the nano-layered double-metal CoAl hydroxide is synthesized by a hydrothermal reaction, and the method comprises the following steps:
respectively weighing Al (NO) according to a certain proportion3)3·9H2O、Co(NO3)2·6H2Adding O (wherein the molar ratio of Co to Al is 3:1) and urea into deionized water, fully stirring, carefully transferring the light red solution into a stainless steel reaction kettle, sealing, placing in a drying oven for hydrothermal treatment, cooling and standing the reaction product, centrifuging, and drying in vacuum to finally obtain the CoAl-LDH.
The invention provides a composite intumescent flame retardant high impact polystyrene material, which consists of High Impact Polystyrene (HIPS) and a composite intumescent flame retardant in a mass ratio of 70: 30.
The invention provides a preparation method of the composite intumescent flame-retardant high impact polystyrene material, which comprises the following steps:
mixing the high impact polystyrene and the composite intumescent flame retardant in proportion, extruding, granulating and injecting to obtain the flame-retardant high impact polystyrene material.
Compared with the prior art, the invention has the following advantages:
(1) the compatibility between the high impact polystyrene matrix and the flame retardant can be promoted by using the flaky nano CoAl-LDH.
(2) In the combustion process, combustion products of APP and LDH, such as pyrophosphoric acid, cobalt oxide and aluminum oxide, have high chemical activity, can catalyze high impact polystyrene and pentaerythritol to dehydrate into charcoal to form a cross-linked and compact charcoal layer, and play a role in blocking, so that the flame retardant property of the high impact polystyrene is improved;
(3) the flaky nano CoAl-LDH has a small-size effect, can be uniformly dispersed in an HIPS matrix, contains a large amount of hydroxyl groups between layers, and can form interaction force among molecular chains and between the matrix and the molecular chains so as to improve the mechanical property of the HIPS composite material.
(4) At the time of combustion, IFR is decomposed by heating to generate PO & and HPO & free radicals, and combustible free radicals H & and HO & in the surrounding environment are easy to capture; while CoAl-LDH is decomposed by heating to produce H2O、NH3、CO2The concentration of the combustible gas is diluted by non-combustible gas to generate phosphate, CoO and Al2O3Covering and isolating thermal oxygen to delay combustion, thereby improving the flame retardant property of HIPS;
(5) the composite intumescent flame retardant is a halogen-free green flame retardant, and the combustion process and the combustion products have little harm to the environment.
Drawings
FIG. 1 is a diagram showing the mechanical properties of the flame-retardant high impact polystyrene material of the present invention.
FIG. 2 is a graph of the flame retardant properties of the flame retardant high impact polystyrene material of the present invention.
Detailed Description
The present invention will be described in more detail with reference to the following examples and the accompanying drawings.
The invention takes layered double metal hydroxide (LDH) as a synergistic flame retardant, improves the flame retardant efficiency and simultaneously improves the mechanical property of the composite material. The layered double metal hydroxide (LDH) contains a large amount of hydroxyl and metal elements, can promote molecular chain crosslinking to realize flame retardance, and is a nano flame retardant with wide application.
Example 1
Preparation of CoAl-LDH:
separately weighing Al (NO) with an analytical balance3)3·9H2O 0.0938g、Co(NO3)2·6H2Adding 0.218g of O and 0.5255g of urea into 20mL of deionized water, fully stirring for 10min, carefully transferring the light red solution into a stainless steel reaction kettle, sealing, placing in a 100 ℃ oven for hydrothermal treatment for 24h, cooling and standing the reaction product, centrifuging, and drying in vacuum for 24h to finally obtain the CoAl-LDH.
Example 2
And sequentially weighing 29.9g of IFR and 0.1g of CoAl-LDH to form 30g of composite intumescent flame retardant, adding the composite intumescent flame retardant into 70g of HIPS particles, mechanically stirring to uniformly disperse the composite intumescent flame retardant, extruding the mixture through a micro extruder, granulating the mixture through a granulator, secondarily extruding the mixture through an extruder, and performing injection molding through an injection molding machine to obtain the test sample strip. Temperature of four sections of the extruder: 190 deg.C, 210 deg.C, 220 deg.C, 200 deg.C. And (3) injection molding temperature: 230 ℃ to 230 ℃. And is marked as HIPS-2. The tensile strength is 23.38MPa, the limiting oxygen index is 27 percent and the vertical burning grade is V-2 grade according to the test method of GB/T2406-1993.
Example 3
And sequentially weighing 29.7g of IFR and 0.3g of CoAl-LDH to form 30g of composite intumescent flame retardant, adding the composite intumescent flame retardant into 70g of HIPS particles, mechanically stirring to uniformly disperse the composite intumescent flame retardant, extruding the mixture through a micro extruder, granulating the mixture through a granulator, secondarily extruding the mixture through an extruder, and performing injection molding through an injection molding machine to obtain a test sample strip. Temperature of four sections of the extruder: 190 deg.C, 210 deg.C, 220 deg.C, 200 deg.C. And (3) injection molding temperature: 230 ℃ to 230 ℃. And is marked as HIPS-3. The tensile strength is 24.03MPa, the limiting oxygen index is 28.5 percent and the vertical burning grade is V-0 grade according to the test method of GB/T2406-1993 measurement.
Example 4
And sequentially weighing 29.5g of IFR and 0.5g of CoAl-LDH to form 30g of composite intumescent flame retardant, adding the composite intumescent flame retardant into 70g of HIPS particles, mechanically stirring to uniformly disperse the composite intumescent flame retardant, extruding the mixture through a micro extruder, granulating the mixture through a granulator, secondarily extruding the mixture through an extruder, and performing injection molding through an injection molding machine to obtain a test sample strip. Temperature of four sections of the extruder: 190 deg.C, 210 deg.C, 220 deg.C, 200 deg.C. And (3) injection molding temperature: 230 ℃ to 230 ℃. And is marked as HIPS-4. The tensile strength is 23.53MPa, the limiting oxygen index is 27.5 percent and the vertical burning grade is V-1 grade according to the test method of GB/T2406-1993.
Example 5
And sequentially weighing 29.3g of IFR and 0.7g of CoAl-LDH to form 30g of composite intumescent flame retardant, adding the composite intumescent flame retardant into 70g of HIPS particles, mechanically stirring to uniformly disperse the composite intumescent flame retardant, extruding the mixture through a micro extruder, granulating the mixture through a granulator, secondarily extruding the mixture through an extruder, and performing injection molding through an injection molding machine to obtain a test sample strip. Temperature of four sections of the extruder: 190 deg.C, 210 deg.C, 220 deg.C, 200 deg.C. And (3) injection molding temperature: 230 ℃ to 230 ℃. And is marked as HIPS-5. The tensile strength is 23.14MPa, the limiting oxygen index is 27 percent and the vertical burning grade is V-2 grade according to the test method of GB/T2406-1993.
Comparative example 1
Weighing 100g of pure HIPS particles, mechanically stirring to uniformly disperse the particles, extruding the particles by a micro extruder, granulating by a granulator, extruding for the second time by an extruder, and performing injection molding by an injection molding machine to obtain a test sample strip. Temperature of four sections of the extruder: 190 deg.C, 210 deg.C, 220 deg.C, 200 deg.C. And (3) injection molding temperature: 230 ℃ to 230 ℃. And is denoted as HIPS. The tensile strength is 36.22MPa, the limiting oxygen index is 18 percent and the vertical burning grade is NR grade according to the test method of GB/T2406-1993.
Comparative example 2
And sequentially weighing 30g of IFR as an intumescent flame retardant, adding the IFR into 70g of HIPS particles, mechanically stirring to uniformly disperse the IFR, extruding the IFR by using a miniature extruder, granulating by using a granulator, extruding for the second time by using an extruder, and performing injection molding by using an injection molding machine to obtain a test sample strip. Temperature of four sections of the extruder: 190 deg.C, 210 deg.C, 220 deg.C, 200 deg.C. And (3) injection molding temperature: 230 ℃ to 230 ℃. It is denoted as HIPS-1. The tensile strength is 20.45MPa, the limiting oxygen index is 26 percent and the vertical burning grade is V-2 grade according to the test method of GB/T2406-1993 measurement.
FIG. 1 is a line graph of tensile strength and impact strength for the flame retardant composites described in examples 2-5 and comparative examples 1-2. As can be seen from the figure, the tensile strength and the impact strength of the composite material both tend to increase and then decrease with the increase of the content of the CoAl-LDH. When only 30% of IFR is added, the tensile strength of the composite material is greatly reduced from 36.22MPa of pure HIPS to 20.45MPa, the total amount of the flame retardant is kept unchanged, and after 0.1 wt% of LDH is added, the tensile strength is obviously improved to 23.38 MPa. The composite tensile strength increased to a maximum of 24.03MPa when 0.3 wt% LDH was added, a 17.5% improvement over the IFR addition alone. The tensile properties begin to decrease as LDH content continues to increase. But all composites had higher tensile strength than if IFR was added alone. The impact strength is similar, and when 0.1 wt% LDH is added, the impact strength is preferably 3.04KJ/m2, which is 38% higher than that when IFR is added alone. And all composites were higher than if IFR was added alone. The reason is probably that LDH is used as a nano material, has small size effect, is uniformly dispersed, contains a large amount of hydroxyl groups between laminates, plays a role in interfacial compatibility in the material, has interaction force among molecular chains, and can promote the molecular chains and a small amount of cross-linking among the molecular chains, thereby improving the mechanical property of HIPS. When the LDH is added excessively, a large amount of agglomerates can be formed, stress concentration is caused, and the mechanical property of the composite material begins to be reduced.
FIG. 2 is a graph of the LOI test results for the flame retardant composites described in examples 2-5 and comparative examples 1-2, with pure HIPS having an LOI of only 18%, being flammable and failing the UL-94 test. After 30 wt% IFR was added, the HIPS-1 composite material reached 26%. The total amount of the flame retardant is kept unchanged, when 0.1 wt% of CoAl-LDH is added, the flame retardant property of the HIPS-2 composite material is obviously improved, the LOI reaches 27%, and the flame retardant can pass a V-2 test of UL-94. When 0.3 wt% of CoAl-LDH is added, the LOI of HIPS-3 reaches 28.5%, and reaches the V-0 grade of UL-94, and the flame retardant property reaches the optimum. When the LDH content exceeds 0.3 wt%, the LOI of the composite material begins to decrease, but the LOI of all the composite materials is higher than that of HIPS-1, and the LOI of UL-94 reaches V-2 level. As can be seen, the CoAl-LDH and IFR have a synergistic flame retardant effect, and the flame retardant property of HIPS can be improved.
Claims (5)
1. The composite intumescent flame retardant is characterized by comprising 97.67-99.67 wt% of intumescent flame retardant and 0.33-2.33 wt% of nano layered double metal CoAl hydroxide.
2. A composite intumescent flame retardant as claimed in claim 1, characterized in that the intumescent flame retardant consists of ammonium polyphosphate and pentaerythritol in a mass ratio of 3: 1.
3. A composite intumescent flame retardant as claimed in claim 1, characterized in that said nano-layered bi-metallic CoAl hydroxide is obtained by hydrothermal reaction, comprising the following steps: mixing Al (NO)3)3·9H2O、Co(NO3)2·6H2And (3) placing O and urea in deionized water, fully stirring, performing hydrothermal reaction, centrifuging, and drying in vacuum to obtain the nano layered double-metal CoAl hydroxide, wherein the molar ratio of Co to Al is 3: 1.
4. A composite intumescent flame retardant high impact polystyrene material, characterized by consisting of high impact polystyrene with a mass ratio of 70:30 and a composite intumescent flame retardant as claimed in any one of claims 1 to 3.
5. A preparation method of a composite intumescent flame-retardant high impact polystyrene material is characterized by comprising the following steps: mixing high impact polystyrene and the composite intumescent flame retardant as claimed in any one of claims 1 to 3 in proportion, extruding, granulating and injecting to obtain the flame-retardant high impact polystyrene material.
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| CN112480474A (en) * | 2020-11-25 | 2021-03-12 | 华东理工大学 | Smoke suppression intumescent flame retardant containing multiple anion intercalated Ca-based ternary hydrotalcite and preparation method thereof |
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