CN113416349B - Molybdate composition flame-retardant smoke suppressant and preparation method thereof - Google Patents
Molybdate composition flame-retardant smoke suppressant and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a molybdate composition flame-retardant smoke suppressant and a preparation method thereof, and the preparation method comprises the following specific steps: molybdenum trioxide MoO 3 Zinc oxide or copper oxide, talcum powder or montmorillonite are mixed physically and then placed in a rotary furnace, protective gas is introduced, the mixture is calcined for 2 to 4 hours at 400 to 600 ℃, and the mixture is sieved after being cooled to room temperature, so that the molybdate composition flame-retardant smoke suppressant is obtained. The PVC material prepared by the flame-retardant smoke inhibitor has good flame-retardant performance and excellent smoke control performance, and can reduce the generation of smoke in fire accidents.
Description
Technical Field
The invention relates to a flame-retardant smoke suppressant for a polymer material, in particular to a molybdate composition flame-retardant smoke suppressant and a preparation method thereof.
Background
Polyvinyl chloride (PVC) has many advantages of light weight, long life, high strength, wear resistance, chemical corrosion resistance, better flame retardancy and insulation, and is widely used in the fields of industry, agriculture, construction, electronic and electrical appliances, automobiles, power communication, and the like. The PVC material can generate a large amount of smoke, toxic and corrosive gases during combustion, so that the harm of fire to life and property of people is increased, and the problem of smoke suppression and toxicity suppression is a problem to be solved, so that the preparation of the smoke suppression flame retardant PVC material has important application significance.
In recent years, much research has been conducted on the smoke suppression and flame retardance of PVC, and currently, PVC smoke suppressants capable of forming a carbonized layer, such as molybdenum trioxide, mixtures of inorganic molybdenum (such as zinc molybdate or ammonium octamolybdate), zinc-magnesium complexes, transition metal oxides, and the like, are widely used in industry. Research shows that the most effective for inhibiting the PVC smoke is molybdenum compound, the content of which is 5 percent can reduce the smoke generation amount of the PVC material by more than 50 percent, but the molybdenum compound is often used in combination with other flame-retardant smoke inhibitors such as MoO because the molybdenum compound has high price and non-ideal flame retardant property 3 /ZnO，MoO 3 /Cu 2 O，MoO 3 /Fe 2 O 3 ， MoO 3 /SnO 2 Etc. these compounds not only reduce costs, but also utilize synergistic effects between componentsShould improve the smoke suppression and flame retardant effect. For example, Kemgard9llA developed by Shemin Williams, USA, is a small amount of zinc and molybdenum complex, and adding 4% to PVC can reduce l/3 smoke.
The patent No. CN 104448607A discloses a high-fire-resistance PVC-U pipe and a preparation method thereof, a compound of a zinc-molybdenum-silicon compound and nano aluminum hydroxide powder is used as a flame-retardant smoke suppressant, and 15% -30% of the flame-retardant smoke suppressant is filled to ensure that the flame propagation grade of the PVC-U pipe is less than or equal to 25 and the smoke generation grade is less than or equal to 50, so that the flame-retardant and smoke suppression performance of the PVC-U pipe is greatly improved. The disclosed technology shows that the zinc/molybdenum compound has synergistic smoke abatement effect when used in a composite way, but the flame retardant smoke suppressant is prepared by only physically mixing, and has the defects of non-uniform composite process and non-maximized molybdenum-based advantages.
In order to solve the problems, the invention discloses a molybdate composition flame-retardant smoke suppressant, which is characterized in that molybdate is coated on the surface of a synergistic flame retardant, and the structure maximizes the contact area of the molybdate and a material matrix, so that the molybdenum-based smoke suppression efficiency can be improved, the consumption of molybdenum elements can be reduced, and the problem that the conventional molybdenum-based flame-retardant smoke suppressant is high in price is solved. In addition, the core material with flame retardant synergy can also improve the flame retardant performance.
Disclosure of Invention
The invention aims to provide a flame-retardant smoke suppressant, which solves the problem of large smoke generation amount of the existing PVC material during combustion.
The molybdate composition flame-retardant smoke suppressant is characterized by comprising the following specific preparation steps:
(1) molybdenum trioxide (MoO) 3 Physically mixing the divalent metal oxide MO and the synergistic flame retardant to obtain a mixed material;
(2) and (3) placing the mixed materials in the steps into a rotary furnace, introducing nitrogen protective gas, heating to 400-600 ℃ at the speed of 10-20 ℃/min, preserving the heat for 2-4h, slowly cooling to room temperature at the speed of 5-10 ℃/min, and then sieving to obtain the product.
The molybdate composition flame-retardant smoke suppressant is formed by the following steps: first MoO 3 Chemically reacting with divalent metal oxides at elevated temperaturesMolybdate should be formed; secondly, the formed molybdate starts sublimation and vaporization when the temperature reaches above 400 ℃, vaporized molybdate molecules are diffused in a rotary furnace containing talcum powder or montmorillonite under the protection of nitrogen, and the gas molecules of the molybdate gradually deposit on the surface of the talcum powder or the montmorillonite along with the rotation and slow temperature reduction of the rotary furnace.
The divalent metal oxide MO is ZnO or CuO. ZnO and CuO at high temperature
All can be reacted with MoO 3 The reaction takes place, the specific reaction equation of which is as follows:
the talcum powder or montmorillonite of the synergistic flame retardant can form a barrier layer when heated, separates a flame-retardant main body from a heat source, reduces the permeation of oxygen and the dropping of a melt, is non-toxic, does not generate toxic and corrosive gases when heated, and can improve the flame retardant property of the material and reduce the smoke amount by matching with molybdate.
Mo in the molybdenum trioxide and the divalent metal oxide: the M molar ratio is 1: 0.5-1: 2, and the mass ratio of the oxide to the synergistic flame retardant is 1: 10-1: 20. When the molybdenum trioxide in the oxide is excessive, the residual molybdenum trioxide after complete reaction can be sublimated and vaporized at high temperature and also coated on the surface of the synergistic flame retardant along with slow temperature reduction; when other metal oxides are excessive, the zinc oxide and the copper oxide can not be vaporized at the calcining temperature due to higher melting points and saturated vapor pressures, but can be uniformly mixed with the molybdate composition along with the continuous dynamic heating of the rotary furnace, and the flame retardance and smoke suppression performance of the prepared compound can also be enhanced due to the synergistic effect of the transition metal oxides and the molybdenum compounds.
The median diameter D50 of the molybdenum trioxide and the divalent metal oxide is 1-3 μm.
The median diameter D50 of the synergistic flame retardant is 5-20 μm.
The rotating speed of the rotary furnace is 3 r/min-10 r/min.
The step (2) adopts calcining coating in a rotary furnace, the heating efficiency is high, the heating surface of the material along with the movement of the rotary furnace is large, and the material is uniformly mixed; and secondly, the rotary furnace has good air tightness, and ensures that the vaporized compound can have sufficient time to contact and coat with the synergistic flame retardant in the furnace. In addition, the slow cooling is beneficial to the uniform thickness of the coating shell layer, and the phenomenon of nonuniform surface coating of the synergistic flame retardant caused by the rapid cooling is avoided.
The flame-retardant smoke-suppression PVC product can be a PVC soft product or a PVC hard product, for example, the molybdate composition flame-retardant smoke-suppression agent is used for PVC wires and cables, and the flame-retardant smoke-suppression PVC product comprises the following specific components in parts by mass: 100 parts of PVC resin, 5-10 parts of molybdate composition flame-retardant smoke inhibitor, 10-30 parts of calcium carbonate, 10-20 parts of inorganic flame retardant, 0.5-3 parts of calcium-zinc stabilizer and 20-40 parts of plasticizer.
The inorganic flame retardant is magnesium hydroxide or aluminum hydroxide, and the plasticizer is dioctyl phthalate.
The technical advantages of the invention are as follows:
(1) the molybdate composition smoke suppressant prepared by the invention coats molybdate on the surface of the synergistic flame retardant, the contact area of molybdate and PVC material is increased due to the structure, and simultaneously, divalent metal and molybdenum compound are combined to have the synergistic smoke suppression effect, so that the smoke suppression efficiency can be improved, the consumption of molybdenum element is greatly reduced, and the cost for preparing the flame-retardant smoke suppressant PVC material is reduced.
(2) The solid-phase reaction adopts a dynamic sintering rotary furnace device with good tightness, generates no by-products and toxic gases, and is environment-friendly and pollution-free.
Drawings
FIG. 1 is an SEM image of a smoke suppressant of the molybdate composition prepared in example 1, FIG. 2 is a corresponding EDS elemental map, wherein FIG. 2(1) is a Mo elemental map, and FIG. 2(2) is a Zn elemental map.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. The exemplary embodiments and descriptions of the present invention are provided to explain the present invention, but the present invention is not limited thereto. The specific implementation mode is as follows:
example 1
(1) Uniformly mixing 29g of molybdenum trioxide, 16g of zinc oxide (Mo: Zn is 1:1) and 450g of talcum powder in a high-speed mixer at the speed of 800r/min for 5min, putting the mixed powder in a rotary furnace at the rotating speed of 3r/min, introducing nitrogen, heating to 500 ℃ at the speed of 10 ℃/min, calcining for 2h, slowly cooling to room temperature at the speed of 10 ℃/min, and sieving by a 120-mesh sieve to obtain the flame-retardant smoke inhibitor;
(2) respectively adding 10 parts of calcium carbonate, 15 parts of aluminum hydroxide, 1 part of calcium-zinc stabilizer, 25 parts of dioctyl phthalate and 10 parts of the flame-retardant smoke suppressant (with the Mo content of 0.5 part) into 100 parts of PVC resin, uniformly mixing in a high-speed dispersion machine, mixing for 5min at 150 ℃ on an open mill, hot pressing for 5min at 170 ℃ in a hydraulic press, and cold pressing for 2min in a flat vulcanizing machine to obtain the PVC material.
Example 2
(1) Uniformly mixing 26g of molybdenum trioxide, 10g of zinc oxide (Mo: Zn is 1.5:1) and 300g of talcum powder in a high-speed mixer at the speed of 800r/min for 4min, putting the mixed powder in a rotary furnace at the rotating speed of 5r/min, introducing nitrogen, heating to 550 ℃ at the speed of 10 ℃/min, calcining for 2h, slowly cooling to room temperature at the speed of 10 ℃/min, and sieving by a 120-mesh sieve to obtain the flame-retardant smoke inhibitor;
(2) respectively adding 10 parts of calcium carbonate, 15 parts of aluminum hydroxide, 1 part of calcium-zinc stabilizer, 25 parts of dioctyl phthalate and 10 parts of the flame-retardant smoke suppressant (with the Mo content of 0.6 part) into 100 parts of PVC resin, uniformly mixing in a high-speed dispersion machine, mixing for 5min at 150 ℃ on an open mill, hot-pressing for 5min at 170 ℃ in a hydraulic press, and cold-pressing for 2min in a flat vulcanizing machine to obtain the PVC material.
Example 3
(1) Uniformly mixing 28g of molybdenum trioxide, 24g of zinc oxide (Mo: Zn is 1: 1.5) and 820g of talcum powder in a high-speed mixer at 1000r/min for 2min, putting the mixed powder in a rotary furnace at the rotating speed of 10r/min, introducing nitrogen, heating to 400 ℃ at the speed of 15 ℃/min, calcining for 4h, slowly cooling to room temperature at the speed of 5 ℃/min, and sieving by a 120-mesh sieve to obtain the flame-retardant smoke inhibitor;
(2) respectively adding 10 parts of calcium carbonate, 10 parts of magnesium hydroxide, 5 parts of aluminum hydroxide, 1 part of calcium-zinc stabilizer, 25 parts of dioctyl phthalate and 10 parts of the flame-retardant smoke suppressant (the content of Mo is 0.1 part) into 100 parts of PVC resin, uniformly mixing in a high-speed dispersion machine, mixing for 5min at 150 ℃ on an open mill, hot-pressing for 5min at 170 ℃ in a hydraulic press, and cold-pressing for 2min in a flat-plate vulcanizing machine to obtain the PVC material.
Example 4
(1) Uniformly mixing 29g of molybdenum trioxide, 16g of copper oxide (Mo: Cu is 1:1) and 700g of talcum powder in a high-speed mixer at 500r/min for 5min, putting the mixed powder in a rotary furnace at the rotating speed of 6r/min, introducing helium, heating to 450 ℃ at the speed of 10 ℃/min, calcining for 4h, slowly cooling to room temperature at the speed of 10 ℃/min, and sieving by a 120-mesh sieve to obtain the flame-retardant smoke inhibitor;
(2) respectively adding 20 parts of calcium carbonate, 10 parts of magnesium hydroxide, 10 parts of aluminum hydroxide, 3 parts of calcium-zinc stabilizer, 20 parts of dioctyl phthalate and 10 parts of the flame-retardant smoke suppressant (the content of Mo is 0.24 part) into 100 parts of PVC resin, uniformly mixing in a high-speed dispersion machine, mixing for 5min at 150 ℃ on an open mill, hot-pressing for 5min at 170 ℃ in a hydraulic press, and cold-pressing for 2min in a flat-plate vulcanizing machine to obtain the PVC material.
Example 5
(1) Uniformly mixing 40g of molybdenum trioxide, 11g of copper oxide (Mo: Cu is 2:1) and 510g of talcum powder in a high-speed mixer at 1000r/min for 2.5min, putting the mixed powder in a rotary furnace at the rotating speed of 5r/min, introducing nitrogen, heating to 600 ℃ at the speed of 15 ℃/min, calcining for 2h, slowly cooling to room temperature at the speed of 5 ℃/min, and sieving by a 120-mesh sieve to obtain the flame-retardant smoke inhibitor;
(2) respectively adding 10 parts of calcium carbonate, 20 parts of aluminum hydroxide, 2 parts of calcium-zinc stabilizer, 40 parts of dioctyl phthalate and 5 parts of the flame-retardant smoke inhibitor (the content of Mo is 0.33 part) into 100 parts of PVC resin, uniformly mixing in a high-speed dispersion machine, mixing for 5min at 150 ℃ on an open mill, hot-pressing for 5min at 170 ℃ in a hydraulic press, and cold-pressing for 2min in a flat vulcanizing machine to obtain the PVC material.
Example 6
(1) Uniformly mixing 20g of molybdenum trioxide, 22g of copper oxide (Mo: Cu is 1:2) and 800g of talcum powder in a high-speed mixer at the speed of 800r/min for 3min, putting the mixed powder in a rotary furnace at the rotating speed of 5r/min, introducing nitrogen, heating to 500 ℃ at the speed of 20 ℃/min, calcining for 4h, slowly cooling to room temperature at the speed of 5 ℃/min, and sieving by a 120-mesh sieve to obtain the flame-retardant smoke inhibitor;
(2) respectively adding 30 parts of calcium carbonate, 5 parts of magnesium hydroxide, 5 parts of aluminum hydroxide, 1.5 parts of calcium zinc stabilizer, 40 parts of dioctyl phthalate and 10 parts of the flame-retardant smoke suppressant (with the Mo content of 0.17 part) into 100 parts of PVC resin, uniformly mixing in a high-speed dispersion machine, mixing for 5min at 150 ℃ on an open mill, hot-pressing for 5min at 170 ℃ in a hydraulic press, and cold-pressing for 2min in a flat-plate vulcanizing machine to obtain the PVC material.
Comparative example 1
The flame retardant smoke suppressant of comparative example 1 was prepared by physical mixing, the specific preparation procedure was as follows:
(1) uniformly mixing 29g of molybdenum trioxide, 16g of zinc oxide (Mo: Zn: 1) and 450g of talcum powder in a high-speed mixer at a speed of 800r/min for 5min to obtain the flame-retardant smoke suppressant;
(2) the 10 parts of the flame-retardant smoke-suppressing agent (Mo content of 0.5 part) in example 1 was replaced with 10 parts of the flame-retardant smoke-suppressing agent (Mo content of 0.5 part) prepared by (1) comparative example 1, and the other raw materials and PVC preparation process were the same as in example 1.
Comparative example 2
The flame retardant smoke suppressant of comparative example 2 was prepared by using molybdenum trioxide, replacing 10 parts of the flame retardant smoke suppressant of example 1 (Mo content: 0.5 part) with 2 parts of molybdenum trioxide (Mo content: 1.3 part), and preparing the other raw materials and PVC in the same manner as in example 1.
Comparative example 3
The flame retardant smoke suppressant of comparative example 1 was prepared by physical mixing, the specific preparation procedure was as follows:
(1) uniformly mixing 29g of molybdenum trioxide, 16g of copper oxide (Mo: Cu is 1:1) and 700g of talcum powder in a high-speed mixer at a speed of 500r/min for 5min to obtain the flame-retardant smoke suppressant;
(2) the 10 parts of the flame-retardant smoke-suppressing agent (Mo content of 0.3 part) in example 4 was replaced with 10 parts of the flame-retardant smoke-suppressing agent (Mo content of 0.3 part) prepared by comparative example 2(1), and the other raw materials and PVC preparation process were the same as in example 4.
Comparative example 4
The flame retardant smoke suppressant of comparative example 4 was molybdenum trioxide, 10 parts of the flame retardant smoke suppressant of example 4 (Mo content: 0.3 part) was replaced with 1.5 parts of molybdenum trioxide (Mo content: 1 part), and the other raw materials and PVC preparation process were the same as in example 4.
Performance test of the PVC materials prepared in examples 1-6 and comparative examples 1-4
Method and standard for performance detection
The density grade was tested in a smoke density test chamber according to GB/T8627-1999; the vertical combustion is tested according to GB/T2408-2008; the oxygen index is tested according to GB/T2406; the tensile strength and the elongation at break of the structural adhesive are tested according to the method GB/T1040.1, and the average value is taken for 3 times.
Table 1: performance detection result of PVC material
Note: the blank case refers to that the flame retardant smoke suppressant product is not added in the PVC material formula.
As can be seen from the data results in table 1:
(1) the molybdate composition prepared by the invention is an effective flame-retardant smoke suppressant for PVC materials. Compared with the comparative example 1 of the molybdenum-zinc flame-retardant smoke suppressant prepared by physical mixing, the embodiment 1 of selecting the molybdenum-zinc composition flame-retardant smoke suppressant prepared by selecting a rotary furnace and a process thereof has the advantages that the smoke density grade of the application of the embodiment 1 of selecting the flame-retardant smoke suppressant disclosed by the invention in PVC is reduced from 70 to 56 under the condition of the same part, the smoke density grade of the molybdenum-copper composition flame-retardant smoke suppressant of the embodiment 4 and the molybdenum-copper composition of the comparative example 3 are also the same, and the smoke density grade of the application of the method disclosed by the invention in PVC is reduced from 72 to 61, so that the molybdate composition flame-retardant smoke suppressant disclosed by the invention is superior to the conventional compound smoke suppressant prepared by simple physical mixing;
(2) the molybdate composition prepared by the invention effectively improves the utilization rate of molybdenum. From example 1 and comparative example 2, it is observed that the smoke density grade of the PVC material prepared in comparative example 2 with the molybdenum base content of 1.3 parts can reach example 1 with the molybdenum base content of 0.5 parts only marginally; similarly, in example 4, compared with comparative example 4, the smoke density grade of the PVC material prepared in comparative example 4 with the molybdenum base content of 1 part can reach example 4 with the molybdenum base content of 0.3 part; the flame-retardant smoke suppressant effectively improves the utilization rate of molybdenum, and can prepare the flame-retardant smoke suppressant with excellent smoke suppression performance by using a small amount of molybdenum;
(3) the zinc molybdate compositions in the embodiments 1 to 3 can be observed to have higher content of added zinc molybdate, and lower smoke density grade of the prepared PVC material; the copper molybdate compositions of examples 4 to 6 also have the same effect in PVC materials, and the smoke density level decreases as the copper molybdate content increases.
Claims (5)
1. The molybdate composition flame-retardant smoke suppressant is characterized by comprising the following specific preparation steps:
(1) molybdenum trioxide MoO 3 Physically mixing the divalent metal oxide MO and the synergistic flame retardant to obtain a mixed material;
(2) placing the mixed materials in the steps in a rotary furnace, introducing nitrogen for protection, heating to 400-600 ℃ at the speed of 10-20 ℃/min, preserving the heat for 2-4h, slowly cooling to room temperature at the speed of 5-10 ℃/min, and then sieving to obtain the molybdate composition flame-retardant smoke suppressant;
wherein the divalent metal oxide MO is ZnO or CuO; the synergistic flame retardant is talcum powder or montmorillonite.
2. The molybdate composition flame-retardant smoke suppressant according to claim 1, wherein the molar ratio of Mo to M in the molybdenum trioxide and the divalent metal oxide is 1: 0.5-1: 2, and the mass ratio of the oxide to the synergistic flame retardant is 1: 10-1: 20.
3. The molybdate composition flame-retardant smoke suppressant according to claim 1, wherein the median diameter D50 of said molybdenum trioxide and divalent metal oxide is 1 μm to 3 μm.
4. The molybdate composition flame-retardant smoke suppressant according to claim 1, wherein the median diameter D50 of the synergistic flame retardant is 5-20 μm.
5. The molybdate composition flame retardant and smoke suppressant composition of claim 1, for use in the preparation of flame retardant and smoke suppressant PVC products.
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| CN107141576A (en) * | 2017-05-18 | 2017-09-08 | 三斯达（江苏）环保科技有限公司 | The preparation of halogen-free flame retardants and its application in EVA expanded materials |
| CN107652596A (en) * | 2017-10-27 | 2018-02-02 | 安徽嘉中金属材料有限公司 | A kind of fire-resistant cable material of high temperature resistant cracking resistance and preparation method thereof |
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