CN114044907B - Intumescent flame retardant functionalized POSS flame retardant and preparation method thereof - Google Patents
Intumescent flame retardant functionalized POSS flame retardant and preparation method thereof Download PDFInfo
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- CN114044907B CN114044907B CN202111533776.6A CN202111533776A CN114044907B CN 114044907 B CN114044907 B CN 114044907B CN 202111533776 A CN202111533776 A CN 202111533776A CN 114044907 B CN114044907 B CN 114044907B
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/045—Polysiloxanes containing less than 25 silicon atoms
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
Abstract
The invention discloses an intumescent flame-retardant functionalized POSS flame retardant and a preparation method thereof, wherein the flame retardant is prepared by functionalizing POSS and PAMAM partial terminal-NH 2 Reacting, and reacting the residual-NH of PAMAM by phosphorus oxychloride 2 And end-capping reaction. The prepared intumescent flame retardant functionalized POSS flame retardant not only has flame retardance, but also can reinforce a polymer matrix. The flame retardant elements of phosphorus and nitrogen are loaded on the surface of the POSS, so that the flame retardant elements of phosphorus, nitrogen and silicon can be uniformly dispersed in a polymer matrix in the preparation process of the flame retardant material, the problem of dispersity of the flame retardant in a high polymer material is solved, and the phosphorus and nitrogen elements are anchored on the surface of the POSS, so that the toxicity and the harm to the environment in use are greatly reduced; the mechanical property and the flame retardant property of the flame retardant material can be improved; the flame retardant disclosed by the invention is low in addition amount, good in flame retardant effect and wide in application range.
Description
Technical Field
The invention relates to a flame retardant, in particular to an intumescent flame retardant functionalized POSS flame retardant and a preparation method thereof.
Background
According to the flame retardant element classification, the flame retardant comprises a halogen flame retardant and a phosphorus flame retardant. The halogen flame retardant is one of the main flame retardants applied in plastics, has the advantages of high flame retardant efficiency, good weather resistance, high thermal stability and the like, and has small influence on the mechanical properties of materials. However, the halogen-based flame retardant releases corrosive gas and dense smoke during combustion, increasing the harm to the environment and human health, and in addition, releasing dense smoke and irritating gas also brings difficulty to escape of people in fire. The phosphorus flame retardant is mainly used for promoting the dehydration and carbonization of a high polymer material through oxyacid with high boiling point, and has the advantages of low toxicity, weak corrosivity, high thermal stability, low price and the like. In recent years, with the continuous and prominent global environmental problems, the silicon flame retardant with green and environmental protection performance is rapidly developed, and the Si-O-Si structure in the silicon flame retardant interacts with a high polymer material to form a compact barrier carbon layer in the combustion process, so that the silicon flame retardant has the functions of preventing dripping and inhibiting smoke. Polyhedral oligomeric silsesquioxane (POSS) is a cage-shaped nano-framework formed by silicon-oxygen bonds, eight corners of the cage-shaped nano-framework are active sites which can be further modified, and a unique cage-shaped structure has good solubility, structural stability and heat resistance and has great application prospect in the field of designing novel flame retardants. The POSS contributes to flame retardancy of polymers three points: (1) The cage structure of POSS can reduce the movement rate of polymer molecular chains and improve the thermal stability of the polymer; (2) When the polymer composite mixed with POSS is combusted, the decomposition of groups on eight corners of POSS consumes a part of heat, thereby effectively slowing down the degradation rate of the polymer; (3) The POSS can generate a layer of heat-insulating silicon carbon layer to cover the surface of the polymer after being combusted, so that the heat conduction is further slowed down. However, the desirable flame retardant effect of current POSS flame retardants often requires large amounts of addition, which greatly increases the cost of use of such flame retardants. Therefore, how to find a material which can cooperate with flame retardant and reduce the cost is one of the research focuses for developing novel POSS flame retardant.
Disclosure of Invention
The invention aims to provide an intumescent flame retardant functionalized POSS flame retardant.
One structural schematic diagram of the intumescent flame retardant functionalized POSS flame retardant is shown in figure 1, in the figure, a cage-shaped Si-O-Si structural part is POSS, a middle dendritic macromolecule is polyamide-amine (PAMAM), and an end-capping part is phosphorus oxychloride.
The intumescent flame retardant functionalized POSS flame retardant is prepared by functionalizing POSS and PAMAM terminal-NH 2 Partial reaction, and then phosphorus oxychloride is used to react with the residual-NH of PAMAM 2 And end-capping reaction.
The intumescent flame retardant functionalized POSS flame retardant is characterized in that the mass ratio of PAMAM, POSS and phosphorus oxychloride is 1:1 to 3:3 to 13.
Wherein the generation number of the dendritic macromolecule PAMAM is one generation, two generations or three generations.
The phosphoryl chloride is 2-oxo-2-chloro-5,5-dimethyl-1,3,2-Dioxaphosphorinane (DCCP).
The second technical problem to be solved by the invention is to provide a preparation method of the flame retardant.
The preparation method of the intumescent flame retardant functionalized POSS flame retardant comprises the following steps:
(1) POSS and PAMAM terminal-NH containing one benzyl chloride 2 And carrying out nucleophilic addition-elimination substitution reaction to obtain the PAMAM-POSS.
(2) PAMAM-POSS and 2-oxo-2-chlorine-5,5-dimethyl-1,3,2-Dioxaphosphorinane (DCCP) are subjected to end-capping reaction to prepare the intumescent flame retardant functionalized POSS flame retardant (PAMAM-POSS-DPPC).
The following describes each of the steps (1) to (2) in detail.
The reaction in step (1) of the present invention may be specifically carried out as follows: dissolving PAMAM in a solvent, adding a certain amount of acid-binding agent, then dropwise adding POSS suspension containing benzyl chloride, stirring and reacting for 8-36 hours at the temperature of 35-90 ℃, and separating to obtain PAMAM-POSS.
In the step (1), the ratio of the amount of the PAMAM to the POSS containing one benzyl chloride is 1:1 to 3.
In the step (1), the acid-binding agent is selected from one of the following: triethylamine and pyridine, wherein the amount ratio of the acid-binding agent to the POSS material containing one benzyl chloride is (1.0-1.5): 1.0.
in the step (1), the solvent is selected from one of the following solvents: alcohols, furans, amides; preferably one of the following: methanol, ethanol, tetrahydrofuran, and N, N' -dimethylformamide.
After the reaction in the step (1), PAMAM-POSS can be obtained by adopting conventional separation methods such as distillation and the like.
The reaction in step (2) of the present invention may be specifically carried out as follows: in a solvent, the PAMAM-POSS prepared in the step (1) and the DPPC react for 6 to 24 hours at the temperature of between 25 and 60 ℃ in the presence of an acid binding agent, and the PAMAM-POSS-DPPC is obtained by separation.
In the step (2), the ratio of the amount of the PAMAM-POSS to the amount of the DPPC feeding materials is 1:3 to 13.
In the step (2), the acid-binding agent is selected from one of the following: sodium bicarbonate and sodium carbonate, wherein the ratio of the acid-binding agent to the amount of the material fed into the DPPC is 1.0-1.2: 1.0.
in the step (2), the solvent is selected from one of the following solvents: halogenated hydrocarbons, ketones; preferably one of the following: chloroform, acetone.
After the reaction in the step (2), PAMAM-POSS-DPPC can be obtained by adopting conventional separation methods such as distillation and the like.
Compared with the prior art, the beneficial effects of the invention are embodied in the following aspects:
the prepared intumescent flame retardant functionalized POSS flame retardant not only has flame retardance, but also can reinforce a polymer matrix. Chemically modifying POSS by utilizing a grafting reaction and the like, loading flame-retardant elements of phosphorus and nitrogen on the surface of POSS, and uniformly dispersing the flame-retardant elements of phosphorus, nitrogen and silicon in a polymer matrix through the preparation of a flame-retardant material, so that the problem of the dispersibility of the flame retardant in a high-molecular material is solved, and the flame-retardant effect of the flame retardant on the polymer is improved; according to the intumescent flame retardant functionalized POSS flame retardant, phosphorus and nitrogen elements are anchored on the surface of POSS, so that the toxicity and the harm to the environment during use are greatly reduced; the expansion flame-retardant functionalized POSS flame retardant disclosed by the invention takes POSS as a nano reinforcing filler, has a reinforcing effect on a polymer matrix, and improves the mechanical property of a flame-retardant material; the flame retardant disclosed by the invention utilizes the synergistic flame retardant effect of the phosphorus-nitrogen compound and POSS, so that the flame retardant effect on a high polymer material is improved, the use amount of the flame retardant in the high polymer material is reduced, and the cost of the flame retardant material is reduced. The flame retardant disclosed by the invention is low in addition amount, good in flame retardant effect and wide in application range.
Drawings
FIG. 1 is a schematic diagram of an example of a PAMAM-POSS-DPPC structure;
FIG. 2 is a schematic diagram of the PAMAM-POSS-DPPC reaction based on the second generation PAMAM;
FIG. 3 is an infrared spectrum of PAMAM-POSS and PAMAM-POSS-DPPC;
FIG. 4 is an XPS energy spectrum of PAMAM, PAMAM-POSS, and PAMAM-POSS-DPPC;
FIG. 5 is an SEM image and elemental distribution of PAMAM-POSS-DPPC.
Detailed Description
The technical solution of the present invention is described below by using specific examples, but the scope of the present invention is not limited thereto:
example 1
Heating the second generation PAMAM to 50 ℃, fully dissolving 3.56g of the second generation PAMAM by using 20ml of methanol, adding the solution into a three-neck flask, and adding 2ml of triethylamine into the three-neck flask; then, 4.4g of POSS containing one benzyl chloride is dissolved by 25ml of methanol, the mixture is slowly dripped into a three-neck flask by using a constant pressure dropping funnel, the mixture is continuously stirred and reacted for 24 hours at the temperature of 50 ℃, and light yellow solid PAMAM-POSS is obtained after the reduced pressure distillation treatment, wherein the yield is 94.8%.
Example 2
The synthesis of PAMAM-POSS was performed as described in example 1. The ratio of the amounts of feed materials of PAMAM and POSS containing one benzyl chloride was 1:1, the generation number of PAMAM is one generation, the ratio of the acid-binding agent pyridine to the amount of POSS feed material containing one benzyl chloride is 1.5:1.0, the solvent is tetrahydrofuran, the reaction temperature is 90 ℃, the reaction time is 8 hours, and the product yield is 86.2%.
Example 3
The synthesis of PAMAM-POSS was performed as described in example 1. The ratio of the amounts of feed materials of PAMAM to POSS containing one benzyl chloride was 1:2.5, the generation number of PAMAM is two, the quantity ratio of acid-binding agent triethylamine to POSS material containing benzyl chloride is 1.2:1.0, the solvent is ethanol, the reaction temperature is 35 ℃, the reaction time is 36 hours, and the product yield is 96.7 percent.
Example 4
The synthesis of PAMAM-POSS was performed as described in example 1. The ratio of the amounts of feed materials of PAMAM to POSS containing one benzyl chloride was 1:3, the generation number of PAMAM is three, the ratio of the acid-binding agent pyridine to the amount of POSS material containing one benzyl chloride is 1.4:1.0, the solvent is N, N' -dimethylformamide, the reaction temperature is 45 ℃, the reaction time is 18 hours, and the product yield is 89.3 percent.
Example 5
The synthesis of PAMAM-POSS was performed as described in example 1. 4.6g of the PAMAM-POSS prepared above is dissolved in 50ml of trichloromethane, 1.2g of sodium bicarbonate is added, then a mixed solution of 25ml of trichloromethane dissolved with 1.55g of DPPC is slowly dripped into the PAMAM-POSS solution by using a constant pressure dropping funnel, the mixture is stirred and reacted for 24 hours at the temperature of 35 ℃, and the obtained product is subjected to reduced pressure distillation and purification to obtain yellow solid PAMAM-POSS-DPPC, wherein the yield is 93.5%.
Example 6
The procedure for synthesizing PAMAM-POSS was the same as in example 2, and the procedure for synthesizing PAMAM-POSS-DPPC was the same as in example 5. The ratio of the amount of the PAMAM-POSS to the amount of the DPPC feed material is 1:3, the ratio of the amount of the acid-binding agent sodium bicarbonate to the amount of the material fed into the DPPC is 1.2:1.0, the solvent is dichloromethane, the reaction temperature is 25 ℃, the reaction time is 24 hours, and the product yield is 92.4 percent.
Example 7
The procedure for synthesizing PAMAM-POSS was the same as in example 4, and the procedure for synthesizing PAMAM-POSS-DPPC was the same as in example 5. The ratio of the amount of the PAMAM-POSS to the amount of the DPPC feeding materials is 1:13, the ratio of the acid-binding agent sodium carbonate to the amount of the material of DPPC is 1.2:1.0, the solvent is acetone, the reaction temperature is 60 ℃, the reaction time is 6 hours, and the product yield is 77.4 percent.
Example 8: application of intumescent flame retardant functionalized POSS flame retardant
The preparation operation of the intumescent flame retardant functionalized POSS flame retardant PAMAM-POSS-DPPC is the same as that in example 5. 950g of thermoplastic dynamic vulcanized rubber (TPV) (manufacturer is Jinhu chemical, model is Innoprene TPV) and 50g of PAMAM-POSS-DPPC are put into a dispersion machine to be stirred for 20 minutes, the mixture is taken out and extruded and granulated by a screw extruder (the processing temperature range is 170-190 ℃) to obtain the TPV/PAMAM-POSS-DPPC composite material, and the results of measuring the mechanical property and the flame retardant property of the composite material are shown as follows.
TABLE 1
Note-TPV: neat thermoplastic dynamic vulcanizates; TPV/POSS composite material: POSS accounts for 5 percent of the mass of the thermoplastic dynamic vulcanized rubber; TPV/PAMAM-POSS-DPPC composite material: PAMAM-POSS-DPPC is prepared as in example 5, with a PAMAM-POSS-DPPC mass fraction of 5% of the thermoplastic dynamic vulcanizate.
As can be seen from Table 1, the tensile strength of the thermoplastic dynamic vulcanizate with 5% POSS addition (TPV/POSS) composite was increased by 35% compared to the pure thermoplastic dynamic vulcanizate and the tensile strength of the thermoplastic dynamic vulcanizate with 5% addition of intumescent flame retardant functionalized POSS flame retardant (TPV/PAMAM-POSS-DPPC) composite was increased by 60%, indicating that the intumescent flame retardant functionalized POSS has a significant reinforcing effect on the thermoplastic dynamic vulcanizate and the reinforcing effect is better than that of the unfunctionalized POSS. Furthermore, in terms of flame retardant performance improvement, the peak heat release rate of the thermoplastic dynamic vulcanizate (TPV/POSS) composite with 5% post added was reduced by 26% and the ignition time was extended by only 5 seconds, and the peak heat release rate of the thermoplastic dynamic vulcanizate (TPV/PAMAM-POSS-DPPC) composite with 5% intumescent flame retardant functionalized POSS flame retardant added was reduced by 38.6% and the ignition time was extended by 12 seconds, which greatly reduced the fire risk of the material, compared to the pure thermoplastic dynamic vulcanizate. The total heat release amount and the average mass loss rate of the TPV/PAMAM-POSS-DPPC composite material are lower than those of the TPV/POSS composite material. These show that the intumescent flame retardant functionalized POSS has a significant flame retardant effect on thermoplastic dynamic vulcanized rubber, and the flame retardant effect is superior to that of unfunctionalized POSS. In summary, the intumescent flame retardant functionalized POSS flame retardant has a flame retardant effect on matrix resin, can obviously improve the strength of the material, has a modification effect superior to that of unfunctionalized POSS, and well solves the technical problem that the mechanical property of the material is deteriorated when the flame retardancy of a high molecular material is improved by the conventional small molecular flame retardant.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (8)
1. The method for preparing the intumescent flame retardant functionalized POSS flame retardant is characterized by comprising the following steps:
(1) The POSS containing one benzyl chloride and part of PAMAM are terminated by-NH 2 Carrying out nucleophilic addition-elimination substitution reaction to obtain PAMAM-POSS;
(2) Performing end-capping reaction on PAMAM-POSS and 2-oxo-2-chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane DPPC to prepare an intumescent flame retardant functionalized POSS flame retardant PAMAM-POSS-DPPC; the mass ratio of the PAMAM, POSS and DPPC is 1:1~3:3 to 13.
2. The preparation method of the intumescent flame retardant functionalized POSS flame retardant of claim 1, wherein the step (1) is specifically: dissolving PAMAM in a solvent, adding a certain amount of an acid-binding agent, then dropwise adding a POSS suspension containing benzyl chloride, stirring and reacting at the temperature of 35-90 ℃ for 8-36 hours, and separating to obtain PAMAM-POSS; the ratio of the amount of the PAMAM to the POSS containing one benzyl chloride is 1:1~3, the ratio of the acid-binding agent to the POSS material containing one benzyl chloride is 1.0-1.5: 1.0.
3. the preparation method of the intumescent flame retardant functionalized POSS flame retardant of claim 2, characterized in that the acid scavenger is selected from triethylamine and pyridine.
4. The method for preparing the intumescent flame retardant functionalized POSS flame retardant as claimed in claim 2, wherein in the step (1), the solvent is selected from one of the following: alcohols, furans and amides.
5. The method for preparing the intumescent flame retardant functionalized POSS flame retardant of claim 1 wherein step (2) is specifically: in a solvent, the PAMAM-POSS prepared in the step (1) and DPPC react for 6 to 24 hours at the temperature of 25 to 60 ℃ in the presence of an acid binding agent, and PAMAM-POSS-DPPC is obtained through separation; the mass ratio of the PAMAM-POSS to the DPPC is 1:3 to 13, wherein the ratio of the acid binding agent to the amount of the material to be charged of the DPPC in the step is 1.0 to 1.2:1.0.
6. the method for preparing the intumescent flame retardant functionalized POSS flame retardant of claim 5, wherein in the step (2), the acid scavenger is selected from sodium bicarbonate and sodium carbonate.
7. The method of preparing an intumescent flame retardant functionalized POSS flame retardant of claim 5 wherein in step (2) said solvent is selected from the group consisting of: halogenated hydrocarbons, ketones.
8. An intumescent flame retardant functionalized POSS flame retardant made by the method of any of claims 1-7.
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| PCT/CN2022/138321 WO2023109737A1 (en) | 2021-12-15 | 2022-12-12 | Intumescent, flame-retardant and functionalized poss flame retardant and preparation method therefor |
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| CN115521543B (en) * | 2022-09-30 | 2024-03-22 | 天津金发新材料有限公司 | Flame-retardant PP material with low smoke toxicity, low heat release rate and high oxygen index, and preparation method and application thereof |
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