CN114933770A - Coated polytetrafluoroethylene anti-dripping agent and preparation method thereof - Google Patents
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- C08J3/205—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase
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- C08K5/49—Phosphorus-containing compounds
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- C08K5/52—Phosphorus bound to oxygen only
- C08K5/521—Esters of phosphoric acids, e.g. of H3PO4
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- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
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- C08K5/527—Cyclic esters
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- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
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Abstract
The invention discloses a coated polytetrafluoroethylene anti-dripping agent and a preparation method thereof, wherein the coated polytetrafluoroethylene anti-dripping agent is prepared by coating an organic ester emulsifier on the surface of polytetrafluoroethylene; the organic ester emulsifier comprises one or a mixture of fatty acid ester emulsifier and phosphate ester emulsifier; the fatty acid ester emulsifier is mono-diglycerol fatty acid ester; the phosphate ester emulsifier is any one or mixture of pentaerythritol phosphate, phosphoglyceride, triethyl phosphate and triphenyl phosphate. The coated anti-dripping agent provided by the invention has better flame-retardant anti-dripping performance, simple preparation process and low production cost, can effectively reduce the outlet expansion during resin processing, and ensures the transparency of the material.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a coated polytetrafluoroethylene anti-dripping agent and a preparation method thereof.
Background
Plastic products are liable to melt and drip during combustion, and thus the fire tends to spread, and in order to improve the flame retardancy of plastics, it is necessary to add an anti-dripping agent to the plastics. The anti-dripping agent is prepared by specially modifying polytetrafluoroethylene powder with different molecular weights, and is added into a formula of an engineering plastic flame retardant to increase the melt strength and the flexural modulus, so that the flame retardance of a product is improved, and dripping caused by combustion is prevented. The anti-dripping agent has excellent dispersibility and easy operability, is one of important formulas of flame-retardant engineering plastics, and takes the anti-dripping effect as the large molecular weight polytetrafluoroethylene is fiberized under the shearing force of a screw to form a net structure.
The polytetrafluoroethylene used as an anti-dripping agent has three main types: emulsion type, pure powder type, and coating type. The emulsion type anti-dripping agent is an emulsion formed by dispersing polytetrafluoroethylene in water through the action of a dispersing agent to form suspension. Since the resin such as polycarbonate PC is easily hydrolyzed by containing about 40% of water therein, it is difficult to use the resin, and the demand for plastic processing equipment and processing technology is high. The pure powder type anti-dripping agent is pure polytetrafluoroethylene powder. The pure powder type anti-dripping agent has the problem of poor dispersion due to poor compatibility of polytetrafluoroethylene and other plastics. The surface of the pure polytetrafluoroethylene powder needs to be sintered, so that the fluidity and the dispersibility of the product are improved, the product can be well dispersed during premixing, and the product is not easy to fibrillate in advance. The coated anti-dripping agent is prepared by coating a layer of styrene-acrylonitrile copolymer SAN or polymethyl methacrylate PMMA, polystyrene PS and the like on the outer layer of polytetrafluoroethylene PTFE, so that the anti-dripping agent can be well dispersed in polycarbonate PC, acrylonitrile-butadiene-styrene copolymer ABS, polystyrene PS and the like. The coated anti-dripping agent has low requirements on production equipment, and the preparation process is simple and is widely applied.
The patent with the application number of 201910900749.4 discloses a preparation method of a polytetrafluoroethylene anti-dripping agent, which is characterized by comprising the following steps: the method comprises the following steps: s1, adding 0.1-5 parts of anionic emulsifier, 0.1-5 parts of nonionic emulsifier and 30-70 parts of water into a reaction kettle according to parts by weight, uniformly stirring, heating to 30-80 ℃, then adding 5-95 parts of polycarbonate resin powder, and uniformly stirring to obtain a polycarbonate mixed solution; s2, adding 5-95 parts of polytetrafluoroethylene dispersion liquid into the polycarbonate mixed liquid obtained in the step (S1), and blending for 60-180min at the temperature of 30-80 ℃ to obtain a mixed emulsion; s3, adding the mixed emulsion obtained in the step S2 into a coagulant solution, and then sequentially carrying out centrifugation, separation, washing and drying to obtain the polytetrafluoroethylene anti-dripping agent. Although this anti-dripping agent can be applied well to polycarbonate systems, it is difficult to use it in nylon PA and polypropylene PP.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: aiming at the defects in the prior art, the invention provides the coated polytetrafluoroethylene anti-dripping agent which can effectively solve the problems of dispersion, hydrolysis and compatibility of the conventional coated polytetrafluoroethylene anti-dripping agent in various plastic applications.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a coated polytetrafluoroethylene anti-dripping agent is prepared by coating organic ester emulsifier on the surface of polytetrafluoroethylene; the organic ester emulsifier comprises one or a mixture of fatty acid ester emulsifier and phosphate ester emulsifier; the fatty acid ester emulsifier is mono-diglycerol fatty acid ester; the phosphate ester emulsifier is any one or mixture of pentaerythritol phosphate, phosphoglyceride, triethyl phosphate and triphenyl phosphate.
Preferably, the fatty acid in the mono-or diglycerol fatty acid ester includes one or more of oleic acid, linoleic acid, linolenic acid, palmitic acid, behenic acid, stearic acid, and lauric acid.
In order to better solve the technical scheme, the invention also discloses the following technical scheme:
a preparation method of a coated polytetrafluoroethylene anti-dripping agent comprises the following steps:
(1) adding an organic ester emulsifier into the polytetrafluoroethylene emulsion, and stirring and emulsifying to obtain an organic ester/polytetrafluoroethylene emulsion;
(2) and (3) performing emulsion breaking treatment on the prepared organic ester/polytetrafluoroethylene emulsion, collecting the precipitate, drying the obtained precipitate, and then crushing to prepare the coated polytetrafluoroethylene anti-dripping agent.
Preferably, in the step (1), the solid content of the polytetrafluoroethylene emulsion is 58-62%, the average molecular weight of the polytetrafluoroethylene is 100-1000 ten thousand, the particle size of the emulsion is 0.01-0.30 μm, and the viscosity is 10-100mPa · S.
Preferably, in the step (1), the addition amount of the organic ester emulsifier is 10-100% of the mass of the polytetrafluoroethylene emulsion.
Preferably, in the step (1), the temperature of the emulsification treatment is 25-90 ℃ and the time is 0.5-8 h.
Preferably, in the step (2), the demulsification treatment is one of heating demulsification, centrifugal demulsification, salting-out demulsification, electric demulsification and ultrasonic demulsification, and further the demulsification treatment is centrifugal demulsification; when in centrifugal demulsification, the adopted centrifugal rotating speed is 4500-5500 rpm, and the centrifugal time is 20-30 min.
Preferably, in the step (2), the drying method is one of vacuum drying, freeze drying, forced air drying, spray drying, infrared drying and microwave drying; further, the drying mode is vacuum drying, the temperature during vacuum drying is 70-80 ℃, the vacuum degree is 0.095MPa, and the drying time is 3-5 h.
Preferably, in the step (2), the crushing treatment is one of grinding, ball milling, jet milling and high-speed stirring and pulverizing; furthermore, the crushing treatment mode is air flow crushing, the crushing pressure during the air flow crushing is 0.4-0.8MPa, air is used as a working medium, the feeding pressure is 0.5-1.0MPa, and the feeding amount is 40-100 kg/h.
In the above aspect, in the step (2), the coated polytetrafluoroethylene anti-dripping agent preferably has an average particle size of 100 μm to 4 mm.
Due to the adoption of the technical scheme, the invention has the beneficial effects that:
(1) the coated polytetrafluoroethylene provided by the invention is prepared by coating the polytetrafluoroethylene with the organic ester emulsifier, the polytetrafluoroethylene can be uniformly dispersed in various resin materials without surface sintering treatment after being coated with the organic ester emulsifier, the dispersion problem of a pure powder type anti-dripping agent is solved, and the expansion condition of an outlet during processing after plastic is added is effectively improved.
(2) The invention firstly mixes the organic ester emulsifier and the polytetrafluoroethylene emulsion, carries out emulsification treatment at a certain temperature, and then carries out emulsion breaking, collection and precipitation, drying and crushing in sequence to prepare the polytetrafluoroethylene emulsion, wherein the polytetrafluoroethylene has strong hydrophobicity, organic phase oil drops in a water phase can be formed in the emulsification process, the organic ester emulsifier has moderate hydrophilicity and lipophilicity and can be enriched on the outer layer of the oil drops, and the organic ester emulsifier is uniformly coated on the outer layer of the polytetrafluoroethylene after emulsion breaking and drying.
(3) After the polytetrafluoroethylene is coated by the organic ester emulsifier, emulsion is broken, dried and crushed, the water content of the coated anti-dripping agent is extremely low, and the water resistance of the organic ester emulsifier is added, so that the problem of application of the emulsion anti-dripping agent to PC resin is solved.
(4) The compatibility of the existing styrene-acrylonitrile copolymer coated (SAN coated), polymethyl methacrylate coated (PMMA coated) and polystyrene coated (PS coated) anti-dripping agents with nylon PA and polypropylene PP materials is poor, and the organic ester coated polytetrafluoroethylene anti-dripping agents are difficult to use in the resin, so that the compatibility of the organic ester coated polytetrafluoroethylene anti-dripping agents with PA and PP is greatly improved, the transparency of plastic products is not influenced in use, and when the addition amount of the organic ester coated polytetrafluoroethylene anti-dripping agents in the resin materials such as PC, PP, PA, PE and ABS is 0.1% -1.0%, the effect of preventing dripping can be achieved in combustion.
Detailed Description
The invention is further illustrated by the following examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
Unless otherwise specified, the raw materials in the examples of the present application were all purchased commercially.
Wherein, glyceryl oleate, glyceryl linolenate, glyceryl palmitate, glyceryl stearate, glyceryl laurate, pentaerythritol phosphate, glyceryl phosphate, triethyl phosphate, and triphenyl phosphate are available from Aladdin reagent (Shanghai) Inc.
Polytetrafluoroethylene emulsions were purchased from Zhejiang Kyoho Ltd.
Unless otherwise specified, the reactions in the examples were carried out at room temperature.
The analysis method in the examples of the present application is as follows:
carrying out a vertical combustion anti-dripping performance test by using a UL94 horizontal vertical combustor;
the transmittance was measured using a transmittance haze meter.
Example 1
S1: weighing 500g of polytetrafluoroethylene emulsion with the solid content of 60%, pouring the polytetrafluoroethylene emulsion into a 2L glass flask with a stirrer for stirring, dropwise adding 200g of the weighed glycerol oleate into the glass flask, heating to 60 ℃ after dropwise adding, keeping the temperature for heat preservation, continuously stirring for 6 hours, cooling to room temperature, and stopping stirring to obtain the organic ester/polytetrafluoroethylene emulsion;
s2: placing the organic ester/polytetrafluoroethylene emulsion in a centrifuge, centrifuging for 30 minutes at the rotating speed of 5000 r/min, standing and taking out after the centrifugation is finished, pouring supernatant liquid, and collecting lower-layer precipitate;
s3: putting the collected centrifugal precipitate into a vacuum drying oven, drying for 4 hours at 75 ℃ under the vacuum degree of 0.095MPa, cooling to room temperature, and taking out;
s4: and (3) putting the dried material in the S4 into an airflow crusher for airflow crushing, controlling the crushing pressure to be 0.5MPa, taking air as a working medium, feeding the working medium under the pressure of 0.6MPa and feeding the working medium at the feeding quantity of 50kg/h, and then sieving to obtain the coated polytetrafluoroethylene anti-dripping agent with the average particle size of 600 microns, which is recorded as C1.
Example 2
In this example, a coated polytetrafluoroethylene anti-dripping agent, designated as C2, was obtained using glycerol linolenate in place of the glycerol oleate used in example 1 under the same conditions as in example 1.
Example 3
In this example, a coated polytetrafluoroethylene anti-dripping agent, designated as C3, was obtained under the same conditions as in example 1 except that glyceryl palmitate was used in place of glyceryl oleate in example 1.
Example 4
In this example, a coated polytetrafluoroethylene anti-dripping agent, designated as C4, was obtained using glyceryl stearate in place of glyceryl oleate in example 1 under the same conditions as in example 1.
Example 5
In this example, a coated polytetrafluoroethylene anti-dripping agent, designated as C5, was obtained under the same conditions as in example 1 except that glycerol laurate was used in place of glycerol oleate in example 1.
Example 6
In this example, pentaerythritol phosphate was used instead of the oleic acid glyceride in example 1, and the coated polytetrafluoroethylene anti-dripping agent, designated as C6, was obtained under the same conditions as in example 1.
Example 7
In this example, a coated polytetrafluoroethylene anti-dripping agent, designated as C7, was obtained under the same conditions as in example 1 except that phosphoglyceride was used instead of the glyceryl oleate used in example 1.
Example 8
In this example, triethyl phosphate was used in place of the glyceryl oleate used in example 1 under the same conditions as in example 1, to obtain an encapsulated polytetrafluoroethylene anti-dripping agent designated as C8.
Example 9
In this example, triphenyl phosphate was used instead of the glyceryl oleate used in example 1, and the other conditions were the same as in example 1, to obtain a coated polytetrafluoroethylene anti-dripping agent, which was designated as C9.
Application examples
The coated polytetrafluoroethylene anti-dripping agents obtained in examples 1 to 9 were blended with PC polycarbonate, PA nylon, and PP polypropylene in an amount of 0.5%, respectively, and then subjected to strand-forming and pellet-forming to obtain resin particles to which the anti-dripping agent was added, and the expansion at the outlet of the extruder was observed. And (3) carrying out sample bar injection molding on the resin particles added with the anti-dripping agent by using an injection molding machine, and carrying out appearance evaluation, anti-dripping performance test and transparency test on the sample bars.
Comparative example 1
The commercial pure powder polytetrafluoroethylene anti-dripping agent is marked as D1, and the pure powder polytetrafluoroethylene anti-dripping agent is respectively blended, pulled into strips and granulated with PC polycarbonate, PA nylon and PP polypropylene according to the addition of 0.3 percent by using a double-screw extruder to obtain resin particles added with the anti-dripping agent, and the expansion condition of an outlet of the extruder is observed. And (3) carrying out sample bar injection molding on the resin particles added with the anti-dripping agent by using an injection molding machine, and carrying out appearance evaluation, anti-dripping performance test and transparency test on the sample bars.
Comparative example 2
A commercially available emulsion type polytetrafluoroethylene anti-dripping agent is characterized in that the mass fraction of polytetrafluoroethylene is 50%, and is recorded as D2, a double-screw extruder is used for blending, bracing and granulating the emulsion type polytetrafluoroethylene anti-dripping agent with PC polycarbonate, PA nylon and PP polypropylene respectively according to the addition amount of 0.6%, so as to obtain resin particles added with the anti-dripping agent, and the expansion condition of an outlet of the extruder is observed. And (3) carrying out sample bar injection molding on the resin particles added with the anti-dripping agent by using an injection molding machine, and carrying out appearance evaluation, anti-dripping performance test and transparency test on the sample bars.
Comparative example 3
A commercially available SAN-coated polytetrafluoroethylene anti-dripping agent is characterized in that the mass fraction of polytetrafluoroethylene is 50%, and is recorded as D3, a double-screw extruder is used for blending, bracing and granulating the SAN-coated polytetrafluoroethylene anti-dripping agent with PC polycarbonate, PA nylon and PP polypropylene respectively according to the addition amount of 0.6%, so as to obtain resin particles added with the anti-dripping agent, and the expansion condition of an outlet of the extruder is observed. And (3) carrying out sample bar injection molding on the resin particles added with the anti-dripping agent by using an injection molding machine, and carrying out appearance evaluation, anti-dripping performance test and transparency test on the sample bars.
The processability and appearance test results are shown in Table 1, the anti-dripping property is shown in Table 2, and the transparency test result is shown in Table 3.
TABLE 1
As can be seen from the test results in Table 1, the coated polytetrafluoroethylene resin prepared by the invention added to PC, PA and PP resins has only slight outlet expansion during twin-screw extrusion processing, while the PC resin added with pure powder polytetrafluoroethylene anti-dripping agent and the PA and PP resin added with SAN coated anti-dripping agent can cause more serious outlet expansion. In the appearance of the processed particles and the appearance of the sample strips, the emulsion type polytetrafluoroethylene anti-dripping agent is added to cause serious bubble and air hole phenomena in the resin, because water contained in the emulsion type anti-dripping agent causes the decomposition of the resin during processing, and the addition of the pure powder type polytetrafluoroethylene anti-dripping agent or the SAN coated polytetrafluoroethylene anti-dripping agent causes internal filamentous flocculent foreign matters to show that the two anti-dripping agents are not well dispersed in the resin.
TABLE 2
As can be seen from the test results in Table 2, under the condition of adding the same amount of pure polytetrafluoroethylene, the pure powder type anti-dripping agent and the coated polytetrafluoroethylene anti-dripping agent provided by the invention can exert anti-dripping effects in PC, PA and PP, while the emulsion type anti-dripping agent has anti-dripping failure due to hydrolysis of PC resin, and the result shows that the emulsion type anti-dripping agent is not suitable for use in PC resin, the SAN coated anti-dripping agent has anti-dripping failure in PA and PP resin, and the result shows that the SAN coated anti-dripping agent is not suitable for use in PA and PP resin.
TABLE 3
As can be seen from the test results in Table 3, the light transmittance of the PC resin modified by the coated polytetrafluoroethylene anti-dripping agent provided by the invention is higher than 90%, and the PC resin can be well dispersed in PC without affecting the transparency of PC. While pure powder polytetrafluoroethylene D1 dispersed slightly in PC, and the transparency decreased. SAN-coated anti-dripping agents also cause a greater reduction in transparency, less than 85%, due to the difference in refractive index between SAN and PC. The emulsion type anti-dripping agent contains water, so that PC is partially hydrolyzed, and the transparency is greatly reduced to be less than 75%.
Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Claims (10)
1. A coated polytetrafluoroethylene anti-dripping agent is characterized in that the coated polytetrafluoroethylene is prepared by coating an organic ester emulsifier on the surface of polytetrafluoroethylene; the organic ester emulsifier comprises one or a mixture of fatty acid ester emulsifier and phosphate ester emulsifier; the fatty acid ester emulsifier is mono-diglycerol fatty acid ester; the phosphate ester emulsifier is any one or mixture of pentaerythritol phosphate, phosphoglyceride, triethyl phosphate and triphenyl phosphate.
2. The coated polytetrafluoroethylene anti-dripping agent according to claim 1, wherein the fatty acid in the mono-glycerol fatty acid ester and the diglycerol fatty acid ester comprises one or more of oleic acid, linoleic acid, linolenic acid, palmitic acid, behenic acid, stearic acid and lauric acid.
3. The method for preparing the coated polytetrafluoroethylene anti-dripping agent according to claim 1 or 2, wherein the method comprises the following steps:
(1) adding an organic ester emulsifier into the polytetrafluoroethylene emulsion, and stirring and emulsifying to obtain an organic ester/polytetrafluoroethylene emulsion;
(2) and (3) performing demulsification treatment on the prepared organic ester/polytetrafluoroethylene emulsion, then collecting the precipitate, drying the obtained precipitate, and then performing crushing treatment to prepare the coated polytetrafluoroethylene anti-dripping agent.
4. The preparation method of the coated polytetrafluoroethylene anti-dripping agent according to claim 3, wherein in the step (1), the solid content of the polytetrafluoroethylene emulsion is 58% -62%, the average molecular weight of the polytetrafluoroethylene is 100-1000 ten thousand, the particle size of the emulsion is 0.01-0.30 μm, and the viscosity is 10-100mPa · S.
5. The preparation method of the coated polytetrafluoroethylene anti-dripping agent according to claim 3, wherein in the step (1), the addition amount of the organic ester emulsifier is 10-100% of the mass of the polytetrafluoroethylene emulsion.
6. The method for preparing the coated polytetrafluoroethylene anti-dripping agent according to claim 3, wherein the temperature of the stirring and emulsifying treatment in the step (1) is 25-90 ℃ and the time is 0.5-8 h.
7. The preparation method of the coated polytetrafluoroethylene anti-dripping agent according to claim 3, wherein in the step (2), the demulsification treatment is one of heating demulsification, centrifugal demulsification, salting-out demulsification, electric demulsification and ultrasonic demulsification.
8. The method for preparing the coated polytetrafluoroethylene anti-dripping agent according to claim 3, wherein in the step (2), the drying mode is one of vacuum drying, freeze drying, air-blast drying, spray drying, infrared drying and microwave drying.
9. The method for preparing the coated polytetrafluoroethylene anti-dripping agent according to claim 3, wherein in the step (2), the crushing treatment is one of grinding, ball milling, jet milling and high-speed stirring and powdering.
10. The method for preparing the coated polytetrafluoroethylene anti-dripping agent according to claim 3, wherein in the step (2), the coated polytetrafluoroethylene anti-dripping agent has an average particle size of 100 μm-4 mm.
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