CN105440689A - Silicon-antimony composite flame retardant, and preparation method and applications thereof - Google Patents
Silicon-antimony composite flame retardant, and preparation method and applications thereof Download PDFInfo
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- CN105440689A CN105440689A CN201510957221.2A CN201510957221A CN105440689A CN 105440689 A CN105440689 A CN 105440689A CN 201510957221 A CN201510957221 A CN 201510957221A CN 105440689 A CN105440689 A CN 105440689A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
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Abstract
The invention provides a silicon-antimony composite flame retardant, and a preparation method and applications thereof. The silicon-antimony composite flame retardant is prepared from 20 to 40% of organic silicon, 5 to 15% of silicone master batch, 5 to 15% of antimonous oxide, 10 to 15% of tetrabromo diphenylethane, and 15 to 60% of a carrier material. The silicon-antimony composite flame retardant is obtained via blend doping and extrusion; high oxygen index flame resistance of the silicon-antimony composite flame retardant is capable of reaching V0 grade; when adding amount of the silicon-antimony composite flame retardant in ester resin base materials is 4%, flame resistance of the ester resin base materials can be improved to V0 grade; excellent dispersity, and mechanical and physical effects are achieved at a low adding amount; cost is low; the silicon-antimony composite flame retardant can be used for replacing antimonous oxide as a flame retardant, can be applied to the fields such as microelectronics, electric appliance, medical treatment, electric wire and cable, industrial and mining, fire protection, petrochemical engineering, train, car, and airplane, and possesses excellent flame resistance.
Description
Technical field
The invention belongs to fire retardant preparation field, relate to a kind of silicon antimony composite flame-retardant agent and its preparation method and application.
Background technology
At present, along with the extensive application of building plastic material and normal domestic plastics, the requirement of its plastic material in flame retardant properties is also more and more higher, and in order to adapt to the development need of national economy, increasing plastics all require to reach certain fire-retardant rank.Because the additive of plastics requirement is except liquid or high temperature can melt, the granularity of required additive material is very thin, to obtain good product performance.And as fire retarding synergist the most frequently used in fire retardant material---the general particle diameter of fineness of antimonous oxide is at about 1.0 μm, so carry out mixing when very tiny antimonous oxide powder is joined in reisn base material, in the process of granulation, a large amount of dust pollutions and noise will be created, work situation is comparatively severe, in addition antimonous oxide is heavy metal oxide, can cause prestige evil to HUMAN HEALTH.
CN105111569A discloses and a kind of preparation method of antimonous oxide fire-retardant master granule, in the invention: by 96% ~ 98% (weight percent, antimonous oxide powder down together), the vector resin of 2% ~ 4%, homogenizer high-speed stirring to 70 DEG C ~ 110 DEG C, when being stirred to without dust, mixed material is joined melting in screw extrusion press, plasticizing, extrude, pelletizing prepares antimonous oxide fire-retardant master granule again, in this fire-retardant master granule, antimonous oxide content is higher, in preparation process, dust hazard is larger, and cost is high, be not suitable for the application of suitability for industrialized production.
Therefore, find in the art a kind of with low cost and the antimony fire retardant with fine flame retardant properties is the problem needing solution badly.
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide a kind of silicon antimony composite flame-retardant agent machine preparation method and application.
For reaching this object, the present invention by the following technical solutions:
On the one hand, the invention provides a kind of silicon antimony composite flame-retardant agent, described silicon antimony composite flame-retardant agent is prepared by the raw material that weight percent is following:
In the raw material of silicon antimony composite flame-retardant agent of the present invention, organosilyl consumption is 20-40%, such as 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, 30%, 32%, 34%, 36%, 38%, 39% or 40%.
In the raw material of silicon antimony composite flame-retardant agent of the present invention, the consumption of silicone master batch is 5-15%, such as 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14% or 14.5%.
In the raw material of silicon antimony composite flame-retardant agent of the present invention, the consumption of antimonous oxide is 5-15%, such as 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14% or 14.5%.
In the raw material of silicon antimony composite flame-retardant agent of the present invention, the consumption of four bromo diphenylethanes is 10-15%, such as 10.5%, 11%, 11.5%, 12%, 12.5%, 13%, 13.5%, 14%, 14.5% or 15%.
In the raw material of silicon antimony composite flame-retardant agent of the present invention, the consumption of solid support material is 15-60%, such as 15.5%, 16%, 17%, 18%, 20%, 23%, 25%, 28%, 30%, 33%, 36%, 38%, 40%, 43%, 45%, 48%, 50%, 52%, 55%, 58% or 59%.
In silicon antimony composite flame-retardant agent of the present invention, described organosilicon is the combination of any one or at least two kinds in silicone grease, silicon emulsion, silicon rubber, sulphurated siliastic or silicone resin.
In silicon antimony composite flame-retardant agent of the present invention, described solid support material is the combination of any one or at least two kinds in high density ethylene, dihydroxyphenyl propane, monomer polymeric amide, polystyrene resin, polyvinyl chloride, polypropylene, ABS resin (acrylonitrile-butadiene-styrene copolymer) or PBT resin (polybutylene terephthalate).Described monomer polymeric amide is nylon.
Preferably, the relative density of described high density ethylene is 0.941 ~ 0.960.
Preferably, described silicon antimony composite flame-retardant agent is prepared by the raw material that weight percent is following:
On the other hand, the invention provides the preparation method of described silicon antimony composite flame-retardant agent, said method comprising the steps of:
(1) silicone master batch, solid support material and four bromo diphenylethanes are added in mixer carry out blended doping, obtain mixture;
(2) in step (1) gained mixture, add organosilicon and antimonous oxide, be uniformly mixed, then utilize extruding pelletization in forcing machine, obtain described silicon antimony composite flame-retardant agent.
In the method for the invention, step (1) described blended doping time stir speed (S.S.) be 80-100r/min, such as 8r/min, 83r/min, 85r/min, 88r/min, 90r/min, 92r/min, 94r/min, 96r/min, 98r/min or 99r/min.
Preferably, the mixing time of the described blended doping of step (1) is 10-30min, such as 11min, 12min, 13min, 14min, 15min, 16min, 17min, 18min, 19min, 20min, 21min, 22min, 23min, 24min, 25min, 26min, 27min, 28min or 29min.
In preparation method of the present invention, the stir speed (S.S.) be uniformly mixed described in step (2) is 100-200r/min, such as 110r/min, 120r/min, 130r/min, 140r/min, 150r/min, 160r/min, 170r/min, 180r/min, 190r/min or 200r/min.
Preferably, step (2) described mixing time is 5-15min, such as 6min, 7min, 8min, 9min, 10min, 11min, 12min, 13min, 14min or 15min.
Preferably, step (2) described forcing machine is twin screw extruder.
Preferably, the preheating temperature in the described extruder screw region of step (2) is 200-300 DEG C, such as 210 DEG C, 220 DEG C, 230 DEG C, 240 DEG C, 250 DEG C, 260 DEG C, 270 DEG C, 280 DEG C, 290 DEG C or 295 DEG C.
Preferably, the screw speed of step (2) described forcing machine is 200-350r/min, such as 210r/min, 220r/min, 230r/min, 250r/min, 270r/min, 290r/min, 300r/min, 320r/min, 330r/min or 340r/min.
As the preferred technical solution of the present invention, the preparation method of silicon antimony composite flame-retardant agent of the present invention comprises the following steps:
(1) silicone master batch, solid support material and four bromo diphenylethanes are added in mixer and carry out blended doping, stir speed (S.S.) is 80-100r/min, and blended doping 10-30min, obtains mixture;
(2) in step (1) gained mixture, organosilicon and antimonous oxide is added, 5-15min is uniformly mixed under the stir speed (S.S.) of 100-200r/min, then utilize extruding pelletization in forcing machine, the preheating temperature in described extruder screw region is 200-300 DEG C, screw speed is 200-350r/min, obtains described silicon antimony composite flame-retardant agent.
On the other hand, the invention provides the application of described silicon antimony composite flame-retardant agent in resin base material.
Preferably, described resin base material is the combination of any one or at least two kinds in polyethylene, nylon, polystyrene resin, polyvinyl chloride, polypropylene, ABS resin or PBT resin.
Preferably, the addition of described silicon antimony composite flame-retardant agent in resin base material is 1-10%, such as 1.5%, 2%, 3%, 4%, 5%, 6%, 7%, 8% or 9%, preferably 4%.
Relative to prior art, the present invention has following beneficial effect:
Silicon antimony composite flame-retardant agent of the present invention is by 20-40% organosilicon, 5-15% silicone master batch, 5-15% antimonous oxide, 10-15% tetra-bromo diphenylethane and 15-60% solid support material prepare, the present invention passes through blended doping, extrude and obtain described silicon antimony composite flame-retardant agent, its high oxygen index flame retardant resistance is made to reach V0 level, when in resin base material, addition is 4%, the flame retardant resistance of resin material can be made to reach V0 level, the little dispersiveness of addition is excellent, mechanics physical effect is good, cost is low, antimonous oxide can be substituted as fire retardant, be applied to microelectronics, electrical equipment, medical treatment, weaving, printing, industrial and mineral, war industry equipment, fire-fighting, firer, petrochemical complex, train vehicle aircraft, packaging, the fields such as transport, there is superior flame retardant effect.
Embodiment
Technical scheme of the present invention is further illustrated below by embodiment.Those skilled in the art should understand, described embodiment is only help to understand the present invention, should not be considered as concrete restriction of the present invention.
Embodiment 1
In the present embodiment, silicon antimony composite flame-retardant agent is prepared by following raw material:
Preparation method is as follows:
(1) silicone master batch, solid support material and four bromo diphenylethanes are added in mixer and carry out blended doping, stir speed (S.S.) is 100r/min, and blended doping 10min, obtains mixture;
(2) in step (1) gained mixture, organosilicon and antimonous oxide is added, 10min is uniformly mixed under the stir speed (S.S.) of 150r/min, then utilize extruding pelletization in forcing machine, the preheating temperature in described extruder screw region is 200 DEG C, screw speed is 300r/min, obtains described silicon antimony composite flame-retardant agent.
Embodiment 2
In the present embodiment, silicon antimony composite flame-retardant agent is prepared by following raw material:
Preparation method is as follows:
(1) silicone master batch, solid support material and four bromo diphenylethanes are added in mixer and carry out blended doping, stir speed (S.S.) is 80r/min, and blended doping 30min, obtains mixture;
(2) in step (1) gained mixture, organosilicon and antimonous oxide is added, 15min is uniformly mixed under the stir speed (S.S.) of 100r/min, then utilize extruding pelletization in forcing machine, the preheating temperature in described extruder screw region is 300 DEG C, screw speed is 200r/min, obtains described silicon antimony composite flame-retardant agent.
Embodiment 3
In the present embodiment, silicon antimony composite flame-retardant agent is prepared by following raw material:
Preparation method is as follows:
(1) silicone master batch, solid support material and four bromo diphenylethanes are added in mixer and carry out blended doping, stir speed (S.S.) is 90r/min, and blended doping 20min, obtains mixture;
(2) in step (1) gained mixture, organosilicon and antimonous oxide is added, 5min is uniformly mixed under the stir speed (S.S.) of 180r/min, then utilize extruding pelletization in forcing machine, the preheating temperature in described extruder screw region is 300 DEG C, screw speed is 350r/min, obtains described silicon antimony composite flame-retardant agent.
Embodiment 4
In the present embodiment, silicon antimony composite flame-retardant agent is prepared by following raw material:
Preparation method is as follows:
(1) silicone master batch, solid support material and four bromo diphenylethanes are added in mixer and carry out blended doping, stir speed (S.S.) is 100r/min, and blended doping 15min, obtains mixture;
(2) in step (1) gained mixture, organosilicon and antimonous oxide is added, 15min is uniformly mixed under the stir speed (S.S.) of 200r/min, then utilize extruding pelletization in forcing machine, the preheating temperature in described extruder screw region is 200-300 DEG C, screw speed is 200-350r/min, obtains described silicon antimony composite flame-retardant agent.
Embodiment 5
In the present embodiment, silicon antimony composite flame-retardant agent is prepared by following raw material:
Preparation method is as follows:
(1) silicone master batch, solid support material and four bromo diphenylethanes are added in mixer and carry out blended doping, stir speed (S.S.) is 80r/min, and blended doping 30min, obtains mixture;
(2) in step (1) gained mixture, add organosilicon and antimonous oxide, under the stir speed (S.S.) of 150r/min, be uniformly mixed 15min, then utilize extruding pelletization in forcing machine, obtain described fire-retardant, electrostatic-conducting dissipative type master batch., the preheating temperature in described extruder screw region is 250 DEG C, and screw speed is 200r/min, obtains described silicon antimony composite flame-retardant agent.
Comparative example 1
In this comparative example, prepare fire retardant by following raw material:
Preparation method is identical with embodiment 1 with condition.
Comparative example 2
In this comparative example, prepare fire retardant by following raw material:
Preparation method is identical with embodiment 1 with condition.
Comparative example 3
In this comparative example, prepare fire retardant by following raw material:
Preparation method is identical with embodiment 1 with condition.
Comparative example 4
In this comparative example, prepare fire retardant by following raw material:
Preparation method is identical with embodiment 1 with condition.
Comparative example 5
In this comparative example, prepare fire retardant by following raw material:
Preparation method is identical with embodiment 1 with condition.
Comparative example 6
In this comparative example, prepare fire retardant by following raw material:
Preparation method is identical with embodiment 1 with condition.
By the fire retardant of embodiment 1-5 and comparative example 1-6 with 4% addition be added in pvc material, utilize UL94 flammability test to carry out the flame retardant properties of test material, result is as shown in table 1.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 4 | Embodiment 4 | Embodiment 5 | ||
| Flame retardant resistance | V0 level | V1 level | V0 level | V0 level | V1 level | |
| Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 | |
| Flame retardant resistance | V2 level | V2 level | V2 level | V2 level | V2 level | V2 level |
As can be seen from Table 1, when silicon antimony composite flame-retardant agent of the present invention is added in vinylchlorid material, flame retardant properties preferably can reach V0 level, and when when preparing fire retardant, when only adding antimonous oxide or four bromo diphenylethanes, such as comparative example 1 or 2, it all can not make the flame retardant properties of pvc material be significantly increased, and in the embodiment of the present invention 1, add antimonous oxide and four bromo diphenylethanes simultaneously, flame retardant properties then can be made to reach V0 level, therefore illustrate that antimonous oxide and four bromo diphenylethanes have synergy in the present invention, in addition, when the consumption of antimonous oxide or four bromo diphenylethanes too much or very few time (such as comparative example 3-6), all can not improve the flame retardant resistance of vinylchlorid material.
Applicant states, the present invention illustrates method detailed of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned method detailed, does not namely mean that the present invention must rely on above-mentioned method detailed and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (10)
1. a silicon antimony composite flame-retardant agent, is characterized in that, described silicon antimony composite flame-retardant agent is prepared by the raw material that weight percent is following:
2. silicon antimony composite flame-retardant agent according to claim 1, is characterized in that, described organosilicon is the combination of any one or at least two kinds in silicone grease, silicon emulsion, silicon rubber, sulphurated siliastic or silicone resin.
3. silicon antimony composite flame-retardant agent according to claim 1 and 2, it is characterized in that, described solid support material is the combination of any one or at least two kinds in high density ethylene, dihydroxyphenyl propane, monomer polymeric amide, polystyrene resin, polyvinyl chloride, polypropylene, ABS resin or PBT resin.
4. silicon antimony composite flame-retardant agent according to claim 3, is characterized in that, the relative density of described high density ethylene is 0.941 ~ 0.960.
5. the silicon antimony composite flame-retardant agent according to any one of claim 1-4, is characterized in that, described silicon antimony composite flame-retardant agent is prepared by the raw material that weight percent is following:
6. the preparation method of the silicon antimony composite flame-retardant agent according to any one of claim 1-5, is characterized in that, said method comprising the steps of:
(1) silicone master batch, solid support material and four bromo diphenylethanes are added in mixer carry out blended doping, obtain mixture;
(2) in step (1) gained mixture, add organosilicon and antimonous oxide, be uniformly mixed, then utilize extruding pelletization in forcing machine, obtain described silicon antimony composite flame-retardant agent.
7. preparation method according to claim 6, is characterized in that, step (1) described blended doping time stir speed (S.S.) be 80-100r/min;
Preferably, the mixing time of the described blended doping of step (1) is 10-30min.
8. the preparation method according to claim 6 or 7, is characterized in that, the stir speed (S.S.) be uniformly mixed described in step (2) is 100-200r/min;
Preferably, step (2) described mixing time is 5-15min;
Preferably, step (2) described forcing machine is twin screw extruder;
Preferably, the preheating temperature in the described extruder screw region of step (2) is 200-300 DEG C;
Preferably, the screw speed of step (2) described forcing machine is 200-350r/min.
9. the preparation method according to any one of claim 6-8, is characterized in that, said method comprising the steps of:
(1) silicone master batch, solid support material and four bromo diphenylethanes are added in mixer and carry out blended doping, stir speed (S.S.) is 80-100r/min, and blended doping 10-30min, obtains mixture;
(2) in step (1) gained mixture, organosilicon and antimonous oxide is added, 5-15min is uniformly mixed under the stir speed (S.S.) of 100-200r/min, then utilize extruding pelletization in forcing machine, the preheating temperature in described extruder screw region is 200-300 DEG C, screw speed is 200-350r/min, obtains described silicon antimony composite flame-retardant agent.
10. the application of silicon antimony composite flame-retardant agent in resin base material according to any one of claim 1-5;
Preferably, described resin base material is the combination of any one or at least two kinds in polyethylene, nylon, polystyrene resin, polyvinyl chloride, polypropylene, ABS resin or PBT resin;
Preferably, the addition of described silicon antimony composite flame-retardant agent in resin base material is 1-10%, preferably 4%.
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| CN106751593B (en) * | 2017-01-18 | 2019-06-21 | 东莞市票友机电科技有限公司 | Binder motor mount PBT engineering plastics and motor mount |
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Application publication date: 20160330 |