CN104418967A - Flame-retardant poly-alpha-methylstyrene composite material and preparation method thereof - Google Patents
Flame-retardant poly-alpha-methylstyrene composite material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a flame-retardant poly-alpha-methylstyrene composite material. The flame-retardant poly-alpha-methylstyrene composite material is prepared from 2-4 parts of nano-antimony trioxide, 7-10 parts of vinyl bromide, 80-100 parts of alpha-methylstyrene and 0.5-2 parts of an initiator. The invention further discloses a method for preparing the composite material by adopting a self-making method, and the method mainly comprises the following steps: preparing nano-antimony trioxide sol, then adding an alpha-methylstyrene monomer, a vinyl bromide monomer and the initiator, finally heating to initiate polymerization reaction of the alpha-methylstyrene and vinyl bromide monomers, and performing purification, drying and other treatment processes on the flame-retardant poly-alpha-methylstyrene composite material obtained after reaction to finally prepare the composite material. The composite material has good flame retardance.
Description
Technical field
The invention belongs to technical field of composite materials, particularly relate to a kind of fire-retardant poly alpha methylstyrene matrix material and prepare the method for fire-retardant poly alpha methylstyrene matrix material.
Background technology
One of fire retardant the earliest applied by antimonous oxide, reaches flame retardant effect as being used alone it, and the consumption of needs is very large, and flame retardant effect is poor; But when it is with halogen-containing compound and the used time, both have good synergistic effect, and very well, the fire retardant of therefore bromine/antimony compound system is widely used in the plastic materials such as epoxy resin, urethane, chloroprene rubber, polystyrene to flame retardant effect.The content of antimony element in the earth's crust is 0.0001%, and its antimony resource is on earth limited; Reduce its consumption in plastic material, reaching same flame retardant effect is the target that the mankind expect.
When material is in nanoscale scope, due to surface effects, small-size effect, quantum size effect and macro quanta tunnel effect etc., the beneficial characteristics that material is had can be brought into play more fully.In recent years, along with the continuous progress of nanosecond science and technology and matrix material technology of preparing, it is found that and nano-powder is combined with polymer materials, the matrix material obtained has the main characteristic of nano-powder and polymer materials, and the beneficial effect of powder body material can be made greatly to improve, therefore such matrix material receives extensive concern and the research of researcher.
Li Mingying etc. adopt twin screw extruder, nanometer grade antimony trioxide/MCA/PA flame-proof composite material has been prepared by the method for extruding pelletization, result of study shows, the flame retardant properties of dispersiveness on matrix material of nanometer grade antimony trioxide has larger impact (Li Mingying, Fan Zhangfan, Zhang Yu, etc. nanometer grade antimony trioxide and MCA cooperative flame retardant performance are on the impact [J] of PA6. plastics industry, 2008,36(12): 42-45).Nie Hongyun etc. adopt open type plastic purificating set, have prepared flame-proof polyvinyl chloride material by the method for plasticating.Comparative study common micro level antimonous oxide and nanometer grade antimony trioxide are on the impact of pvc material flame retardant properties, result of study shows, for micron order antimonous oxide, nanometer grade antimony trioxide will reach identical flame retardant effect, and addition can significantly reduce.This result of study shows, under identical environment for use, nanometer grade antimony trioxide has better flame retardant effect (Nie Hongyun, Nie is stood tall and upright, Xia Rui, etc. the research [J] of polyvinyl chloride (PVC) CABLE MATERIALS flame retardant properties. plastics industry, 2012,40(1): 104-106).
The above-mentioned method preparing nanmeter antimong trioxide/polymer composites, mainly by the machine such as twin screw extruder or plastics processing mill, realizes the dispersion of nanometer grade antimony trioxide in polymeric matrix by physical method.But these methods also also exist some shortcomings part, realize antimonous oxide as being difficult in polymeric matrix, reach nano level dispersion.Comparatively speaking, the preparation of ignition resistant polymeric composite is carried out in position under state, nanometer grade antimony trioxide dispersing uniformity in the composite can be made to be greatly improved, thus to give full play of the composite flame retardant effect of bromine/antimony, reach better flame retardant effect.
Summary of the invention
For the deficiency of nanmeter antimong trioxide in prior art/polymer composites research, an object of the present invention is to provide a kind of nanmeter antimong trioxide/poly alpha methylstyrene matrix material with good flame retardant properties; Another object of the present invention there is provided a kind of preparation method of fire-retardant poly alpha methylstyrene matrix material.
Object of the present invention can be achieved through the following technical solutions:
A kind of fire-retardant poly alpha methylstyrene matrix material is prepared from by weight by following composition:
Nanmeter antimong trioxide 2 ~ 4 parts;
Bromine ethene 7 ~ 10 parts;
Alpha-methyl styrene 80 ~ 100 parts;
Initiator 0.5 ~ 2 part.
Described initiator is at least one in Diisopropyl azodicarboxylate, Potassium Persulphate and ammonium persulphate.
Prepare a method for above-mentioned fire-retardant poly alpha methylstyrene matrix material, comprise the following steps:
(1) preparation of nanmeter antimong trioxide colloidal sol:
By the nanmeter antimong trioxide of 2 ~ 4 parts, the deionized water of 200 ~ 300 parts, the emulsifying agent of 40 ~ 60 parts joins in reactor, under continuously stirring state, the temperature of system is risen to 40 ~ 60 DEG C, continues to pass into nitrogen simultaneously; Then above-mentioned mixing solutions is carried out ultrasonic disperse 10 ~ 30 minutes, obtain nanmeter antimong trioxide colloidal sol.
(2) preparation of fire-retardant poly alpha methylstyrene matrix material:
In proportion nanmeter antimong trioxide colloidal sol and 80 ~ 100 parts of alpha-methyl styrenes, 7 ~ 10 parts of bromine ethene, 0.5 ~ 2 part of initiator are placed in reactor, under continuously stirring state, carry out ultrasonic disperse 10 ~ 30 minutes, continue to pass into nitrogen simultaneously;
Emulsifying agent is at least one in sodium lauryl sulphate and Sodium dodecylbenzene sulfonate in described step (1).
The polymeric reaction temperature of described step (2) is 70 ~ 90 DEG C, polymerization reaction time 10 ~ 16h.
Described step (2) purifying flow process refers in composite solution, to add the dehydrated alcohol or methanol solution that volume is 3 ~ 8 times of composite solution volume, abandoning supernatant after precipitation, centrifugation, again the material of lower floor is added in dehydrated alcohol or methanol solution again, repeat aforesaid operations 4 ~ 6 times, the lower floor's material obtained for the last time is placed in vacuum drying oven dry, obtains fire-retardant poly alpha methylstyrene matrix material.
So compared with prior art, the present invention has the following advantages and beneficial effect:
1, the present invention has prepared nanmeter antimong trioxide/poly alpha methylstyrene matrix material, because antimonous oxide is dispersed in poly alpha methylstyrene matrix with nano particle state, therefore makes matrix material have good flame retardant properties.
2, the present invention adopts Homemade method to prepare fire-retardant poly alpha methylstyrene matrix material, and this polyreaction is carried out under state in position, and nanmeter antimong trioxide particle can be made to be uniformly dispersed in the composite; Meanwhile, bromo element is in the course of the polymerization process, is introduced by bromine vinyl monomer, and the dispersiveness of bromo element in composite system is fine; Therefore give full play to the flame retardant effect that bromine/antimony is composite, make matrix material have better flame retardant properties.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Following examples nanmeter antimong trioxide used, bromine ethene, alpha-methyl styrene, sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, Diisopropyl azodicarboxylate, Potassium Persulphate, ammonium persulphate are Aladdin reagent company limited;
Ultrasonic cleaner used is Hefei Jin Nike ultrasonic cleaning company limited;
Injection moulding machine manufacturer used is Zhejiang Haitian Machinery Co., Ltd., and model is MA600/100;
Following examples agents useful for same is only and illustrates, is not limited to protection scope of the present invention, and other embodiments of the invention still can select all optional reagents in right.If no special instructions, described number is mass parts.
embodiment 1
(1) preparation of nanmeter antimong trioxide colloidal sol:
By the nanmeter antimong trioxide of 2 parts, the deionized water of 200 parts, the emulsifier sodium lauryl sulfate of 40 parts joins in reactor, under continuously stirring state, the temperature of system is risen to 40 DEG C, continues to pass into nitrogen simultaneously; Then above-mentioned mixing solutions is carried out ultrasonic disperse 10 minutes, obtain nanmeter antimong trioxide colloidal sol.
(2) preparation of fire-retardant poly alpha methylstyrene matrix material:
The nanmeter antimong trioxide colloidal sol obtained in (1) and the alpha-methyl styrene of 80 parts, the bromine ethene of 7 parts, the initiator Diisopropyl azodicarboxylate of 0.5 part are placed in reactor, under continuously stirring state, carry out ultrasonic disperse 10 minutes, continue to pass into nitrogen simultaneously;
Then be warming up to 70 DEG C and carry out polyreaction, reaction times is 16 hours, obtain composite solution, under agitation, in composite solution, add the ethanol solution that volume is 3 times of composite solution volume, abandoning supernatant after precipitation, centrifugation finally, again the material of lower floor is added in ethanol solution again, repeat aforesaid operations 4 times, the lower floor's material obtained for the last time is placed in vacuum drying oven dry, obtains fire-retardant poly alpha methylstyrene matrix material.
embodiment 2
(1) preparation of nanmeter antimong trioxide colloidal sol:
By the nanmeter antimong trioxide of 3 parts, the deionized water of 250 parts, the emulsifier sodium lauryl sulfate of 50 parts joins in reactor, under continuously stirring state, the temperature of system is risen to 50 DEG C, continues to pass into nitrogen simultaneously; Then above-mentioned mixing solutions is carried out ultrasonic disperse 20 minutes, obtain nanmeter antimong trioxide colloidal sol.
(2) preparation of fire-retardant poly alpha methylstyrene matrix material:
The nanmeter antimong trioxide colloidal sol obtained in (1) and the alpha-methyl styrene of 90 parts, the bromine ethene of 9 parts, the initiator Diisopropyl azodicarboxylate of 0.5 part, the initiator potassium persulfate of 0.5 part are placed in reactor, under continuously stirring state, carry out ultrasonic disperse 20 minutes, continue to pass into nitrogen simultaneously;
Then be warming up to 80 DEG C and carry out polyreaction, reaction times is 14 hours, obtain composite solution, under agitation, in composite solution, add the ethanol solution that volume is 6 times of composite solution volume, abandoning supernatant after precipitation, centrifugation finally, again the material of lower floor is added in ethanol solution again, repeat aforesaid operations 5 times, the lower floor's material obtained for the last time is placed in vacuum drying oven dry, obtains fire-retardant poly alpha methylstyrene matrix material.
embodiment 3
(1) preparation of nanmeter antimong trioxide colloidal sol:
By the nanmeter antimong trioxide of 4 parts, the deionized water of 300 parts, the emulsifying agent Sodium dodecylbenzene sulfonate of 60 parts joins in reactor, under continuously stirring state, the temperature of system is risen to 60 DEG C, continues to pass into nitrogen simultaneously; Then above-mentioned mixing solutions is carried out ultrasonic disperse 30 minutes, obtain nanmeter antimong trioxide colloidal sol.
(2) preparation of fire-retardant poly alpha methylstyrene matrix material:
The nanmeter antimong trioxide colloidal sol obtained in (1) and the alpha-methyl styrene of 100 parts, the bromine ethene of 10 parts, the initiator Diisopropyl azodicarboxylate of 0.5 part, the initiator potassium persulfate of 1 part are placed in reactor, under continuously stirring state, carry out ultrasonic disperse 30 minutes, continue to pass into nitrogen simultaneously;
Then be warming up to 90 DEG C and carry out polyreaction, reaction times is 10 hours, obtain composite solution, under agitation, in composite solution, add the ethanol solution that volume is 8 times of composite solution volume, abandoning supernatant after precipitation, centrifugation finally, again the material of lower floor is added in absolute methanol solution again, repeat aforesaid operations 6 times, the lower floor's material obtained for the last time is placed in vacuum drying oven dry, obtains fire-retardant poly alpha methylstyrene matrix material.
embodiment 4
(1) preparation of nanmeter antimong trioxide colloidal sol:
By the nanmeter antimong trioxide of 2 parts, the deionized water of 250 parts, the emulsifying agent Sodium dodecylbenzene sulfonate of 45 parts joins in reactor, under continuously stirring state, the temperature of system is risen to 40 DEG C, continues to pass into nitrogen simultaneously; Then above-mentioned mixing solutions is carried out ultrasonic disperse 15 minutes, obtain nanmeter antimong trioxide colloidal sol.
(2) preparation of fire-retardant poly alpha methylstyrene matrix material:
The nanmeter antimong trioxide colloidal sol obtained in (1) and the alpha-methyl styrene of 85 parts, the bromine ethene of 8 parts, the initiator potassium persulfate of 2 parts are placed in reactor, under continuously stirring state, carry out ultrasonic disperse 15 minutes, continue to pass into nitrogen simultaneously;
Then be warming up to 70 DEG C and carry out polyreaction, reaction times is 16 hours, obtain composite solution, under agitation, in composite solution, add the ethanol solution that volume is 3 times of composite solution volume, abandoning supernatant after precipitation, centrifugation finally, again the material of lower floor is added in absolute methanol solution again, repeat aforesaid operations 6 times, the lower floor's material obtained for the last time is placed in vacuum drying oven dry, obtains fire-retardant poly alpha methylstyrene matrix material.
embodiment 5
(1) preparation of nanmeter antimong trioxide colloidal sol:
By the nanmeter antimong trioxide of 3 parts, the deionized water of 280 parts, the emulsifying agent Sodium dodecylbenzene sulfonate of 55 parts joins in reactor, under continuously stirring state, the temperature of system is risen to 55 DEG C, continues to pass into nitrogen simultaneously; Then above-mentioned mixing solutions is carried out ultrasonic disperse 25 minutes, obtain nanmeter antimong trioxide colloidal sol.
(2) preparation of fire-retardant poly alpha methylstyrene matrix material:
The nanmeter antimong trioxide colloidal sol obtained in (1) and the alpha-methyl styrene of 90 parts, the bromine ethene of 8 parts, the initiator potassium persulfate of 1 part, the initiator ammonium persulfate of 1 part are placed in reactor, under continuously stirring state, carry out ultrasonic disperse 20 minutes, continue to pass into nitrogen simultaneously;
Then be warming up to 80 DEG C and carry out polyreaction, reaction times is 12 hours, obtain composite solution, under agitation, in composite solution, add the ethanol solution that volume is 5 times of composite solution volume, abandoning supernatant after precipitation, centrifugation finally, again the material of lower floor is added in absolute methanol solution again, repeat aforesaid operations 5 times, the lower floor's material obtained for the last time is placed in vacuum drying oven dry, obtains fire-retardant poly alpha methylstyrene matrix material.
embodiment 6
(1) preparation of nanmeter antimong trioxide colloidal sol:
By the nanmeter antimong trioxide of 4 parts, the deionized water of 300 parts, the emulsifying agent Sodium dodecylbenzene sulfonate of 60 parts joins in reactor, under continuously stirring state, the temperature of system is risen to 60 DEG C, continues to pass into nitrogen simultaneously; Then above-mentioned mixing solutions is carried out ultrasonic disperse 30 minutes, obtain nanmeter antimong trioxide colloidal sol.
(2) preparation of fire-retardant poly alpha methylstyrene matrix material:
The nanmeter antimong trioxide colloidal sol obtained in (1) and the alpha-methyl styrene of 90 parts, the bromine ethene of 7 parts, the initiator Diisopropyl azodicarboxylate of 1 part, the initiator ammonium persulfate of 1 part are placed in reactor, under continuously stirring state, carry out ultrasonic disperse 20 minutes, continue to pass into nitrogen simultaneously;
Then be warming up to 80 DEG C and carry out polyreaction, reaction times is 14 hours, obtain composite solution, under agitation, in composite solution, add the absolute methanol solution that volume is 4 times of composite solution volume, abandoning supernatant after precipitation, centrifugation finally, again the material of lower floor is added in absolute methanol solution again, repeat aforesaid operations 6 times, the lower floor's material obtained for the last time is placed in vacuum drying oven dry, obtains fire-retardant poly alpha methylstyrene matrix material.
comparative example 1
(1) nanmeter antimong trioxide of 2 parts, the bromine ethene of 10 parts, the poly alpha methylstyrene resin of 80 parts are used 1000rpm rotating speed mixing 5min in high-speed mixer, obtain the mixture after dispersion treatment;
(2) by step (1) gained mixture extruding pelletization in twin screw extruder, fire-retardant poly alpha methylstyrene matrix material pellet is obtained.Twin screw extruder comprises six districts, and wherein each district temperature and screw speed are respectively: district's temperature 170 DEG C, two district's temperature 180 DEG C, three district's temperature 190 DEG C, four district's temperature 190 DEG C, five district's temperature 200 DEG C, six district's temperature 210 DEG C, head temperature 210 DEG C; Screw speed 250r/min.
comparative example 2
(1) nanmeter antimong trioxide of 3 parts, the bromine ethene of 8 parts, the poly alpha methylstyrene resin of 90 parts are used 800rpm rotating speed mixing 10min in high-speed mixer, obtain the mixture after dispersion treatment;
(2) by step (1) gained mixture extruding pelletization in twin screw extruder, fire-retardant poly alpha methylstyrene matrix material pellet is obtained.Twin screw extruder comprises six districts, and wherein each district temperature and screw speed are respectively: district's temperature 160 DEG C, two district's temperature 170 DEG C, three district's temperature 180 DEG C, four district's temperature 190 DEG C, five district's temperature 200 DEG C, six district's temperature 200 DEG C, head temperature 200 DEG C; Screw speed 300r/min.
comparative example 3
(1) nanmeter antimong trioxide of 4 parts, the bromine ethene of 7 parts, the poly alpha methylstyrene resin of 100 parts are used 1200rpm rotating speed mixing 5min in high-speed mixer, obtain the mixture after dispersion treatment;
(2) by step (1) gained mixture extruding pelletization in twin screw extruder, fire-retardant poly alpha methylstyrene matrix material pellet is obtained.Twin screw extruder comprises six districts, and wherein each district temperature and screw speed are respectively: district's temperature 170 DEG C, two district's temperature 175 DEG C, three district's temperature 180 DEG C, four district's temperature 185 DEG C, five district's temperature 190 DEG C, six district's temperature 195 DEG C, head temperature 200 DEG C; Screw speed 350r/min.
By the fire-retardant poly alpha methylstyrene matrix material of preparation in embodiment 1 ~ 9, carry out injection moulding according to ASTM, batten thickness is 3.2mm, injection moulding batten 23 DEG C, stablize 48h under relative humidity 50% condition after, carry out combustionproperty test according to UL 94-1996, test result is in table 1.
The flame retardant properties of table 1 embodiment 1 ~ 6 and comparative example 1 ~ 3 gained matrix material
Flame retardant properties test result contrast as can be seen from table 1, the flame retardant properties of the fire-retardant poly alpha methylstyrene matrix material prepared by the polymerisation process in the present invention, obviously be better than the fire-retardant poly alpha methylstyrene matrix material adopting double-screw extruding pelletizing method to prepare, mainly due to adopt polymerisation process of the present invention obtained matrix material in, nanmeter antimong trioxide particle has good dispersiveness in poly alpha methylstyrene matrix, bromo element is in the course of the polymerization process, introduced by bromine vinyl monomer, the dispersiveness of bromo element in material system is better, therefore the composite flame retardant effect of bromine/antimony can more be given full play to, matrix material is made to have better flame retardant properties.
The above-mentioned description to embodiment can understand and apply the invention for ease of those skilled in the art.Person skilled in the art obviously easily can make various amendment to these embodiments, and General Principle described herein is applied in other embodiments and need not through performing creative labour.Therefore, the invention is not restricted to embodiment here, those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.
Claims (6)
1. a fire-retardant poly alpha methylstyrene matrix material, is characterized in that: be prepared from by weight by following composition:
Nanmeter antimong trioxide 2 ~ 4 parts;
Bromine ethene 7 ~ 10 parts;
Alpha-methyl styrene 80 ~ 100 parts;
Initiator 0.5 ~ 2 part.
2. the fire-retardant poly alpha methylstyrene matrix material of one according to claim 1, is characterized in that: described initiator is at least one in Diisopropyl azodicarboxylate, Potassium Persulphate and ammonium persulphate.
3. the preparation method of a kind of fire-retardant poly alpha methylstyrene matrix material according to claim 1, is characterized in that, comprise the following steps:
(1) preparation of nanmeter antimong trioxide colloidal sol:
By the nanmeter antimong trioxide of 2 ~ 4 parts, the deionized water of 200 ~ 300 parts, the emulsifying agent of 40 ~ 60 parts joins in reactor, under continuously stirring state, the temperature of system is risen to 40 ~ 60 DEG C, continues to pass into nitrogen simultaneously; Then above-mentioned mixing solutions is carried out ultrasonic disperse 10 ~ 30 minutes, obtain nanmeter antimong trioxide colloidal sol;
(2) preparation of fire-retardant poly alpha methylstyrene matrix material:
In proportion nanmeter antimong trioxide colloidal sol and 80 ~ 100 parts of alpha-methyl styrenes, 7 ~ 10 parts of bromine ethene, 0.5 ~ 2 part of initiator are placed in reactor, under continuously stirring state, carry out ultrasonic disperse 10 ~ 30 minutes, continue to pass into nitrogen simultaneously;
Then heat up and carry out polyreaction and obtain composite solution, under agitation, the purified flow process of composite solution obtains fire-retardant poly alpha methylstyrene matrix material finally.
4. the preparation method of a kind of fire-retardant poly alpha methylstyrene matrix material according to claim 3, is characterized in that: emulsifying agent is at least one in sodium lauryl sulphate and Sodium dodecylbenzene sulfonate in described step (1).
5. the preparation method of a kind of fire-retardant poly alpha methylstyrene matrix material according to claim 3, is characterized in that: the polymeric reaction temperature of described step (2) is 70 ~ 90 DEG C, polymerization reaction time 10 ~ 16h.
6. the preparation method of a kind of fire-retardant poly alpha methylstyrene matrix material according to claim 3, it is characterized in that: described step (2) purifying flow process refers in composite solution, to add the dehydrated alcohol or methanol solution that volume is 3 ~ 8 times of composite solution volume, abandoning supernatant after precipitation, centrifugation, again the material of lower floor is added in dehydrated alcohol or methanol solution again, repeat aforesaid operations 4 ~ 6 times, the lower floor's material obtained for the last time is placed in vacuum drying oven dry, obtains fire-retardant poly alpha methylstyrene matrix material.
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Application publication date: 20150318 |