CN105111506A - Antimonic smoke-abating flame-retardant master batch and preparation method thereof - Google Patents
Antimonic smoke-abating flame-retardant master batch and preparation method thereof Download PDFInfo
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- CN105111506A CN105111506A CN201510198681.1A CN201510198681A CN105111506A CN 105111506 A CN105111506 A CN 105111506A CN 201510198681 A CN201510198681 A CN 201510198681A CN 105111506 A CN105111506 A CN 105111506A
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Abstract
The invention discloses an antimonic smoke-abating flame-retardant master batch and a preparation method thereof. The master batch comprises the following raw materials by mass: 60 to 80% of compound antimonide, 5 to 10% of a stabilizing agent, 5 to 10% of a coupling agent and 10 to 20% of a smoke suppressor, wherein the compound antimonide is a compound of two or three selected from the group consisting of antimonous oxide, sodium antimonate and antimony pentoxide, the stabilizing agent is zinc stearate, the coupling agent is titanate or silane, and the smoke suppressor is zinc molybdate. The preparation method comprises the following steps: modifying the compound antimonide; then putting the modified compound antimonide, the stabilizing agent and the smoke suppressor into a three-dimensional mixer for complete mixing; extruding the mixed materials through a double screw extruder; granulating the extruded materials by using an automatic powder granulator; and successively carrying out screening with a vibrating centrifugal screening machine, drying and packaging. According to the invention, smoke amount in usage of the fire retardant is reduced while flame retardation effect is improved; and preparation process is simplified.
Description
[technical field]
The invention belongs to fire retardant material field, be specifically related to a kind of antimony system smoke resistance flame resistance master batch and preparation method thereof.
[background technology]
Flame-retardant master batch also claims fire-retardant master granule, fire prevention master batch, is a kind of novel flame retardant products.Flame-retardant master batch has and to be easy to add in resin, and sanitation and hygiene, dust are few, and flame retarding efficiency is high, addition is little, little to the Effect on Mechanical Properties of resin, not easily there is the bad phenomenon such as layering, decorative pattern, precipitation after interpolation, save the plurality of advantages such as human and material resources cost and time.At present, develop the flame-retardant master batch that some contain antimony, but mostly these fire retardants are that with organic halogen fire retardant be main fire retardant, as: Korean patent document (publication number: KR200826501A) discloses a kind of flame-retardant master batch containing polypropylene, eight bromo ether, antimonous oxide, stablizer and antioxidant; Canadian Patent document (publication number: CA2498342A) discloses a kind of for polyolefinic flame-retardant master batch, the halogen flame that this flame-retardant master batch composition (based on polyolefine and fire retardant total amount) is 4-14%, the aluminium hydroxide of 4-15%, the antimonous oxide of 1-5%.Because halogen flame can produce a large amount of smog and poisonous corrosive hydrogen halides gas when fire-retardant, cause secondary injury, thus, the non-halogen cry of fire retardant also improves day by day.
Sb system fire retardant is one of important inorganic combustion inhibitor; but; the research and development taking Sb system fire retardant as the fire-retardant master granule of main component or compositional flame-retardant masterbatch are less; by carrying out refinement, modification, the optimization design such as composite to conventional oxidation antimony flame retardant products, be a trend of Sb system fire retardant future development.Chinese patent literature " a kind of manufacture method of antimony trioxide parent particle " (application number: CN200710000830.4) disclose a kind of with antimonous oxide powder, carrier, dispersion agent and coupling agent for raw material, through modification, extrude, method that granulation, screening, the process such as drying prepare antimony trioxide parent particle.Chinese patent literature " a kind of antimony trioxide parent particle and preparation method thereof " (application number: CN201110429778.0) discloses a kind of antimony trioxide parent particle being raw material with nanmeter antimong trioxide, carrier, modification ethylene bis-fatty acid amides.Above-mentioned antimony trioxide parent particle only adopts a kind of inorganic combustion inhibitor of antimonous oxide, flame retardant effect and smoke suppressing effect limited.Chinese patent literature " a kind of low cigarette type antimonous oxide compound flame retardant and preparation method thereof " (application number: CN201210143074.1) discloses a kind of low cigarette type antimonous oxide compound flame retardant comprising antimonous oxide, hydrotalcite, zinc borate, polynite and coupling agent, but this method adopts common high-speed mixer in mixing of materials, mixed effect is limited, adopt two step screenings in sieving technology, simplify not.
[summary of the invention]
The present invention is directed to halogen containing flame-retardant in prior art antimony system fire-retardant master granule more, poisonous corrosive gases is easily produced during burning, flame retardant effect and the limited deficiency of smoke suppressing effect, a kind of antimony system smoke resistance flame resistance master batch is provided, object is to improve fire-retardant, smoke suppressing effect, simplify preparation technology, enhance productivity.
Technical solution of the present invention is as follows:
A kind of antimony system smoke resistance flame resistance master batch, comprises the raw material of following mass percent: compound stibnide 60%-80%, stablizer 5%-10%, coupling agent 5%-10%, smoke suppressor 10%-20%.
Preferably, described compound stibnide is the mixture of antimonous oxide, sodium antimonate, antimony peroxide mixture or three between two.
Preferably, described stablizer is Zinic stearas.
Preferably, described coupling agent is titanic acid ester or silane.
Preferably, described smoke suppressor is zinc molybdate.
The present invention also provides the preparation method of a kind of antimony system smoke resistance flame resistance master batch, the steps include:
S1: compound stibnide modification: compound stibnide and coupling agent are dropped into homogenizer and carries out modification, modification temperature 100 DEG C ~ 140 DEG C, stir speed (S.S.) 2000r/min ~ 4000r/min, churning time 3.5h ~ 4.5h, obtained modification compound stibnide;
S2: three-dimensional hybrid: modification compound stibnide obtained for step S1 and stablizer and smoke suppressor are placed in three-dimensional powder mixer and carry out three-dimensional hybrid, the three-dimensional mixer speed of mainshaft is 5r/min-15r/min, mixing time is 30min-60min, obtained mixture;
S3: extrude: the mixture that step S2 is obtained is extruded through twin screw extruder, and extruder barrel temperature controls at 120 DEG C-160 DEG C, and the speed of mainshaft controls at 600r/min-900r/min, obtained extruded material;
S4: granulation: the extruded material automatic powder granulator granulation obtained by step S3, pelletizing speed 100rpm-200rpm, i.e. obtained antimony system smoke resistance flame resistance master batch;
S5: screening: by the centrifugal vibrating screen classifier screening of antimony system smoke resistance flame resistance master batch circular rotatable dish that step S4 is obtained, the speed of mainshaft controls at 900r/min-1300r/min;
S6: dry: by the antimony system smoke resistance flame resistance master batch drying after screening, pack and get final product.
Beneficial effect of the present invention: (1) by compound stibnide and smoke suppressor zinc molybdate composite, raising flame retardant resistance while improve smoke suppressing effect; (2) three-dimensional powder mixer is adopted better by mixing of materials, dispersiveness, the homogeneity of material can be improved; (3) adopt vibration centrifugal sieve apparatus vibrosieve and centrifugal screen to be divided to unite two into one, simplify technique, improve production efficiency.
[embodiment]
Below in conjunction with embodiment, the present invention is further described, but do not limit the scope of the invention.
Embodiment 1
A kind of antimony system smoke resistance flame resistance master batch, its composition and mass percent are: antimonous oxide 30%, sodium antimonate 30%, Zinic stearas 10%, titanic acid ester 10%, zinc molybdate 20%.
Described antimony system smoke resistance flame resistance master batch, its preparation process is:
S1: compound stibnide modification: compound stibnide and titanic acid ester are dropped into homogenizer and carries out modification, modification temperature 130 DEG C, stir speed (S.S.) 3000r/min, churning time 3.5h, obtained modification compound stibnide;
S2: three-dimensional hybrid: modification compound stibnide obtained for step S1 is placed in three-dimensional powder mixer with Zinic stearas and zinc molybdate and carries out three-dimensional hybrid, the three-dimensional mixer speed of mainshaft is 15r/min, and mixing time is 60min, obtains mixture;
S3: extrude: the mixture that step S2 is obtained is extruded through twin screw extruder, and extruder barrel temperature controls at 140 DEG C, and the speed of mainshaft controls at 900r/min, obtained extruded material;
S4: granulation: the extruded material automatic powder granulator granulation obtained by step S3, pelletizing speed 150rpm, i.e. obtained antimony system smoke resistance flame resistance master batch;
S5: screening: by the centrifugal vibrating screen classifier screening of antimony system smoke resistance flame resistance master batch circular rotatable dish that step S4 is obtained, the speed of mainshaft controls at 1200r/min;
S6: dry: by the antimony system smoke resistance flame resistance master batch drying after screening, pack and get final product.
Embodiment 2
A kind of antimony system smoke resistance flame resistance master batch, its composition and mass percent are: antimonous oxide 40%, sodium antimonate 30%, Zinic stearas 7%, titanic acid ester 8%, zinc molybdate 15%.
Described antimony system smoke resistance flame resistance master batch, its preparation process is:
S1: compound stibnide modification: antimonous oxide and titanic acid ester are dropped into homogenizer and carries out modification, modification temperature 100 DEG C, stir speed (S.S.) 2000r/min, churning time 3.5h, obtained modification compound stibnide;
S2: three-dimensional hybrid: modification compound stibnide obtained for step S1 is placed in three-dimensional powder mixer with Zinic stearas and zinc molybdate and carries out three-dimensional hybrid, the three-dimensional mixer speed of mainshaft is 10r/min, and mixing time is 30min, obtains mixture;
S3: extrude: the mixture that step S2 is obtained is extruded through twin screw extruder, and extruder barrel temperature controls at 120 DEG C, and the speed of mainshaft controls at 800r/min, obtained extruded material;
S4: granulation: the extruded material automatic powder granulator granulation obtained by step S3, pelletizing speed 200rpm, i.e. obtained antimony system smoke resistance flame resistance master batch;
S5: screening: by the centrifugal vibrating screen classifier screening of antimony system smoke resistance flame resistance master batch circular rotatable dish that step S4 is obtained, the speed of mainshaft controls at 900r/min;
S6: dry: by the antimony system smoke resistance flame resistance master batch drying after screening, pack and get final product.
Embodiment 3
A kind of antimony system smoke resistance flame resistance master batch, its composition and mass percent are: antimonous oxide 40%, sodium antimonate 40%, Zinic stearas 5%, titanic acid ester 5%, zinc molybdate 10%.
Described antimony system smoke resistance flame resistance master batch, its preparation process is:
S1: compound stibnide modification: antimonous oxide and titanic acid ester are dropped into homogenizer and carries out modification, modification temperature 140 DEG C, stir speed (S.S.) 4000r/min, churning time 4.5h, obtained modification compound stibnide;
S2: three-dimensional hybrid: modification compound stibnide obtained for step S1 is placed in three-dimensional powder mixer with Zinic stearas and zinc molybdate and carries out three-dimensional hybrid, the three-dimensional mixer speed of mainshaft is 5r/min, and mixing time is 45min, obtains mixture;
S3: extrude: the mixture that step S2 is obtained is extruded through twin screw extruder, and extruder barrel temperature controls at 160 DEG C, and the speed of mainshaft controls at 600r/min, obtained extruded material;
S4: granulation: the extruded material automatic powder granulator granulation obtained by step S3, pelletizing speed 100rpm, i.e. obtained antimony system smoke resistance flame resistance master batch;
S5: screening: by the centrifugal vibrating screen classifier screening of antimony system smoke resistance flame resistance master batch circular rotatable dish that step S4 is obtained, the speed of mainshaft controls at 1300r/min;
S6: dry: by the antimony system smoke resistance flame resistance master batch drying after screening, pack and get final product.
Be applied to respectively in HDPE material by product obtained by above embodiment 1-3, formula composition and mass percent are: HDPE87%, antimony system smoke resistance flame resistance master batch 7%, lubricant 0.35%, dispersion agent 0.25%, according to the performance of national standard test material, the performance test results is as shown in table 1.
The HDPE product performance index of table 1 Application Example antimony system smoke resistance flame resistance master batch
| Performance | Smoke density grade | Limiting oxygen index(LOI)/% | Vertical combustion grade |
| Standard | GB/T 8627-2007 | GB/T 2406-2009 | GB/T 2408-2008 |
| Embodiment 1 product | 49.62 | 27.6 | V-0 |
| Embodiment 2 product | 50.75 | 28.4 | V-0 |
| Embodiment 3 product | 48.18 | 27.9 | V-0 |
Above content can not assert that specific embodiment of the invention is confined to these explanations; for general technical staff of the technical field of the invention; without departing from the inventive concept of the premise; some simple deduction or replace can also be made, all should be considered as belonging to the scope of patent protection that the present invention is determined by submitted to claims.
Claims (6)
1. an antimony system smoke resistance flame resistance master batch, is characterized in that, described master batch comprises the raw material of following mass percent: compound stibnide 60%-80%, stablizer 5%-10%, coupling agent 5%-10%, smoke suppressor 10%-20%.
2. antimony system according to claim 1 smoke resistance flame resistance master batch, is characterized in that, described compound stibnide is the mixture of antimonous oxide, sodium antimonate, antimony peroxide mixture or three between two.
3. antimony system according to claim 1 smoke resistance flame resistance master batch, is characterized in that, described stablizer is Zinic stearas.
4. antimony system according to claim 1 smoke resistance flame resistance master batch, is characterized in that, described coupling agent is titanic acid ester or silane.
5. antimony system according to claim 1 smoke resistance flame resistance master batch, is characterized in that, described smoke suppressor is zinc molybdate.
6. a preparation method for the antimony system smoke resistance flame resistance master batch according to any one of claim 1-5, is characterized in that, comprise the steps:
S1: compound stibnide modification: compound stibnide and coupling agent are dropped into homogenizer and carries out modification, modification temperature 100 DEG C ~ 140 DEG C, stir speed (S.S.) 2000r/min ~ 4000r/min, churning time 3.5h ~ 4.5h, obtained modification compound stibnide;
S2: three-dimensional hybrid: modification compound stibnide obtained for step S1 and stablizer and smoke suppressor are placed in three-dimensional powder mixer and carry out three-dimensional hybrid, the three-dimensional mixer speed of mainshaft is 5r/min-15r/min, mixing time is 30min-60min, obtained mixture;
S3: extrude: the mixture that step S2 is obtained is extruded through twin screw extruder, and extruder barrel temperature controls at 120 DEG C-160 DEG C, and the speed of mainshaft controls at 600r/min-900r/min, obtained extruded material;
S4: granulation: the extruded material automatic powder granulator granulation obtained by step S3, pelletizing speed 100rpm-200rpm, i.e. obtained antimony system smoke resistance flame resistance master batch;
S5: screening: by the centrifugal vibrating screen classifier screening of antimony system smoke resistance flame resistance master batch circular rotatable dish that step S4 is obtained, the speed of mainshaft controls at 900r/min-1300r/min;
S6: dry: by the antimony system smoke resistance flame resistance master batch drying after screening, pack and get final product.
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| CN201510198681.1A CN105111506A (en) | 2015-04-23 | 2015-04-23 | Antimonic smoke-abating flame-retardant master batch and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0953603A2 (en) * | 1998-04-27 | 1999-11-03 | Shin-Etsu Chemical Co., Ltd. | Flame retardant semiconductor encapsulating epoxy resin compositions |
| CN100999334A (en) * | 2007-01-16 | 2007-07-18 | 北京理工大学 | Manufacturing method of antimony trioxide parent particle |
| CN102643453A (en) * | 2012-05-10 | 2012-08-22 | 广西华锑科技有限公司 | Low-smoke type antimonous oxide compound fire retardant and preparation method thereof |
| CN103275387A (en) * | 2013-06-03 | 2013-09-04 | 北京理工大学 | Nano antimonous oxide master batch as well as preparation method and application thereof in halogen-free synergistic flame retardant plastic |
-
2015
- 2015-04-23 CN CN201510198681.1A patent/CN105111506A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0953603A2 (en) * | 1998-04-27 | 1999-11-03 | Shin-Etsu Chemical Co., Ltd. | Flame retardant semiconductor encapsulating epoxy resin compositions |
| CN100999334A (en) * | 2007-01-16 | 2007-07-18 | 北京理工大学 | Manufacturing method of antimony trioxide parent particle |
| CN102643453A (en) * | 2012-05-10 | 2012-08-22 | 广西华锑科技有限公司 | Low-smoke type antimonous oxide compound fire retardant and preparation method thereof |
| CN103275387A (en) * | 2013-06-03 | 2013-09-04 | 北京理工大学 | Nano antimonous oxide master batch as well as preparation method and application thereof in halogen-free synergistic flame retardant plastic |
Non-Patent Citations (1)
| Title |
|---|
| 朱春玲 等: "《工业助剂 复配技术》", 31 July 2009, 化学工业出版社 * |
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