CN105086198A - Antimony-based compounding flame retardant masterbatch for PVC and preparation method thereof - Google Patents
Antimony-based compounding flame retardant masterbatch for PVC and preparation method thereof Download PDFInfo
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- CN105086198A CN105086198A CN201510198675.6A CN201510198675A CN105086198A CN 105086198 A CN105086198 A CN 105086198A CN 201510198675 A CN201510198675 A CN 201510198675A CN 105086198 A CN105086198 A CN 105086198A
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Abstract
The present invention discloses an antimony-based compounding flame retardant masterbatch for PVC and a preparation method thereof, and belongs to the technical field of flame retardant materials. The masterbatch includes the following raw materials by weight: 25-40 parts of antimony trioxide, 13-25 parts of molybdenum trioxide, 8-13 parts of montmorillonite, 3-8 parts of organic tin, 3-6 parts of a coupling agent, and 20 to 35 parts of a carrier PVC resin. The flame retardant masterbatch is prepared from the steps of antimony trioxide surface modification, raw material mixing and granulation. The present invention employs antimony trioxide, molybdenum trioxide and montmorillonite and other environmentally friendly halogen-free flame retardants as a compounding flame retardant system, integrates the advantages of the system in synergistic flame retardant, and smoke suppression performance, improves the flame retardancy and smoke suppression of the compounding complex retardant masterbatch. Addition of the flame retardant masterbatch can greatly improve the limiting oxygen index of the PVC composite material and reduce the amount of smoke, and the flame retardant masterbatch has the characteristics of high flame retardancy, strong smoke suppression, no additive migration, easiness to use, and easy dispersion.
Description
Technical field
The invention belongs to fire retardant material technical field, be specifically related to a kind of PVC antimony system compositional flame-retardant master batch and preparation method thereof.
Background technology
PVC is a kind of polarity non-crystalline type polymkeric substance, is divided into different hard material because of the difference of the polymerization degree.Because PVC itself is containing chlorine element, therefore itself there is certain flame retardant resistance.And free radical and the small molecules such as hydrogenchloride, monomer chlorine containing a great deal of in polymkeric substance, cause PVC and weisspiessglanz to have certain fire-retardant synergistic, after adding weisspiessglanz, can significantly improve its flame retardant properties.But current antimony oxide flame retardant PVC adopts the mode of directly adding weisspiessglanz powder to carry out fire-retardant usually, flame retardant effect is poor, the amount of being fuming is large, and due to disperse uneven and interface welding is bad cause the inorganic powders such as weisspiessglanz to add after to the mechanical impact of PVC matrix material comparatively greatly, seriously govern the application of weisspiessglanz in PVC polymkeric substance.For inorganic powder difficult dispersion and difficult problem merged in resin, in industry, normal employing mode that is composite modified or female granulated processed is improved.
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 (publication number: KR200826501A) discloses a kind of flame-retardant master batch containing polypropylene, eight bromo ether, antimonous oxide, stablizer and antioxidant; Canadian Patent (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%.
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, are a trend of Sb system fire retardant future development.Chinese patent " a kind of manufacture method of antimony trioxide parent particle " (patent No.: ZL200710000830.4) 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 " a kind of antimony trioxide parent particle and preparation method thereof " (patent No.: ZL201110429778.0) 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.And the individual character of master batch, specific aim are comparatively strong, and different resins need adopt the fire-retardant master granule of different substrate materials, be difficult to accomplish general.And the existing antimony system fire-retardant master granule for polyvinyl chloride resin finds no Patents.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, provide a kind of PVC antimony system compositional flame-retardant master batch and preparation method thereof, improve fire-retardant, the smoke suppressing of compound product, save production cost, strengthen the feature of environmental protection etc.
To achieve these goals, present invention employs following technical scheme:
A kind of PVC antimony system compositional flame-retardant master batch, comprises the raw material of following weight ratio:
Antimonous oxide 25 ~ 40 parts;
Molybdic oxide 13 ~ 25 parts;
Polynite 8 ~ 13 parts;
Organotin 3 ~ 8 parts;
Coupling agent 3 ~ 6 parts;
PVC vector resin 20 ~ 35 parts.
Preferably, described coupling agent is the one in titanic acid ester or Aluminate.
Preferably, described PVC vector resin is the good modified PVC soft plastic of toughness.
Preferably, described modified PVC soft plastic, its recipe ingredient is PVC (SG-5) 100 parts, DOP65 part, organotin 3 parts, epoxy soybean oil 0.8 part.
The present invention also provides the preparation method of a kind of PVC antimony system compositional flame-retardant master batch, comprises following steps:
S1: antimonous oxide surface modification: adopt coupling agent to antimonous oxide modifying surface, modification temperature 100 ~ 140 DEG C, stir speed (S.S.) 2000 ~ 4000rpm/min, churning time 3.5 ~ 4.5h;
S2: raw material mixes: modification antimonous oxide, molybdic oxide, polynite, organotin are positioned in frequency-conversion agitator and carry out high-speed mixing, rotating speed 2000 ~ 4000rpm/min, temperature controls at 60 ~ 90 DEG C; Mixing adds PVC vector resin when proceeding to secondary mixing, and carry out low speed mixing, rotating speed is 600 ~ 1200rpm/min, mixing time 5 ~ 10min, not temperature control;
S3: granulation: mixture is proceeded to forcing machine granulation, processing temperature is 130 ~ 160 DEG C.
Preferably, the processing temperature described in step S3 is six sections of temperature control scopes, in principle from first paragraph to the 6th section by 3 ~ 8 DEG C for jump increases progressively, and die temperature is slightly lower than the 5th section of temperature 3 ~ 5 DEG C.
Beneficial effect of the present invention:
(1) have employed molybdic oxide, polynite and the antimonous oxide with flame-retardant smoke inhibition function carries out composite, and the advantage of comprehensive each component, has complementary advantages, and improves fire-retardant, the smoke suppressing of compound product;
(2) aspect chosen by composite raw material, do not choose halogenide and antimonous oxide carries out cooperative flame retardant, but makes full use of the small molecules such as free radical, unconverted monomer residual in substrate resin and carry out cooperative flame retardant, not only cost-saving but also strengthen its feature of environmental protection;
(3) adopt coupling agent to organise after coating modification to principal constituent antimonous oxide inorganic powder and carry out composite mixing with molybdic oxide, polynite and organotin etc. again, the consistency of compound flame retardant and resin is improved on the one hand by organic modification, coated by organising on the other hand, reduce weisspiessglanz surface charge and surface tension, reduce the generation of agglomeration, improve dispersed;
(4) be that carrier carries out grainy treatment to modified antimony system compound flame retardant with PVC, its specific aim and weldability can be improved on the one hand, the dust in PVC material processing can be reduced on the other hand, improve processing environment.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
Embodiment 1
Take respectively in following ratio: polyvinyl chloride resin 35 kilograms, antimonous oxide 40 kilograms (main content more than 99.6%, particle diameter 1.0 μm), molybdic oxide 25 kilograms, polynite 13 kilograms, organotin 8 kilograms, titanate coupling agent 6 kilograms.
S1: antimonous oxide modification: take antimonous oxide and titanic acid ester by above-mentioned amount and drop into homogenizer and carry out modification, modification temperature 140 DEG C, stir speed (S.S.) 4000rpm/min, churning time 3.5h;
S2: antimonous oxide good for modification and other components (except polyvinyl chloride resin particle) are put in variable ratio frequency changer high-speed mixer and carry out high-speed mixing, rotating speed 3000rpm/min, temperature controls at 75 DEG C; The material mixed is proceeded to secondary mixing equipment, adds polyvinyl chloride resin particulate material, carry out low speed mixing, rotating speed is 900rpm/min, mixing time 7min, not temperature control;
S3: mixture is proceeded to forcing machine granulation, processing temperature is 130 ~ 160 DEG C.
Processing temperature described in step S3 is six sections of temperature control scopes, in principle from first paragraph to the 6th section by 8 DEG C for jump increases progressively, and die temperature is slightly lower than the 5th section of temperature 5 DEG C.
Embodiment 2
Take respectively in following ratio: polyvinyl chloride resin 20 kilograms, antimonous oxide 25 kilograms (main content more than 99.6%, particle diameter 1.0 μm), molybdic oxide 13 kilograms, polynite 8 kilograms, organotin 3 kilograms, aluminate coupling agent 3 kilograms.
S1: antimonous oxide modification: take antimonous oxide and titanic acid ester by above-mentioned amount and drop into homogenizer and carry out modification, modification temperature 100 DEG C, stir speed (S.S.) 2000rpm/min, churning time 4.5h.
S2: antimonous oxide good for modification and other components (except polyvinyl chloride resin particle) are put in variable ratio frequency changer high-speed mixer and carry out high-speed mixing, rotating speed 2000rpm/min, temperature controls at 90 DEG C; The material mixed is proceeded to secondary mixing equipment, adds polyvinyl chloride resin particulate material, carry out low speed mixing, rotating speed is 6000rpm/min, mixing time 10min, not temperature control.
S3: mixture is proceeded to forcing machine granulation, processing temperature is 130 ~ 150 DEG C.
Processing temperature described in step S3 is six sections of temperature control scopes, in principle from first paragraph to the 6th section by 3 DEG C for jump increases progressively, and die temperature is slightly lower than the 5th section of temperature 3 DEG C.
Embodiment 3
Take respectively in following ratio: polyvinyl chloride resin 28 kilograms, antimonous oxide 32 kilograms (main content more than 99.6%, particle diameter 1.0 μm), molybdic oxide 19 kilograms, polynite 10 kilograms, organotin 6 kilograms, titanate coupling agent 4 kilograms.
S1: antimonous oxide modification: take antimonous oxide and titanic acid ester by above-mentioned amount and drop into homogenizer and carry out modification, modification temperature 120 DEG C, stir speed (S.S.) 3000rpm/min, churning time 4h.
S2: antimonous oxide good for modification and other components (except polyvinyl chloride resin particle) are put in variable ratio frequency changer high-speed mixer and carry out high-speed mixing, rotating speed 4000rpm/min, temperature controls at 60 DEG C; The material mixed is proceeded to secondary mixing equipment, adds polyvinyl chloride resin particulate material, carry out low speed mixing, rotating speed is 1200rpm/min, mixing time 5min, not temperature control.
S3: mixture is proceeded to forcing machine granulation, processing temperature is 130 ~ 160 DEG C.
Processing temperature described in step S3 is six sections of temperature control scopes, in principle from first paragraph to the 6th section by 6 DEG C for jump increases progressively, and die temperature is slightly lower than the 5th section of temperature 4 DEG C.
Embodiment 4
Take respectively in following ratio: polyvinyl chloride resin 25 kilograms, antimonous oxide 30 kilograms (main content more than 99.6%, particle diameter 1.0 μm), molybdic oxide 17 kilograms, polynite 9 kilograms, organotin 5 kilograms, titanate coupling agent 4 kilograms.
S1: antimonous oxide modification: take antimonous oxide and titanic acid ester by above-mentioned amount and drop into homogenizer and carry out modification, modification temperature 120 DEG C, stir speed (S.S.) 4000rpm/min, churning time 3.5h;
S2: antimonous oxide good for modification and other components (except polyvinyl chloride resin particle) are put in variable ratio frequency changer high-speed mixer and carry out high-speed mixing, rotating speed 3000rpm/min, temperature controls at 75 DEG C; The material mixed is proceeded to secondary mixing equipment, adds polyvinyl chloride resin particulate material, carry out low speed mixing, rotating speed is 900rpm/min, mixing time 8min, not temperature control;
S3: mixture is proceeded to forcing machine granulation, processing temperature is 140 ~ 160 DEG C.
Processing temperature described in step S3 is six sections of temperature control scopes, in principle from first paragraph to the 6th section by 4 DEG C for jump increases progressively, and die temperature is slightly lower than the 5th section of temperature 4 DEG C.
Embodiment 5
Take respectively in following ratio: polyvinyl chloride resin 30 kilograms, antimonous oxide 35 kilograms (main content more than 99.6%, particle diameter 1.0 μm), molybdic oxide 21 kilograms, polynite 10 kilograms, organotin 6 kilograms, titanate coupling agent 5 kilograms.
S1: antimonous oxide modification: take antimonous oxide and titanic acid ester by above-mentioned amount and drop into homogenizer and carry out modification, modification temperature 140 DEG C, stir speed (S.S.) 3000rpm/min, churning time 4h;
S2: antimonous oxide good for modification and other components (except polyvinyl chloride resin particle) are put in variable ratio frequency changer high-speed mixer and carry out high-speed mixing, rotating speed 4000rpm/min, temperature controls at 80 DEG C; The material mixed is proceeded to secondary mixing equipment, adds polyvinyl chloride resin particulate material, carry out low speed mixing, rotating speed is 1000rpm/min, mixing time 8min, not temperature control;
S3: mixture is proceeded to forcing machine granulation, processing temperature is 130 ~ 160 DEG C.
Processing temperature described in step S3 is six sections of temperature control scopes, in principle from first paragraph to the 6th section by 7 DEG C for jump increases progressively, and die temperature is slightly lower than the 5th section of temperature 5 DEG C.
Master batch product obtained by above embodiment 1-3 is applied in PVC material respectively, according to the performance of national standard test material, formula composition and the performance test results as follows:
Table 1 is filled a prescription and is formed and the performance test results
Above content is in conjunction with concrete preferred implementation further description made for the present invention, 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. a PVC antimony system compositional flame-retardant master batch, is characterized in that, comprise the raw material of following weight ratio:
Antimonous oxide 25 ~ 40 parts;
Molybdic oxide 13 ~ 25 parts;
Polynite 8 ~ 13 parts;
Organotin 3 ~ 8 parts;
Coupling agent 3 ~ 6 parts;
PVC vector resin 20 ~ 35 parts.
2. PVC antimony system according to claim 1 compositional flame-retardant master batch, is characterized in that: described coupling agent adopts titanic acid ester or Aluminate.
3. PVC antimony system according to claim 1 compositional flame-retardant master batch, is characterized in that: described PVC vector resin is modified PVC soft plastic.
4. PVC antimony system according to claim 3 compositional flame-retardant master batch, is characterized in that: the recipe ingredient of described modified PVC soft plastic is PVC (SG-5) 100 parts, DOP65 part, organotin 3 parts, epoxy soybean oil 0.8 part.
5. the preparation method for antimony system compositional flame-retardant master batch of the PVC according to any one of claim 1-4, is characterized in that: comprise following steps:
S1: antimonous oxide surface modification: adopt titanic acid ester or Aluminate to antimonous oxide modifying surface, modification temperature 100 ~ 140 DEG C, stir speed (S.S.) 2000 ~ 4000rpm/min, churning time 3.5 ~ 4.5h;
S2: raw material mixes: modification antimonous oxide, molybdic oxide, polynite, organotin are positioned in frequency-conversion agitator and carry out high-speed mixing, rotating speed 2000 ~ 4000rpm/min, temperature controls at 60 ~ 90 DEG C; Proceed to secondary mixing after mixing, add PVC vector resin, carry out low speed mixing, rotating speed is 600 ~ 1200rpm/min, mixing time 5 ~ 10min, not temperature control;
S3: granulation: mixture is proceeded to forcing machine granulation, processing temperature is 130 ~ 160 DEG C.
6. the preparation method of PVC antimony system according to claim 5 compositional flame-retardant master batch, is characterized in that: the processing temperature in described step S3 is six sections of temperature control scopes, from first paragraph to the 6th section by 3 ~ 8 DEG C for jump increases progressively.
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| CN106750590A (en) * | 2016-12-07 | 2017-05-31 | 郑州丽福爱生物技术有限公司 | A kind of Automobile interior decoration environmental-friendalloy material and preparation method thereof |
| CN107663348A (en) * | 2017-09-23 | 2018-02-06 | 镇江市太浪新材料科技有限公司 | One kind building special-purpose anti-flaming filler |
| CN107746552A (en) * | 2017-11-16 | 2018-03-02 | 广西华锑科技有限公司 | A kind of PBT high tenacity antimony oxide flame retardant master batches |
| CN107987480A (en) * | 2017-12-14 | 2018-05-04 | 广东机电职业技术学院 | A kind of flame retardant type epoxy/polyvinyl chloride composite foam material and its preparation method and application |
| CN113130127A (en) * | 2021-04-16 | 2021-07-16 | 江西富鸿金属有限公司 | Fire-resistant fire-retardant 5G tinned wire for communication |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113130127A (en) * | 2021-04-16 | 2021-07-16 | 江西富鸿金属有限公司 | Fire-resistant fire-retardant 5G tinned wire for communication |
| CN113130127B (en) * | 2021-04-16 | 2022-08-23 | 江西富鸿金属有限公司 | Fire-resistant fire-retardant 5G tinned wire for communication |
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Application publication date: 20151125 |