CN102643453B - Low-smoke type antimonous oxide compound fire retardant and preparation method thereof - Google Patents
Low-smoke type antimonous oxide compound fire retardant and preparation method thereof Download PDFInfo
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- CN102643453B CN102643453B CN 201210143074 CN201210143074A CN102643453B CN 102643453 B CN102643453 B CN 102643453B CN 201210143074 CN201210143074 CN 201210143074 CN 201210143074 A CN201210143074 A CN 201210143074A CN 102643453 B CN102643453 B CN 102643453B
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Abstract
The invention discloses a low-smoke type antimonous oxide compound fire retardant and a preparation method thereof. The fire retardant comprises components, by weight: 30-60 parts of antimonous oxide, 10-40 parts of hydrotalcite, 10-40 parts of zinc borate, 5-10 parts of montmorillonite and 1-3 parts of coupling reagents. The coupling reagent is selected from one of a titanate coupling agent and an aluminate coupling agent. The fire retardant has good fire retarding and smoke suppression performance and can reduce polymer mechanical property reduction caused by adding the compound fire retardant.
Description
Technical field
The invention belongs to chemical field, relate to a kind of fire retardant, related in particular to a kind of low cigarette type antimonous oxide compound flame retardant and preparation method thereof.
Background technology
Studies show that, in fire, cigarette is to produce at first and the most lethal factor.According to expert statistics, in the people because of fire failure death, be because smog and poisonous gas that the macromolecular material burning is emitted are choked to death the people more than 80% in the world, be not naked light burns body and dies.Macromolecular material produces more smog and toxic gas when burning, this smog gas is factor the most dangerous in fire, because what their velocity of diffusion much larger than the velocity of diffusion of flame, had hindered people in fire withdraws and puts out work, thereby makes lives and properties suffer heavy losses.Therefore in fire-retardant research field, fire-retardant is two eternal topics with pressing down the cigarette problem.
Plastics are to use all a kind of polymer materials very widely at aspects such as household electrical appliances instrument, electronics, automobiles.Because plastics have inflammable characteristics, so usually need to carry out fire-retardant finish to it, wherein the most frequently used flame-retardant system is halogen sb system and inorganic fire-retarded system.Output is maximum in the world at present, and the organic fire-retardant that is most widely used remains halogenated flame retardant, and wherein the bromine Sb system fire retardant occupies sizable ratio.Number be that the fire retardant of putting down in writing in 200910182753.8 disclosed flame-retardant synthetic papers is selected antimonous oxide, tetrabromo-bisphenol, zinc borate, hexabromobenzene, hexabromocyclododecane, tricresyl phosphate (2 as Chinese patent application, 3-two chloropropyls) mixture of one or more in ester, two (2,3-dibromopropyl) fumarate; And for example Chinese patent application number is that in 201010273483.4 disclosed a kind of flame-retardant ACS resins and manufacture method thereof, component comprises ACS resin lOO part, bromide fire retardant lO-20 part, antimonous oxide 3-8 part, stablizer l-4 part, toughner 5-15 part, lubricant 0.5-2 part, oxidation inhibitor 0.5-1.5 part.Yet, studies show that the halogen Sb system fire retardant in use have the amount of being fuming large, produce toxic gas, can produce the shortcoming such as glow, so except fire retardant non-halogenated, need adopt the Halogen macromolecule polymer material and add smoke suppressor and solve the problem of being fuming.But all there is certain negative impact in the now widely used cigarette additive flame retardant that presses down to the performances such as machinery, physics, mechanics and processing of superpolymer; therefore conventional oxidation antimony flame retardant products is optimized upgrading; make its have concurrently fire-retardant, press down hood; suppress the generation of cigarette and toxic gas; simultaneously do not affect the polymer machinery performance, meeting again environmental protection requirement has become the present study hotspot of Sb system fire retardant.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of low cigarette type antimonous oxide compound flame retardant and preparation method thereof is provided.
To achieve these goals, the present invention has adopted following technical scheme: a kind of low cigarette type antimonous oxide compound flame retardant, it is characterized in that: the component of fire retardant comprises antimonous oxide, hydrotalcite, zinc borate, polynite and coupling agent, and the parts by weight of each component are:
The parts by weight of each component of described fire retardant are preferably:
Described polynite is organic modification montmonrillonite.Organic modification montmonrillonite can be bought on market and obtain.
Described coupling agent is selected from a kind of in titanate coupling agent, aluminate coupling agent.
The preparation method of above-mentioned low cigarette type antimonous oxide compound flame retardant comprises the following steps successively:
(1) parts by weight according to each component of fire retardant take antimonous oxide, hydrotalcite, zinc borate, polynite and coupling agent;
(2) ready each component is put in the high-speed mixer with water cooling function mixed, mixing time is 30～60min, and controls temperature of charge in mixing machine lower than 100 ℃ in mixing process;
(3) mass transport after mixing is tentatively sieved to vibratory screening apparatus, and the mass transport that then will tentatively sieve to centrifugal screen further sieves;
(4) will pack from the material that centrifugal screen sieves out, namely get the fire retardant finished product.
The parts by weight of each component of fire retardant described in the preparation method are:
The parts by weight of each component of fire retardant described in the preparation method are preferably:
Polynite described in the preparation method is organic modification montmonrillonite.Organic modification montmonrillonite is to adopt the commercially available prod, can buy to obtain on market.
Coupling agent described in the preparation method is selected from a kind of in titanate coupling agent, aluminate coupling agent.
The vibratory screening apparatus that uses in preparation method of the present invention can adopt the vibratory screening apparatus of zxs series, is the vibratory screening apparatus of zxs1000 type as model, its motor 1.5kw, rotating speed: 1100rpm; It is the centrifugal screen of kemutec k650 type that centrifugal screen can adopt model.
Antimonous oxide is the fire retardant of using the earliest, is applicable to epoxy resin, urethane, chloroprene rubber, polystyrene, polyvinyl chloride, polyester etc., and when using separately, consumption wants large, and flame retardant effect is poor, but composite rear flame retardant effect obviously improves.
Hydrotalcite-based compound (LDHs) is the novel inorganic functional materials that a class has laminate structure.LDHs is when being heated, and its water of constitution laminated sheet hydroxyl and interlayer ion are with water and CO
2Form deviate from, play and reduce combustion gases concentration, intercept O
2Fire retardation; The water of constitution of LDHs, laminate hydroxyl and interlayer ion break away from laminate in different temperature, thereby can (200～800 ℃) discharge fire retardant matter in lower scope.In fire-retardant process, caloric receptivity is large, and the high temperature that produces when being conducive to reduce burning can be used as the high smoke inhibition fire retardant of Halogen, is widely used in the fields such as plastics, rubber, coating.
Zinc borate is one of fire retardant that uses the earliest, is also important inorganic combustion inhibitor, and its characteristics are Heat stability is good, toxicity is low, eliminates smoke, and is composite respond well with other fire retardant, obviously reduce the material combustion smoke density after adding, with the Halogen based flame retardant, the composite successful of antimonous oxide.
Polynite has good dispersing property, can widespread use macromolecular material industry as the additive of nanometer polymer macromolecular material, improve shock resistance, antifatigue, dimensional stability and gas barrier property etc., thereby play the effect that strengthens polymkeric substance comprehensive physical performance, improve simultaneously the materiel machining performance.
Advantage of the present invention:
1. adopt and have the zinc borate, hydrotalcite and the weisspiessglanz that press down hood and carry out composite.Zinc borate in composite product, hydrotalcite have good fire-retardant and smoke suppressing.
2. adopt organo montmorillonite to participate in composite, organo montmorillonite can well promote the abundant mixing of composite material because it has layered nano-structure.In addition because polynite has reinforcing function to the mechanical property of polymkeric substance, to reduce the adding of this component and add the mechanical properties of polymer that causes after compound flame retardant and reduce.
3. add coupling agent to carry out organic modification in all material mixing processes, improve the consistency of composite product and organic polymer, can further reduce mechanical properties of polymer and reduce.
Embodiment
The present invention is further described below in conjunction with embodiment, but do not limit protection scope of the present invention.
Embodiment 1:
(1) take low cigarette type antimonous oxide compound flame retardant raw material: 30 kilograms of antimonous oxides (main content is more than 99.6%), 10 kilograms of hydrotalcites, 10 kilograms of zinc borates, 5 kilograms of organic modification montmonrillonites, 1 kilogram of titanate coupling agent;
(2) above-mentioned ready each component is put in the high-speed mixer with water cooling function mixed, mixing time is 30min, and controls temperature of charge in mixing machine lower than 100 ℃ in mixing process;
(3) mass transport after mixing is tentatively sieved to vibratory screening apparatus, removes the material of macrobead or caking, and the mass transport that then will tentatively sieve to centrifugal screen carries out regrading; Vibratory screening apparatus model: zxs1000 type, motor 1.5kw, rotating speed: 1100rpm; Centrifugal screen model: kemutec k650 type;
(4) will pack from mass transport to the pack-thread that centrifugal screen sieves out, namely get low cigarette type antimonous oxide compound flame retardant finished product.
Embodiment 2:
(1) take low cigarette type antimonous oxide compound flame retardant raw material: 60 kilograms of antimonous oxides (main content is more than 99.6%), 40 kilograms of hydrotalcites, 40 kilograms of zinc borates, 10 kilograms of organic modification montmonrillonites, 3 kilograms of aluminate coupling agents;
(2) above-mentioned ready each component is put in the high-speed mixer with water cooling function mixed, mixing time is 35min, and controls temperature of charge in mixing machine lower than 100 ℃ in mixing process;
(3) mass transport after mixing is tentatively sieved to vibratory screening apparatus, removes the material of macrobead or caking, and the mass transport that then will tentatively sieve to centrifugal screen carries out regrading; Vibratory screening apparatus model: zxs1000 type, motor 1.5kw, rotating speed: 1100rpm; Centrifugal screen model: kemutec k650 type;
(4) will pack from mass transport to the pack-thread that centrifugal screen sieves out, namely get low cigarette type antimonous oxide compound flame retardant finished product.
Embodiment 3:
(1) take low cigarette type antimonous oxide compound flame retardant raw material: 40 kilograms of antimonous oxides (main content is more than 99.6%), 15 kilograms of hydrotalcites, 15 kilograms of zinc borates, 6 kilograms of organic modification montmonrillonites, 1 kilogram of titanate coupling agent;
(2) above-mentioned ready each component is put in the high-speed mixer with water cooling function mixed, mixing time is 55min, and controls temperature of charge in mixing machine lower than 100 ℃ in mixing process;
(3) mass transport after mixing is tentatively sieved to vibratory screening apparatus, removes the material of macrobead or caking, and the mass transport that then will tentatively sieve to centrifugal screen carries out regrading; Vibratory screening apparatus model: zxs1000 type, motor 1.5kw, rotating speed: 1100rpm; Centrifugal screen model: kemutec k650 type;
(4) will pack from mass transport to the pack-thread that centrifugal screen sieves out, namely get low cigarette type antimonous oxide compound flame retardant finished product.
Embodiment 4:
(1) take low cigarette type antimonous oxide compound flame retardant raw material: 50 kilograms of antimonous oxides (main content is more than 99.6%), 35 kilograms of hydrotalcites, 30 kilograms of zinc borates, 8 kilograms of organic modification montmonrillonites, 2 kilograms of titanate coupling agents;
(2) above-mentioned ready each component is put in the high-speed mixer with water cooling function mixed, mixing time is 50min, and controls temperature of charge in mixing machine lower than 100 ℃ in mixing process;
(3) mass transport after mixing is tentatively sieved to vibratory screening apparatus, removes the material of macrobead or caking, and the mass transport that then will tentatively sieve to centrifugal screen carries out regrading; Vibratory screening apparatus model: zxs1000 type, motor 1.5kw, rotating speed: 1100rpm; Centrifugal screen model: kemutec k650 type;
(4) will pack from mass transport to the pack-thread that centrifugal screen sieves out, namely get low cigarette type antimonous oxide compound flame retardant finished product.
Embodiment 5:
(1) take low cigarette type antimonous oxide compound flame retardant raw material: 45 kilograms of antimonous oxides (main content is more than 99.6%), 20 kilograms of hydrotalcites, 20 kilograms of zinc borates, 7 kilograms of organic modification montmonrillonites, 1.5 kilograms of aluminate coupling agents;
(2) above-mentioned ready each component is put in the high-speed mixer with water cooling function mixed, mixing time is 45min, and controls temperature of charge in mixing machine lower than 100 ℃ in mixing process;
(3) mass transport after mixing is tentatively sieved to vibratory screening apparatus, removes the material of macrobead or caking, and the mass transport that then will tentatively sieve to centrifugal screen carries out regrading; Vibratory screening apparatus model: zxs1000 type, motor 1.5kw, rotating speed: 1100rpm; Centrifugal screen model: kemutec k650 type;
(4) will pack from mass transport to the pack-thread that centrifugal screen sieves out, namely get low cigarette type antimonous oxide compound flame retardant finished product.
Embodiment 6:
(1) take low cigarette type antimonous oxide compound flame retardant raw material: 44 kilograms of antimonous oxides (main content is more than 99.6%), 18 kilograms of hydrotalcites, 22 kilograms of zinc borates, 6.5 kilograms of organic modification montmonrillonites, 1.5 kilograms of titanate coupling agents;
(2) above-mentioned ready each component is put in the high-speed mixer with water cooling function mixed, mixing time is 60min, and controls temperature of charge in mixing machine lower than 100 ℃ in mixing process;
(3) mass transport after mixing is tentatively sieved to vibratory screening apparatus, removes the material of macrobead or caking, and the mass transport that then will tentatively sieve to centrifugal screen carries out regrading; Vibratory screening apparatus model: zxs1000 type, motor 1.5kw, rotating speed: 1100rpm; Centrifugal screen model: kemutec k650 type;
(4) will pack from mass transport to the pack-thread that centrifugal screen sieves out, namely get low cigarette type antimonous oxide compound flame retardant finished product.
Application example
The prepared product of above embodiment 1～3 is applied to respectively in PVC, PP material, and according to the performance of national standard test material, formula composition and the performance test results are as follows:
Table 1:PVC formula forms and the performance test results
| Formula | 1# | 2# | 3# | Remarks |
| PVC（SG-3） | 100 | 100 | 100 | |
| CaCO 3 | 20 | 20 | 20 | |
| DOP | 60 | 60 | 60 | |
| Calcium/zinc stabilizer | 4 | 4 | 4 | |
| Embodiment 1 product | 8 | |||
| Embodiment 2 products | 8 | |||
| Embodiment 3 products | 8 | |||
| Performance | ||||
| Smoke density grade | 60.22 | 62.36 | 66.87 | GB/T 8627-2007 |
| Limiting oxygen index(LOI)/% | 31.8 | 32.3 | 33.6 | GB/T 2406-2009 |
| The vertical combustion grade | V-0 | V-0 | V-0 | GB/T 2408-2008 |
Table 2:PP formula forms and the performance test results
| Formula | 1# | 2# | 3# | Remarks |
| PP | 100 | 100 | 100 | |
| TDE | 24 | 24 | 24 | |
| Embodiment 1 product | 8 | |||
| Embodiment 2 products | 8 | |||
| Embodiment 3 products | 8 | |||
| Performance | ||||
| Smoke density grade | 52.62 | 54.35 | 55.67 | GB/T 8627-2007 |
| Limiting oxygen index(LOI)/% | 20.7 | 21.5 | 22.2 | GB/T 2406-2009 |
| The vertical combustion grade | V-0 | V-0 | V-0 | GB/T 2408-2008 |
| Tensile strength/MPa | 1321.92 | 1279.93 | 1247.46 | GB/T1040-1992 |
| Flexural strength/MPa | 40.62 | 40.2 0 | 39.74 | GB/T9341-2000 |
Claims (6)
1. one kind low cigarette type antimonous oxide compound flame retardant, it is characterized in that: the component of fire retardant comprises antimonous oxide, hydrotalcite, zinc borate, polynite and coupling agent, the parts by weight of each component are:
30～60 parts of antimonous oxides,
10～40 parts of hydrotalcites,
10～40 parts of zinc borates,
5～10 parts of polynites,
1～3 part of coupling agent.
2. low cigarette type antimonous oxide compound flame retardant according to claim 1, it is characterized in that: the parts by weight of each component of described fire retardant are:
40～50 parts of antimonous oxides,
15～35 parts of hydrotalcites,
15～30 parts of zinc borates,
6～8 parts of polynites,
1～2 part of coupling agent.
3. arbitrary described low cigarette type antimonous oxide compound flame retardant according to claim 1 and 2, it is characterized in that: described polynite is organic modification montmonrillonite.
4. arbitrary described low cigarette type antimonous oxide compound flame retardant according to claim 1 and 2 is characterized in that: described coupling agent is selected from a kind of in titanate coupling agent, aluminate coupling agent.
5. the preparation method of described low cigarette type antimonous oxide compound flame retardant as arbitrary in claim 1-4, it is characterized in that: this preparation method comprises the following steps successively:
(1) parts by weight according to each component of fire retardant take antimonous oxide, hydrotalcite, zinc borate, polynite and coupling agent;
(2) ready each component is put in the high-speed mixer with water cooling function mixed, mixing time is 30～60min, and controls temperature of charge in mixing machine lower than 100 ℃ in mixing process;
(3) mass transport after mixing is tentatively sieved to vibratory screening apparatus, and the mass transport that then will tentatively sieve to centrifugal screen further sieves;
(4) will pack from the material that centrifugal screen sieves out, namely get the fire retardant finished product.
6. the preparation method of low cigarette type antimonous oxide compound flame retardant according to claim 5, it is characterized in that: the parts by weight of described each component of fire retardant are:
40～50 parts of antimonous oxides,
15～35 parts of hydrotalcites,
16～29 parts of zinc borates,
6～8 parts of polynites,
1～2 part of coupling agent.
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| CN103849005A (en) * | 2012-12-04 | 2014-06-11 | 深圳市联合鑫科技有限公司 | Efficient and environment-friendly flame retardant |
| CN103540098A (en) * | 2013-09-11 | 2014-01-29 | 青岛颐世保塑料有限公司 | Flame-retardant polyformaldehyde material |
| CN104194219A (en) * | 2014-09-01 | 2014-12-10 | 安徽太平洋电缆股份有限公司 | Low-smoke low-halogen flame-retardant PVC cable material and preparation method thereof |
| CN105315493A (en) * | 2015-04-23 | 2016-02-10 | 广西华锑科技有限公司 | Low-smoke environment-friendly type antimony system compound flame retardant and preparation method thereof |
| CN105086198A (en) * | 2015-04-23 | 2015-11-25 | 广西华锑科技有限公司 | Antimony-based compounding flame retardant masterbatch for PVC and preparation method thereof |
| CN105111506A (en) * | 2015-04-23 | 2015-12-02 | 广西华锑科技有限公司 | Antimonic smoke-abating flame-retardant master batch and preparation method thereof |
| CN105111505A (en) * | 2015-04-23 | 2015-12-02 | 广西华锑科技有限公司 | Antimonic compound flame-retardant master batch and preparation method thereof |
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| CN106519496B (en) * | 2016-11-02 | 2018-08-10 | 华北科技学院 | A kind of compound PVC flame retardant, fire proofing and preparation method |
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| CN107286514A (en) * | 2017-07-28 | 2017-10-24 | 张乃斌 | A kind of special antimony base fire retarding synergists of PVC |
| CN109049218A (en) * | 2018-07-27 | 2018-12-21 | 天峨县平昌生态农业有限公司 | A kind of composite flame-retardant agent being used to prepare glued board |
| CN109608695A (en) * | 2018-10-17 | 2019-04-12 | 张古权 | A kind of preparation method of modified oxidized antimony fire retardant |
| CN115975309B (en) * | 2023-02-01 | 2024-07-02 | 包头稀土研究院 | Flame-retardant composition, preparation method and application thereof, PVC resin composition and preparation method thereof |
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