CN105037804A - Preparation method of synergetic silicon-magnesium composite fire retardant with core-shell structure - Google Patents
Preparation method of synergetic silicon-magnesium composite fire retardant with core-shell structure Download PDFInfo
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Abstract
The invention belongs to the technical field of inorganic functional materials, and provides a preparation method of a synergetic silicon-magnesium composite fire retardant with a core-shell structure. The provided high efficient composite fire retardant with a core-shell structure can be obtained by depositing and coating silicon dioxide with a special nano structure on the surface of a magnesium fire retardant with a size of 1000 to 8000 meshes, and has the advantages of large specific surface area, and stable structure and property. The preparation method has the advantages of simple process, convenient operation, low cost, and easily-controlled technical conditions, moreover, the size of the composite fire retardant particles is adjustable, the nano structure of the surface of the fire retardant particles is controllable, and the mechanical properties and fire retardant performance of the polymer composite material can be prominently improved even if the filling amount is low. When the filling amount is less than 60 wt%, the fire retardant is applied to EVA, the tensile strength is larger than 10.00 MPa, the break elongation is more than 150%, and the national requirements on cable sheath materials can be met. When the filling amount is 50 wt%, EVA can reach the fire retardant UL94-V0 grade, and at the same time, the heat releasing speed of EVA composite material is greatly reduced at the same time.
Description
Technical field
The invention belongs to inorganic functional material technical field, be related specifically to a kind of preparation method of nucleocapsid synergistic type silicon magnesium compound fire retardant.
Background technology
Magnesium flame retardant comprises brucite, magnesium hydroxide, magnesium basic carbonate, alkali magnesium sulfate etc., as eco-friendly " green " halogen-free flame retardants and smoke suppressant, has extensive use in rubber plastic field.But magnesium flame retardant when being used alone flame retarding efficiency lower, need higher loading level could meet the flame-retardancy requirements of polymer materials.High filler loading capacity not only reduces Drawing abillity, also makes polymer materials mechanical property sharply worsen.In actual applications in order to reduce flame resistant filler amount, improve the flame retarding efficiency of magnesium flame retardant, often itself and synergist are used jointly, the cooperative flame retardant systems such as such as magnesium system/phosphorus system, magnesium system/nitrogen phosphorus system, magnesium system/expanded graphite, magnesium system/silicon system, magnesium system/zinc borate, magnesium system/carbon nanotube, magnesium system/stannate, magnesium system/polynite.But, these cooperative flame retardant systems are mostly that simple physical mixed uses, its synergy just simply add and, respective defect still exists, in addition, because the interphase interaction of magnesium flame retardant and synergist is more weak, in polymer processing and combustion processes, there will be the phenomenon of each self enrichment, composite materials property is had a negative impact.
Therefore, on the cooperative flame retardant system basis of magnesium system/silicon system physical mixed, in order to make up their respective deficiencies further, reduce the loading level of fire retardant, improve the flame retarding efficiency of fire retardant, the invention provides one with magnesium flame retardant for core, silicon is the preparation method of " nucleocapsid " structure synergistic type silicon magnesium compound fire retardant of shell, not only cost is low, simple to operate, the interphase interaction that simultaneously obtained flame-retardant agent particle has fire retardant and synergist is strong, , material mechanical performance and flame retardant resistance all comparatively high, the requirement of country for cable sheath material is met for EVA plastics.
Summary of the invention
The present invention proposes a kind of preparation method of nucleocapsid synergistic type silicon magnesium compound fire retardant, simple fills the problems such as the low and poor mechanical property of polymer composite flame retarding efficiency that magnesium flame retardant or magnesium system/silicon system physical mixed fire retardant bring to solve.
Technical scheme of the present invention is: with micron order magnesium flame retardant for raw material, slurries are prepared into subsequently to adding a certain proportion of solvent dispersion in reactor, again siliceous alcoholic solution is added drop-wise in reactor by certain formula rate and stirs, make mixing of materials evenly and complete reaction, again through filtering and drying process, obtain nucleocapsid structure synergistic type silicon magnesium compound fire retardant product.Its technical characteristic is that the silicon source of the kind of magnesium flame retardant core, grain graininess, solvent composition, slurry solid-to-liquid ratio, silicon-series five-retardant shell is selected, concentration and formula as follows:
A preparation method for nucleocapsid synergistic type silicon magnesium compound fire retardant, step is as follows:
Step 1: magnesium flame retardant and solvent are made slurry by the given quality of solid-liquid than mix and blend, stirring velocity is 100 ~ 1200r/min, and temperature is room temperature, stirs 10 ~ 100min;
Step 2: continue maintenance 100 ~ 1200r/min stirring velocity, and add a certain amount of silicon source solution, generates silicon-series five-retardant;
Step 3: maintain 100 ~ 1200r/min stirring velocity, and to add silicon source mol ratio be the water of 1 ~ 8, temperature of reaction is room temperature, keeps successive reaction 6 ~ 12h;
Step 4: filter and use water and industrial alcohol to replace washing leaching cake, namely obtains nucleocapsid synergistic type silicon magnesium compound fire retardant after drying;
Described magnesium flame retardant is one or more mixing in brucite, magnesium hydroxide, magnesium basic carbonate, alkali magnesium sulfate, and granularity is 1000 ~ 8000 orders;
Described solvent is one or more mixing in water, C1 ~ C4 alcohol;
Described magnesium flame retardant and the solid-liquid mass ratio of solvent are 1:1 ~ 10;
Water glass, 3-(methacryloxypropyl) propyl trimethoxy silicane, 3-TSL 8330 are selected in silicon source, one or more mixing in polyoxyethylene glycol trimethoxy silicon propyl ether, aminopropyltriethoxy diethoxy silane, tetraethoxy, positive silicic acid propyl ester, silicic acid trimethyl, the mass concentration of siliceous solution is 1.0% ~ 25%; Amount of substance between magnesium flame retardant and silicon-series five-retardant is than being 100:3 ~ 40.
Beneficial effect of the present invention: magnesium flame retardant core surface deposition nano silicon shell significantly can promote the specific surface area of composite flame-retardant agent particle and improve the consistency of magnesium flame retardant and plastics, thus make it be applied to when polymkeric substance prepares matrix material significantly to promote the interaction with polymeric matrix, and then improve composite materials property, loading level is less than tensile strength when 60wt% is applied to EVA and is all greater than 10.00MPa, elongation at break is all greater than 150%, meets the requirement of country for cable sheath material; Simultaneously, because silicon system synergist is tied to magnesium based flameproofing particle surface, avoid the respective enrichment phenomenon in polymeric matrix in processing or combustion processes, the two is made to produce strong cooperative flame retardant effect, loading level 50wt% can meet fire-retardant UL94-V0 rank, EVA matrix material heat release rate can be made to decline greatly simultaneously.
Embodiment
Specific embodiments of the invention are described in detail below in conjunction with technical scheme.
Embodiment 1
Get 5000 order magnesium hydrate powder 10kg and be placed in reactor, add 20L ethanol and make slurry, the 30L ethanolic soln got again containing 1.8kg tetraethoxy keeps 100r/min mixing speed disposable adding in reactor, add 1L deionized water subsequently, sustained reaction 10h, by product filtration washing after having reacted, fluffy composite flame-retardant agent product after drying, can be obtained.By product application in EVA plastics, loading level is less than tensile strength when 60wt% is applied to EVA and is all greater than 10.00MPa, and elongation at break is all greater than 150%, meets the requirement of country for cable sheath material; Loading level 50wt% meets fire-retardant UL94-V0 rank.Its performance is better than equal loading level magnesium hydroxide and the simple mixed type fire retardant of silicon-dioxide.
The limiting oxygen index(LOI) of table 1 silicon magnesium compound fire retardant and the test of UL94 vertical combustion
Embodiment 2
Get 6000 order magnesium basic carbonate powder 12kg and be placed in reactor, add 25L Methanol form slurry, the 20L methanol solution got again containing 2.0kg methyl silicate keeps 150r/min to stir disposable adding in reactor, add 1.2L deionized water subsequently, sustained reaction 6h, by product filtration washing after having reacted, can obtain fluffy composite flame-retardant agent product after drying.By product application in EVA plastics, loading level is less than tensile strength when 60wt% is applied to EVA and is all greater than 10.00MPa, and elongation at break is all greater than 150%, meets the requirement of country for cable sheath material; Loading level 50wt% meets fire-retardant UL94-V0 rank.
Embodiment 3
Get 2500 order brucite powder 10kg and be placed in reactor, add 30L propyl alcohol and make slurry, get the 20L propanol solution being dissolved with 1.8kg positive silicic acid propyl ester again and keep 250r/min mixing speed disposable adding in reactor, add 0.8L deionized water subsequently, sustained reaction 12h; By product filtration washing after having reacted, fluffy composite flame-retardant agent product after drying, can be obtained.By product application in EVA plastics, loading level is less than tensile strength when 60wt% is applied to EVA and is all greater than 10.00MPa, and elongation at break is all greater than 150%, meets the requirement of country for cable sheath material; Loading level 48wt% meets fire-retardant UL94-V0 rank.
Claims (1)
1. a preparation method for nucleocapsid synergistic type silicon magnesium compound fire retardant, it is characterized in that, step is as follows:
Step 1: magnesium flame retardant and solvent are made slurry by the given quality of solid-liquid than mix and blend, stirring velocity is 100 ~ 1200r/min, and temperature is room temperature, stirs 10 ~ 100min;
Step 2: continue maintenance 100 ~ 1200r/min stirring velocity, and add a certain amount of silicon source solution, generates silicon-series five-retardant;
Step 3: maintain 100 ~ 1200r/min stirring velocity, and to add silicon source mol ratio be the water of 1 ~ 8, temperature of reaction is room temperature, keeps successive reaction 6 ~ 12h;
Step 4: filter and use water and industrial alcohol to replace washing leaching cake, namely obtains nucleocapsid synergistic type silicon magnesium compound fire retardant after drying;
Described magnesium flame retardant is one or more mixing in brucite, magnesium hydroxide, magnesium basic carbonate, alkali magnesium sulfate, and granularity is 1000 ~ 8000 orders;
Described solvent is one or more mixing in water, C1 ~ C4 alcohol;
Described magnesium flame retardant and the solid-liquid mass ratio of solvent are 1:1 ~ 10;
Water glass, 3-(methacryloxypropyl) propyl trimethoxy silicane, 3-TSL 8330 are selected in silicon source, one or more mixing in polyoxyethylene glycol trimethoxy silicon propyl ether, aminopropyltriethoxy diethoxy silane, tetraethoxy, positive silicic acid propyl ester, silicic acid trimethyl, the mass concentration of siliceous solution is 1.0% ~ 25%; Amount of substance between magnesium flame retardant and silicon-series five-retardant is than being 100:3 ~ 40.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105304185A (en) * | 2015-11-17 | 2016-02-03 | 宁波云飚电器科技有限公司 | Novel cable with functional layer |
| CN109161055A (en) * | 2018-08-17 | 2019-01-08 | 扬州新奇特电缆材料有限公司 | A kind of preparation method of wire and cable nuclear shell structure nano simaldrate composite flame-retardant agent |
| CN110387066A (en) * | 2019-07-17 | 2019-10-29 | 北京化工大学 | A kind of preparation of microencapsulation modified flame-retardant agent |
| CN110483895A (en) * | 2019-09-09 | 2019-11-22 | 王良仁 | A kind of fire retardant plastic mastre batch and preparation method for cable filling rope |
| CN110903513A (en) * | 2019-12-03 | 2020-03-24 | 苏州诺博恩新材料科技有限公司 | Silicon dioxide core-shell antibacterial flame retardant and preparation method thereof |
| CN111185149A (en) * | 2018-11-15 | 2020-05-22 | 中国科学院大连化学物理研究所 | MgO @ SiO with core-shell structure2Catalyst, preparation method and application thereof |
| CN112574497A (en) * | 2020-12-11 | 2021-03-30 | 南通勘察设计有限公司 | Flame-retardant sound-insulation shock-absorption material for floor and preparation method thereof |
| CN113637228A (en) * | 2021-08-12 | 2021-11-12 | 广东金发科技有限公司 | Intumescent brucite-based composite flame retardant and preparation method and application thereof |
| CN115746570A (en) * | 2022-12-07 | 2023-03-07 | 华力通线缆股份有限公司 | Ceramic fire-resistant sheath material and medium-voltage fire-resistant cable |
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| CN1288859A (en) * | 2000-11-03 | 2001-03-28 | 清华大学 | Preparation of high temperature resisting electrothermal insulating magnesia material |
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| CN1288859A (en) * | 2000-11-03 | 2001-03-28 | 清华大学 | Preparation of high temperature resisting electrothermal insulating magnesia material |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105304185A (en) * | 2015-11-17 | 2016-02-03 | 宁波云飚电器科技有限公司 | Novel cable with functional layer |
| CN109161055A (en) * | 2018-08-17 | 2019-01-08 | 扬州新奇特电缆材料有限公司 | A kind of preparation method of wire and cable nuclear shell structure nano simaldrate composite flame-retardant agent |
| CN111185149A (en) * | 2018-11-15 | 2020-05-22 | 中国科学院大连化学物理研究所 | MgO @ SiO with core-shell structure2Catalyst, preparation method and application thereof |
| CN110387066A (en) * | 2019-07-17 | 2019-10-29 | 北京化工大学 | A kind of preparation of microencapsulation modified flame-retardant agent |
| CN110483895A (en) * | 2019-09-09 | 2019-11-22 | 王良仁 | A kind of fire retardant plastic mastre batch and preparation method for cable filling rope |
| CN110903513A (en) * | 2019-12-03 | 2020-03-24 | 苏州诺博恩新材料科技有限公司 | Silicon dioxide core-shell antibacterial flame retardant and preparation method thereof |
| CN112574497A (en) * | 2020-12-11 | 2021-03-30 | 南通勘察设计有限公司 | Flame-retardant sound-insulation shock-absorption material for floor and preparation method thereof |
| CN113637228A (en) * | 2021-08-12 | 2021-11-12 | 广东金发科技有限公司 | Intumescent brucite-based composite flame retardant and preparation method and application thereof |
| CN115746570A (en) * | 2022-12-07 | 2023-03-07 | 华力通线缆股份有限公司 | Ceramic fire-resistant sheath material and medium-voltage fire-resistant cable |
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Application publication date: 20151111 |