CN105153468A - Phosphorus-nitrogen-silicon compound loaded montmorillonite flame retardant and preparation method thereof - Google Patents
Phosphorus-nitrogen-silicon compound loaded montmorillonite flame retardant and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a flame retardant, in particular to a phosphorus-nitrogen-silicon compound loaded montmorillonite flame retardant and a preparation method thereof. The phosphorus-nitrogen-silicon compound loaded montmorillonite flame retardant is prepared through a solid-phase grafting reaction between a phosphorus-nitrogen-silicon compound and montmorillonite powder particles, wherein the phosphorus-nitrogen-silicon compound comprises an amido containing silane coupling agent and a phosphoryl chloride containing compound, and is grafted onto montmorillonite through chemical bonds. During preparation of the phosphorus-nitrogen-silicon compound loaded montmorillonite flame retardant, an amino in the silane coupling agent reacts with phosphorus oxychloride to generate a by-product, namely hydrogen chloride gas; one part of the hydrogen chloride gas is brought out of the reaction system through nitrogen gas, and the other part of the hydrogen chloride gas serves as a catalyst for a condensation reaction between the silane coupling agent and a hydroxy on the surface of montmorillonite, so that the silane coupling agent can be grafted into the surface of montmorillonite through the solid-phase grafting reaction, the rate of the solid-phase grafting reaction is improved, and the reaction time is shortened.
Description
Technical field
The present invention relates to a kind of fire retardant, particularly a kind of phosphorus nitrogen silicon based compound load montmorillonite fire retardant and preparation method thereof.
Background technology
Polynite, as a kind of flame-retardant additive, has the advantages such as flame retarding efficiency is high, addition is low, Halogen low toxicity, environmental friendliness, has broad application prospects in flame retardance of polymer modification field.Along with deepening continuously of composite technology research, increasing polymer-montmorillonoid matrix material, as high-performance, multi-functional fire retardant material, has more and more extensive use in electronic apparatus, aerospace, building, automobile and other industries.Halogen-free flame retardants---organophosphorus nitrogen compound has the advantages such as few cigarette, low toxicity, hydrolysis, good stability, polynite/polymer composites is the fire retardant material of a kind of " environmental protection ", compared with traditional filled polymer, there is the advantages such as consumption is few, cost is low, flame-retarded efficiency is high, the amount of being fuming is few.In conjunction with both advantage, synthesize the organophosphorus nitrogen silicon based compound that can realize organ-mmt by molecular designing, binding reaction is carried out in this compound and polynite, obtains NEW TYPE OF COMPOSITE fire retardant---phosphorus nitrogen silicon based compound load montmorillonite fire retardant.
Phosphorus nitrogen silicon based compound is utilized to carry out organic modification to polynite, improve the dispersiveness of expansion type flame retardant at polymeric matrix on polynite and its surface of enrichment, reduce the micromolecular transport property of the fire retardant being anchored at polynite surface, make polynite and fire retardant play synergistic effect better, be conducive under the prerequisite of few additive, realize high molecular fire retardant material high performance etc.But, in the preparation of phosphorus nitrogen silicon based compound load montmorillonite fire retardant, because polynite is mineral compound, disperse very poor in organic solvent, need add carrying out smoothly of a large amount of organic solvent guarantee reactions, need after reaction to carry out Distillation recovery to organic solvent, energy consumption is very large, cost is high, is unfavorable for suitability for industrialized production.Solid state shear pulrerizing is utilized to synthesize phosphorus nitrogen silicon based compound load montmorillonite fire retardant, not only enormously simplify synthesis technique, and there is the advantages such as reaction cost is low, energy consumption is little, solvent-free, prepare Problems existing provide a kind of new approach for solving above-mentioned fire retardant.
Summary of the invention
The object of the present invention is to provide a kind of a kind of phosphorus nitrogen silicon based compound load montmorillonite fire retardant with excellent flame retardant performance.
The present invention also provides the preparation method of described phosphorus nitrogen silicon based compound load montmorillonite fire retardant.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of phosphorus nitrogen silicon based compound load montmorillonite fire retardant, the phosphorus nitrogen silicon based compound that this fire retardant is made up of the silane coupling agent of amino-contained, phosphorous chloride compounds and polynite powder particle are obtained by solid state shear pulrerizing, and phosphorus nitrogen silicon based compound is by chemical bond grafting polynite.
A preparation method for described phosphorus nitrogen silicon based compound load montmorillonite fire retardant, obtains phosphorus nitrogen silicon based compound load montmorillonite fire retardant by the silane coupling agent of amino-contained, phosphorous chloride compounds and polynite powder particle by solid state shear pulrerizing.Further, the silane coupling agent of amino-contained and phosphorous chloride compounds, polynite are joined in ball mill, grind 20 ~ 150 minutes under the condition of logical nitrogen, obtained phosphorus nitrogen silicon based compound load montmorillonite fire retardant.
As preferably, the mass ratio that feeds intake of described polynite and the silane coupling agent of amino-contained is 1.0:0.02 ~ 0.38, and the silane coupling agent of described amino-contained feeds intake amount of substance than being 1.0:1.0 ~ 2.5 with phosphorous chloride compounds.
As preferably, the silane coupling agent of described amino-contained is selected from one of the following: N-aminoethyl-γ-aminopropyltrimethoxysilane, 3-(2-aminoethyl base) propyl-triethoxysilicane, 3-aminopropyl trimethoxysilane, 3-aminopropyl triethoxysilane.
As preferably, described phosphorous chloride compounds is selected from one of the following: solutions of dimethyl phosphoryl chlorine, diethylchlorophosphate (C2H5O)2P(O)Cl, diphenyl phosphoryl chlorine.
As preferably, in described preparation process condition, balling drum rotating speed 21.7 ~ 38 revs/min, passing into nitrogen gas stream speed is 0.1 ~ 20 cubic meters per minute.
The application in flame-proof composite material prepared by a kind of described phosphorus nitrogen silicon based compound load montmorillonite fire retardant, in the weight of thermoplastics for 100%, the addition of this phosphorus nitrogen silicon based compound load montmorillonite fire retardant in thermoplastics is 5% ~ 30%.
Compared with prior art, beneficial effect of the present invention is embodied in following several respects:
In the preparation process of 1, phosphorus nitrogen silicon based compound load montmorillonite fire retardant of the present invention, the amino of silane coupling agent and phosphoryl chloride react and generate byproduct hydrogen chloride gas, part takes reaction system out of by nitrogen, part is as the catalyzer of silane coupling agent and the condensation reaction of polynite surface hydroxyl, silane coupling agent is made to be grafted to polynite surface by solid state reaction, be conducive to the raising that solid phase connects speed of reaction, shorten the reaction times;
2, the preparation method of fire retardant of the present invention have employed solid-phase sequencing reaction, not only simplify synthesis route, and reduces the discharge of reaction cost, minimizing energy consumption and pollutent;
3, the preparation method of fire retardant of the present invention utilizes solid state shear pulrerizing, be conducive to the load of phosphorus nitrogen silicon based compound on polynite surface, improve it dispersed simultaneously, enhance the flame retardant effect of fire retardant to macromolecular material, decrease the usage quantity of fire retardant at macromolecular material, reduce the preparation cost of fire retardant material;
4, fire retardant preparation process of the present invention is easy and simple to handle, and operational path is simple, preparation cost is cheap, environmental protection and energy consumption is low, and products therefrom, without the need to being separated, is easy to suitability for industrialized production.
Embodiment
Below by specific embodiment, technical scheme of the present invention is described in further detail.Should be appreciated that enforcement of the present invention is not limited to the following examples, any pro forma accommodation make the present invention and/or change all will fall into scope.
In the present invention, if not refer in particular to, all parts, per-cent are weight unit, and the equipment adopted and raw material etc. all can be buied from market or this area is conventional.Method in following embodiment, if no special instructions, is the ordinary method of this area.
Embodiment 1
1500 kilograms of polynites are joined in the ball mill being connected with nitrogen access tube, ball mill specification is Ф 900 × 1800, ball loadings is 1.5 tons, under the condition of balling drum rotating speed 38 revs/min, add 150 kilograms of 3-aminopropyl trimethoxysilane and 175 kilograms of diphenyl phosphoryl chlorine respectively, pass into nitrogen gas stream speed be 0.5 cubic meters per minute condition under griding reaction 40 minutes, obtained phosphorus nitrogen silicon based compound load montmorillonite fire retardant, yield is 97.9%.
Embodiment 2
The synthetic operation of phosphorus nitrogen silicon based compound load montmorillonite fire retardant is with embodiment 1, and raw material is: polynite, N-aminoethyl-γ-aminopropyltrimethoxysilane, solutions of dimethyl phosphoryl chlorine.The add-on of polynite is 38000 kilograms, the mass ratio that feeds intake of polynite and N-aminoethyl-γ-aminopropyltrimethoxysilane is 1.0:0.02, N-aminoethyl-γ-aminopropyltrimethoxysilane feeds intake amount of substance than being 1.0:2.5 with solutions of dimethyl phosphoryl chlorine, ball mill specification is Ф 2200 × 7500, ball loadings is 35 tons, drum rotational speed 21.7 revs/min, and milling time is 20 minutes, passing into nitrogen gas stream speed is 0.1 cubic meters per minute, and yield is 99.1%.
Embodiment 3
The synthetic operation of phosphorus nitrogen silicon based compound load montmorillonite fire retardant is with embodiment 1, and raw material is: polynite, 3-(2-aminoethyl base) propyl-triethoxysilicane, diethylchlorophosphate (C2H5O)2P(O)Cl.The add-on of polynite is 4500 kilograms, the mass ratio that feeds intake of polynite and 3-(2-aminoethyl base) propyl-triethoxysilicane is 1.0:0.38,3-(2-aminoethyl base) propyl-triethoxysilicane feeds intake amount of substance than being 1.0:2.2 with diethylchlorophosphate (C2H5O)2P(O)Cl, ball mill specification is Ф 1500 × 3000, ball loadings is 7.5 tons, drum rotational speed 29.7 revs/min, milling time is 150 minutes, passing into nitrogen gas stream speed is 20 cubic meters per minute, and yield is 97.3%.
Embodiment 4
The synthetic operation of phosphorus nitrogen silicon based compound load montmorillonite fire retardant is with embodiment 1, and raw material is: polynite, N-aminoethyl-γ-aminopropyltrimethoxysilane, diphenyl phosphoryl chlorine.The add-on of polynite is 4500 kilograms, the mass ratio that feeds intake of polynite and N-aminoethyl-γ-aminopropyltrimethoxysilane is 1.0:0.14, N-aminoethyl-γ-aminopropyltrimethoxysilane feeds intake amount of substance than being 1.0:2.3 with diphenyl phosphoryl chlorine, ball mill specification is Ф 1500 × 3000, ball loadings is 7.5 tons, drum rotational speed 29.7 revs/min, and milling time is 60 minutes, passing into nitrogen gas stream speed is 12 cubic meters per minute, and yield is 98.3%.
Embodiment 5
The synthetic operation of phosphorus nitrogen silicon based compound load montmorillonite fire retardant is with embodiment 1, and raw material is: polynite, 3-aminopropyl triethoxysilane, diethylchlorophosphate (C2H5O)2P(O)Cl.The add-on of polynite is 1200 kilograms, the mass ratio that feeds intake of polynite and 3-aminopropyl triethoxysilane is 1.0:0.22,3-aminopropyl triethoxysilane feeds intake amount of substance than being 1.0:1.25 with diethylchlorophosphate (C2H5O)2P(O)Cl, ball mill specification is Ф 900 × 1800, ball loadings is 1.5 tons, drum rotational speed 36 revs/min, and milling time is 45 minutes, passing into nitrogen gas stream speed is 6.7 cubic meters per minute, and yield is 98.6%.
Embodiment 6: the application of phosphorus nitrogen silicon based compound load montmorillonite fire retardant
The preparation manipulation of phosphorus nitrogen silicon based compound load montmorillonite fire retardant is with embodiment 1.By 120 kg polypropylene, (melting index is 2.3 grams/10 minutes, producer is for raising sub-petrochemical industry) and 15 kilograms of phosphorus nitrogen silicon based compound load montmorillonite fire retardants put into dispersion machine and stir 20 minutes, by said mixture after taking-up, through screw extrusion press (processing temperature scope is 180 ~ 210 DEG C) extruding pelletization, obtain polypropylene/phosphorus nitrogen silicon based compound load montmorillonite fire-retardant composite material, the result that cone calorimetry measures the fire-retardant performance of this matrix material is as shown in table 1.
Table 1
Note: polypropylene/organic montmorillonite fire-retardant composite material: organo montmorillonite and polyacrylic mass ratio are 8:1, organo montmorillonite is the polynite of cetyl trimethylammonium bromide organic-treating, and cetyl trimethylammonium bromide and polynite mass ratio are 25:3; Polypropylene/phosphorus nitrogen silicon based compound load montmorillonite fire-retardant composite material: phosphorus nitrogen silicon based compound load montmorillonite fire retardant and polyacrylic mass ratio are 8:1, and phosphorus nitrogen silicon based compound and polynite mass ratio are 25:3.
Known by table 1, compared with pure polypropylene, the heat release rate peak value that with the addition of the polypropylene/phosphorus nitrogen silicon based compound load montmorillonite fire-retardant composite material of phosphorus nitrogen silicon based compound load montmorillonite reduces 56%, burning time extends about 7 seconds, Thermal release total amount, specific extinction area average, mass loss mean rate all have and decline in various degree, show that phosphorus nitrogen silicon based compound load montmorillonite can effectively improve polyacrylic flame retardant properties, and it is better than similar flame retardant products organo montmorillonite to polyacrylic fire retardation.
Above-described embodiment is one of the present invention preferably scheme, not does any pro forma restriction to the present invention, also has other variant and remodeling under the prerequisite not exceeding the technical scheme described in claim.
Claims (8)
1. a phosphorus nitrogen silicon based compound load montmorillonite fire retardant, it is characterized in that: the phosphorus nitrogen silicon based compound that this fire retardant is made up of the silane coupling agent of amino-contained, phosphorous chloride compounds and polynite powder particle are obtained by solid state shear pulrerizing, phosphorus nitrogen silicon based compound is by chemical bond grafting polynite.
2. a preparation method for phosphorus nitrogen silicon based compound load montmorillonite fire retardant according to claim 1, is characterized in that: the silane coupling agent of amino-contained, phosphorous chloride compounds and polynite powder particle are obtained phosphorus nitrogen silicon based compound load montmorillonite fire retardant by solid state shear pulrerizing.
3. preparation method according to claim 2, it is characterized in that: the silane coupling agent of amino-contained and phosphorous chloride compounds, polynite are joined in ball mill, grind 20 ~ 150 minutes under the condition of logical nitrogen, obtained phosphorus nitrogen silicon based compound load montmorillonite fire retardant.
4. preparation method according to claim 2, it is characterized in that: the mass ratio that feeds intake of described polynite and the silane coupling agent of amino-contained is 1.0:0.02 ~ 0.38, the silane coupling agent of described amino-contained is 1.0:1.0 ~ 2.5 with the amount of substance ratio that feeds intake of phosphorous chloride compounds.
5. preparation method according to claim 2, is characterized in that: the silane coupling agent of described amino-contained is selected from one of the following: N-aminoethyl-γ-aminopropyltrimethoxysilane, 3-(2-aminoethyl base) propyl-triethoxysilicane, 3-aminopropyl trimethoxysilane, 3-aminopropyl triethoxysilane.
6. preparation method according to claim 2, is characterized in that: described phosphorous chloride compounds is selected from one of the following: solutions of dimethyl phosphoryl chlorine, diethylchlorophosphate (C2H5O)2P(O)Cl, diphenyl phosphoryl chlorine.
7. preparation method according to claim 2, is characterized in that: in described preparation process condition, balling drum rotating speed 21.7 ~ 38 revs/min, and passing into nitrogen gas stream speed is 0.1 ~ 20 cubic meters per minute.
8. the application in flame-proof composite material prepared by a phosphorus nitrogen silicon based compound load montmorillonite fire retardant according to claim 1, it is characterized in that: in the weight of thermoplastics for 100%, the addition of this phosphorus nitrogen silicon based compound load montmorillonite fire retardant in thermoplastics is 5% ~ 30%.
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Cited By (8)
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| CN106243475A (en) * | 2016-08-15 | 2016-12-21 | 合肥汇通控股股份有限公司 | A kind of high-performance ethylene-vinyl acetate copolymer composite |
| CN107304299A (en) * | 2016-04-21 | 2017-10-31 | 中国石油化工股份有限公司 | A kind of fire retardant, flame-retardant pitch and preparation method thereof |
| CN109705634A (en) * | 2019-01-15 | 2019-05-03 | 安徽大学 | A kind of concave convex rod soil matrix composite flame-retardant agent and its preparation and application with the modification of Nitrogen-and Phosphorus-containing organic matter |
| CN110628082A (en) * | 2019-10-17 | 2019-12-31 | 西北师范大学 | Multifunctional additive for high polymer material and preparation method thereof |
| CN113429435A (en) * | 2021-06-30 | 2021-09-24 | 成都硅宝科技股份有限公司 | Silane coupling agent containing phosphorus and nitrogen and preparation method thereof |
| CN114316367A (en) * | 2021-12-29 | 2022-04-12 | 江苏扬农化工集团有限公司 | Modified bentonite, preparation method thereof, flame-retardant PTT fiber and application thereof |
| CN115304636A (en) * | 2022-08-15 | 2022-11-08 | 铨盛聚碳科技股份有限公司 | Organic silicon flame retardant containing phosphorus and nitrogen, and preparation method and application thereof |
| CN117467210A (en) * | 2023-12-28 | 2024-01-30 | 南方珠江科技有限公司 | Wind power generation cable with high wear resistance |
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| CN107304299A (en) * | 2016-04-21 | 2017-10-31 | 中国石油化工股份有限公司 | A kind of fire retardant, flame-retardant pitch and preparation method thereof |
| CN107304299B (en) * | 2016-04-21 | 2019-06-18 | 中国石油化工股份有限公司 | A kind of fire retardant, flame-retardant pitch and preparation method thereof |
| CN106243475A (en) * | 2016-08-15 | 2016-12-21 | 合肥汇通控股股份有限公司 | A kind of high-performance ethylene-vinyl acetate copolymer composite |
| CN109705634A (en) * | 2019-01-15 | 2019-05-03 | 安徽大学 | A kind of concave convex rod soil matrix composite flame-retardant agent and its preparation and application with the modification of Nitrogen-and Phosphorus-containing organic matter |
| CN110628082A (en) * | 2019-10-17 | 2019-12-31 | 西北师范大学 | Multifunctional additive for high polymer material and preparation method thereof |
| CN110628082B (en) * | 2019-10-17 | 2021-05-18 | 西北师范大学 | Multifunctional additive for high polymer material and preparation method thereof |
| CN113429435A (en) * | 2021-06-30 | 2021-09-24 | 成都硅宝科技股份有限公司 | Silane coupling agent containing phosphorus and nitrogen and preparation method thereof |
| CN114316367A (en) * | 2021-12-29 | 2022-04-12 | 江苏扬农化工集团有限公司 | Modified bentonite, preparation method thereof, flame-retardant PTT fiber and application thereof |
| CN114316367B (en) * | 2021-12-29 | 2023-11-28 | 江苏扬农化工集团有限公司 | Modified bentonite, preparation method thereof, flame-retardant PTT fiber and application |
| CN115304636A (en) * | 2022-08-15 | 2022-11-08 | 铨盛聚碳科技股份有限公司 | Organic silicon flame retardant containing phosphorus and nitrogen, and preparation method and application thereof |
| CN117467210A (en) * | 2023-12-28 | 2024-01-30 | 南方珠江科技有限公司 | Wind power generation cable with high wear resistance |
| CN117467210B (en) * | 2023-12-28 | 2024-03-08 | 南方珠江科技有限公司 | Wind power generation cable with high wear resistance |
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