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Novel fluorine-containing siloxane fire retardant, and preparation method and application thereof

A technology of siloxane and flame retardant, which is applied in the field of new fluorine-containing siloxane flame retardant and its preparation, can solve the problems of elimination, improvement of drop resistance, and reduction of heat release rate of flame-retardant polypropylene, etc., to achieve The effect of improving water resistance

Active Publication Date: 2017-07-14
铨盛聚碳科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them: (1) Although inorganic flame retardants such as magnesium hydroxide and aluminum hydroxide have both flame-retardant and smoke-suppressing effects and do not produce toxic and corrosive gases when burned, they are seriously affected due to the large amount of addition required. Physical, mechanical properties and processing properties of flame retardant materials
(2) Although organic halogen-based flame retardants have the characteristics of high flame retardant efficiency and high cost performance, their application fields have been limited because HX, which acts as a flame retardant, is a toxic and corrosive gas that is harmful to the environment and human body. , has gradually been eliminated
(3) Halogen-free flame retardant (IFR) has the advantages of low smoke and non-toxicity. IFR uses phosphorus, nitrogen, and carbon as the main core components, and it will produce a synergistic flame retardant effect when heated; the compounded IFR is usually polyphosphoric acid (APP) is the acid source, dicyandiamide (MEL) is used as the foaming agent, and pentaerythritol (PER) is used as the carbon forming agent. When subjected to high heat, a uniform and dense carbon foam layer can be formed, which can insulate heat, oxygen, and inhibit Smoke, anti-droplet, has good flame retardant properties; but most of these flame retardants are hydrophilic, poor compatibility with polymer substrates, and the required addition amount is large, which affects the flame retardant The physical properties of polymer materials cannot meet the needs of polymer materials.
In addition to endowing the substrate with excellent flame retardant properties, organosilicon flame retardants can also improve the processing performance and heat resistance of the substrate; however, due to the high price, the application is also limited
[0003] According to the British "Polymer Degradation and Stability" (Polymer Degradation and Stability, 90: 523-534, 2005), it is prepared by adding an intumescent flame retardant composed of dicyandiamide ammonium sulfate and pentaerythritol, accounting for 40% of the total mass of the system. The flame retardant polypropylene can reach the UL-94V0 level, but the mechanical properties of the material such as tensile strength and breaking strength will decrease due to the large amount of intumescent flame retardant added.
[0004] According to the American Journal of Polymer Science (Journal of Polymer Science, partA: Polymerchemistry 42: 6163-6173, 2004), when the organic montmorillonite and the intumescent flame retardant synergistically flame-retardant polypropylene, when the organic montmorillonite When the soil mass accounts for 4% of the total mass of the system, the heat release rate of flame-retardant polypropylene can be significantly reduced; but as the content of organic montmorillonite increases (after more than 4%) due to agglomeration, its flame-retardant The effect is reduced
In addition, although the flame retardant polymers containing nitrogen and phosphorus intumescent flame retardants or nitrogen and phosphorus intumescent flame retardants and flame retardant synergists prepared by the melt blending method have the characteristics of low smoke, non-toxicity and resistance to solvent droplets, However, the flame retardant effect is still not ideal, and the droplet resistance needs to be improved, and the mechanical properties of the material such as tensile strength and breaking strength will decrease due to the large amount of flame retardant added.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] A preparation method of a novel fluorine-containing silicone flame retardant, comprising the steps of:

[0062] (1) Mix the organosiloxane monomer evenly, add it to the aqueous solution dissolved with the catalyst and emulsifier, react at 30°C for 10 hours, and obtain the organopolysiloxane core emulsion; among them, the organosiloxane monomer The total mass of the water is 40% of the water quality, the consumption of the catalyst is 1% of the mass of the organosiloxane monomer, and the consumption of the emulsifier is 1% of the mass of the organosiloxane monomer;

[0063] (2) Adjust the pH value of the organopolysiloxane core emulsion to 9 with lye, then add fluorine-containing styrene monomer and comonomer, then add initiator, crosslinking agent and chain transfer agent, at 75°C Under stirring reaction 10h, obtain the polymer emulsion of organopolysiloxane grafted fluorine-containing styrene; Wherein, the consumption of fluorine-containing styrene monomer is 5% of org...

Embodiment 2

[0081] A preparation method of a novel fluorine-containing silicone flame retardant, comprising the steps of:

[0082] (1) Mix the organosiloxane monomer evenly, add it to the aqueous solution dissolved with the catalyst and emulsifier, and react at 40°C for 8 hours to obtain the organopolysiloxane core emulsion; among them, the organosiloxane monomer The total mass of the catalyst is 45% of the water quality, the consumption of the catalyst is 2% of the mass of the organosiloxane monomer, and the consumption of the emulsifier is 5% of the mass of the organosiloxane monomer;

[0083] (2) Adjust the pH value of the organopolysiloxane core emulsion to 10 with lye, then add fluorine-containing styrene monomer and comonomer, then add initiator, crosslinking agent and chain transfer agent, at 78°C Under stirring reaction 8h, obtain the polymer emulsion of organopolysiloxane grafted fluorine-containing styrene; Wherein, the consumption of fluorine-containing styrene monomer is 8% of...

Embodiment 3

[0101] A preparation method of a novel fluorine-containing silicone flame retardant, comprising the steps of:

[0102] (1) Mix the organosiloxane monomer evenly, add it to the aqueous solution dissolved with the catalyst and emulsifier, react at 55°C for 7 hours, and obtain the organopolysiloxane core emulsion; among them, the organosiloxane monomer The total mass of the catalyst is 50% of the water quality, the consumption of the catalyst is 3% of the mass of the organosiloxane monomer, and the consumption of the emulsifier is 10% of the mass of the organosiloxane monomer;

[0103] (2) Adjust the pH value of the organopolysiloxane core emulsion to 10.5 with lye, then add fluorine-containing styrene monomer and comonomer, then add initiator, cross-linking agent and chain transfer agent, at 82°C Under stirring reaction 7h, obtain the polymer emulsion of organopolysiloxane grafted fluorine-containing styrene; Wherein, the consumption of fluorine-containing styrene monomer is 10%...

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PUM

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Abstract

The invention relates to the technical field of plastic assistants, and concretely relates to a novel fluorine-containing siloxane fire retardant, and a preparation method and an application thereof. The preparation method comprises the following steps: 1, uniformly mixing organosiloxane monomers, adding the obtained monomer mixture into a catalyst and emulsifier dissolved aqueous solution, and carrying out a reaction to obtain an organopolysiloxane emulsion; 2, adjusting the pH value of the organopolysiloxane emulsion by using an alkali liquid, adding a fluorine-containing styrene monomer and a copolymerization, adding an initiator, a crosslinking agent and a chain transfer agent, and carrying out a reaction to obtain an organosiloxane grafted fluorine-containing styrene polymer emulsion; and 3, diluting the polymer emulsion, adding a de-emulsifier to carry out demulsification, centrifuging the de-emulsified emulsion, and carrying out drying and crushing to prepare the novel fluorine-containing siloxane fire retardant. The novel fluorine-containing siloxane fire retardant prepared in the invention has excellent anti-dripping effect and fire-retardant property without affecting the mechanical properties of a high-molecular material polymer, and also can improve the mechanical properties and the heat resistance of matrix resin.

Description

technical field [0001] The invention relates to the technical field of plastic additives, in particular to a novel fluorine-containing silicone flame retardant and its preparation method and application. Background technique [0002] At present, polymer materials and polymers have been widely used in industrial production and daily life. Most polymer materials Polymers are flammable and play a dominant role in combustible solid fires. Therefore, flame-retardant polymer materials have become a key research direction in the field of materials, and additive flame retardants are currently the most widely used. At present, the annual usage of additive flame retardants exceeds 1 million tons. Among them: (1) Although inorganic flame retardants such as magnesium hydroxide and aluminum hydroxide have both flame-retardant and smoke-suppressing effects and do not produce toxic and corrosive gases when burned, they are seriously affected due to the large amount of addition required. ...

Claims

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Application Information

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IPC IPC(8): C08F283/12C08F212/14C08F212/08C08F212/12C08F220/40C08F226/06C08F222/28C08F222/26C08F2/38C08F2/26C08F2/28C08F2/30C08F220/44C08F222/14C08F222/20C08F220/14C08F220/18C08L69/00C08L51/08C08G77/20
CPCC08F2/26C08F2/28C08F2/30C08F2/38C08F283/124C08G77/20C08L69/00C08L2201/02C08L2201/08C08F212/14C08L51/08
Inventor 王启瑶冯猛
Owner 铨盛聚碳科技股份有限公司
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