Preparation method of ELE-FP fire extinguishing particles

Abstract

The invention discloses a preparation method of ELE-FP fire extinguishing particles, and relates to the field of fire extinguishing materials, the ELE-FP fire extinguishing particles comprise a core material and a capsule shell, the core material is coated in the capsule shell, the core material is perfluoroethanone, and the capsule shell is a polymeric monomer of isophorone diisocyanate and diethylenetriamine. When the perfluorohexanone microcapsule is prepared, the microcapsule with better storage stability can be obtained by adopting a smaller core-wall ratio, and the linear polyurethane microcapsule taking the perfluorohexanone as the core material is prepared by adopting an interfacial polymerization method and taking isophorone diisocyanate and diethylenetriamine as polymeric monomers. Secondly, by adding a polyol cross-linking agent to generate a microcapsule with a net-shaped capsule shell, or by adding polypropylene glycol to form a microcapsule with a polyurea / polyurethane composite structure, storage stability analysis shows that the microcapsule with the net-shaped capsule shell and the microcapsule with the polyurea / polyurethane composite structure greatly improve compactness, so that the storage stability is improved; and the core material is effectively protected.

Description

Technical Field

[0001] The invention relates to the field of fire extinguishing materials, and in particular to a method for preparing ELE-FP fire extinguishing particles. Background Art

[0002] Perfluorohexanone (CAS No. 756-13-8) is a new type of environmentally friendly fire extinguishing agent. It is liquid at room temperature. Its evaporation heat is only 1 / 25 of that of water, and its vapor pressure is 25 times that of water. These properties make it easy to vaporize and can quickly absorb heat to achieve the effect of fire extinguishing. Its ozone depletion potential (ODP): 0, global greenhouse effect potential (GWP): 1, atmospheric survival life (year): 0.014 (5 days). It can replace halon fire extinguishing agent for a long time. However, due to its boiling point of only 49°C, its use as a fire extinguishing agent is still limited. It is currently usually used to replace halon fire extinguishers, or full flooding systems and local application systems for Class B fire protection. In actual applications, it usually needs to be stored in fire extinguishing tanks, or requires a special fire extinguishing system, so it is inconvenient to extinguish fires.

[0003] At present, when perfluorohexanone fire extinguishing microcapsules are prepared, the storage stability of the perfluorohexanone fire extinguishing microcapsules is poor and the core material cannot be effectively protected, which will affect the service life of the perfluorohexanone fire extinguishing microcapsules.

[0004] Therefore, it is necessary to invent a method for preparing ELE-FP fire extinguishing particles to solve the above problems. Summary of the invention

[0005] The object of the present invention is to provide a method for preparing ELE-FP fire extinguishing particles to solve the problems raised in the above background technology.

[0006] To achieve the above objectives, the present invention provides the following technical solutions: a method for preparing ELE-FP fire extinguishing particles, comprising a core material and a capsule shell, wherein the core material is coated in the capsule shell, the core material is perfluoroacetone, and the capsule shell is a polymerized monomer of isophorone diisocyanate and diethylenetriamine.

[0007] Preferably, the particle size of the ELE-FP fire extinguishing particles ranges from 300 to 700 μm, the triggering temperature of the ELE-FP fire extinguishing particles ranges from 90 to 200° C., and the coverage rate of the ELE-FP fire extinguishing particles is greater than 40%.

[0008] A method for preparing ELE-FP fire extinguishing particles comprises the following steps:

[0009] S1: mixing and emulsifying perfluoroacetone, isophorone diisocyanate, diethylenetriamine and an emulsifier to form emulsion droplets;

[0010] S2: The emulsion droplets are cured by ultraviolet light to obtain linear polyurethane microcapsules with perfluorohexanone as the core material.

[0011] Preferably, in S1, the emulsification time is 2000 rpm, the emulsification time is 10 min, and the emulsification amount is 3 g.

[0012] Preferably, in S2, the sum of the internal and external flow rates of the UV curing is 10-50 ml / h, the flow rate ratio of the UV curing is 1:0.8-1:4, and the driving phase flow rate of the UV curing is 800-1500 ml / h.

[0013] Preferably, in S1, the ratio of isophorone diisocyanate to diethylenetriamine is 3:8.

[0014] Preferably, in S1, a polyol cross-linking agent is added into the emulsion droplets to generate microcapsules with a network shell.

[0015] Preferably, in S1, polypropylene glycol is added into the emulsion droplets to form microcapsules with a polyurea / polyurethane composite structure.

[0016] Preferably, in S1, pentaerythritol is added into the emulsion droplets, and the amount of pentaerythritol used is 0.1 g.

[0017] Technical effects and advantages of the present invention:

[0018] The present invention adopts a smaller core-to-wall ratio when preparing perfluorohexanone microcapsules to obtain microcapsules with better storage stability, and adopts an interfacial polymerization method to prepare linear polyurethane microcapsules with perfluorohexanone as a core material by using isophorone diisocyanate and diethylenetriamine as polymerization monomers. Then, a polyol crosslinking agent is added to generate microcapsules with a mesh capsule shell, or polypropylene glycol is added to form microcapsules with a polyurea / polyurethane composite structure. Storage stability analysis shows that the microcapsules with a mesh capsule shell and the microcapsules with a polyurea / polyurethane composite structure have greatly improved compactness, thereby improving storage stability and effectively protecting the core material. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 Schematic diagram of the microscopic image of the ELE-FP fire extinguishing particles of the present invention after drying. DETAILED DESCRIPTION

[0020] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0021] The present invention provides Figure 1 The preparation method of the ELE-FP fire extinguishing particles shown in the figure comprises a core material and a capsule shell, wherein the core material is coated in the capsule shell, the core material is perfluoroacetone, and the capsule shell is a polymerized monomer of isophorone diisocyanate and diethylenetriamine.

[0022] The particle size of the ELE-FP fire extinguishing particles ranges from 300 to 700 μm, the triggering temperature of the ELE-FP fire extinguishing particles ranges from 90 to 200° C., and the coverage rate of the ELE-FP fire extinguishing particles is greater than 40%.

[0023] A method for preparing ELE-FP fire extinguishing particles comprises the following steps:

[0024] S1: mixing perfluoroacetone, isophorone diisocyanate, diethylenetriamine and an emulsifier, emulsifying to form emulsion droplets;

[0025] S2: The emulsion droplets are cured by ultraviolet light to obtain linear polyurethane microcapsules with perfluorohexanone as the core material.

[0026] In S1, the emulsification time is 2000 rpm, the emulsification time is 10 min, and the emulsification amount is 3 g.

[0027] In S2, the sum of the internal and external flow rates of the ultraviolet light curing is 10-50 ml / h, the flow rate ratio of the ultraviolet light curing is 1:0.8-1:4, and the driving phase flow rate of the ultraviolet light curing is 800-1500 ml / h.

[0028] In S1, the ratio of isophorone diisocyanate to diethylenetriamine is 3:8.

[0029] Optical microscopy, infrared spectroscopy, thermogravimetric analyzer and laser particle size analyzer were used to study and analyze the surface morphology, chemical structure, thermal stability, particle size and distribution, and storage stability of the prepared microcapsules. The uniform and stable emulsification of perfluorohexanone and reactive monomers was achieved by using a suitable and efficient compound fluorocarbon surfactant and exploring the factors affecting the stability of the microcapsules. The infrared analysis results showed that the core material perfluorohexanone had been successfully embedded in the polyurethane capsule shell, and the thermogravimetric analysis further verified this conclusion. The optical microscope image of the emulsion droplets showed that when the emulsification speed was 2000rpm and the emulsification time was 10min, the emulsification speed was 2000rpm and the emulsification time was 10min. The emulsification effect is excellent, the dispersion is uniform, and the particle size is uniform. Through infrared spectrum analysis, the optimal ratio of isophorone diisocyanate and diethylenetriamine is determined to be 3:8. Through thermogravimetric analysis, it is found that the increase of emulsification speed and emulsifier dosage can improve the thermal stability and embedding rate of microcapsules, but it should not be too large. The optimal emulsification speed is determined to be 2000rpm, and the amount of emulsifier is 0.3g. In addition, it is found that the effect of using fractional heating is better. Through particle size analysis, it is found that with the increase of emulsification speed, the particle size is significantly reduced and the distribution is more uniform. When the water-oil ratio is 6:1, the particle size distribution of the microcapsules is uniform and the average particle size is small.

[0030] In S1, a polyol cross-linking agent is added into the emulsion droplets to generate microcapsules with a network shell.

[0031] In S1, polypropylene glycol is added into the emulsion droplets to form microcapsules with a polyurea / polyurethane composite structure.

[0032] In S1, in S1, pentaerythritol is added into the emulsion droplets, and the amount of pentaerythritol used is 0.1 g. Properly increasing the amount of pentaerythritol can improve the heat resistance temperature and coverage rate of the microcapsules.

[0033] Secondly, by adding a polyol cross-linking agent, a microcapsule with a mesh shell is generated, or by adding polypropylene glycol, a microcapsule with a polyurea / polyurethane composite structure is formed. Storage stability analysis shows that the microcapsule with a mesh shell and the microcapsule with a polyurea / polyurethane composite structure greatly improves the density, thereby improving the storage stability and effectively protecting the core material.

[0034] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing ELE-FP fire extinguishing particles, characterized in that: The capsule shell comprises a core material and a capsule shell, wherein the core material is coated in the capsule shell, the core material is perfluoroacetone, and the capsule shell is a polymerized monomer of isophorone diisocyanate and diethylenetriamine.

2. The method for preparing the ELE-FP fire extinguishing particles according to claim 1, characterized in that: The particle size of the ELE-FP fire extinguishing particles ranges from 300 to 700 μm, the triggering temperature of the ELE-FP fire extinguishing particles ranges from 90 to 200° C., and the coverage rate of the ELE-FP fire extinguishing particles is greater than 40%.

3. The method for preparing the ELE-FP fire extinguishing particles according to claim 2, characterized in that: The steps include: S1: mixing and emulsifying perfluoroacetone, isophorone diisocyanate, diethylenetriamine and an emulsifier to form emulsion droplets; S2: The emulsion droplets are cured by ultraviolet light to obtain linear polyurethane microcapsules with perfluorohexanone as the core material.

4. The method for preparing the ELE-FP fire extinguishing particles according to claim 3, characterized in that: In S1, the emulsification time is 2000 rpm, the emulsification time is 10 min, and the emulsification amount is 3 g.

5. The method for preparing the ELE-FP fire extinguishing particles according to claim 4, characterized in that: In S2, the sum of the internal and external flow rates of the ultraviolet light curing is 10-50 ml / h, the flow rate ratio of the ultraviolet light curing is 1:0.8-1:4, and the driving phase flow rate of the ultraviolet light curing is 800-1500 ml / h.

6. The method for preparing the ELE-FP fire extinguishing particles according to claim 5, characterized in that: In S1, the ratio of isophorone diisocyanate to diethylenetriamine is 3:

8.

7. The method for preparing ELE-FP fire extinguishing particles according to claim 6, characterized in that: In S1, a polyol cross-linking agent is added into the emulsion droplets to generate microcapsules with a network shell.

8. The method for preparing ELE-FP fire extinguishing particles according to claim 7, characterized in that: In S1, polypropylene glycol is added into the emulsion droplets to form microcapsules with a polyurea / polyurethane composite structure.

9. The method for preparing ELE-FP fire extinguishing particles according to claim 8, characterized in that: In S1, pentaerythritol is added into the emulsion droplets, and the amount of pentaerythritol used is 0.1 g.

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