Perfluorohexanone microcapsule as well as preparation method and application thereof

By adopting specific core-shell structures and cross-linking reactions, the problem of perfluorohexanone microcapsules being easily damaged and agglomerated during drying is solved, and an efficient and stable fire extinguishing effect is achieved.

CN120285501APending Publication Date: 2025-07-11HUANGPU INST OF MATERIALS
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Patent Information

Application Number
CN202510362521.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-26
Publication Date
2025-07-11

AI Technical Summary

Technical Problem

In the prior art, the preparation method of perfluorohexanone microcapsules has problems such as low production efficiency, high cost, difficulty in mass production, and easy to break or agglomerate during drying, resulting in poor fire extinguishing effect.

Method used

A specific core-shell structure is adopted, including the capsule core and the capsule wall composed of the first shell layer, the second shell layer, and the third shell layer, perfluorohexanone microcapsules are prepared through crosslinking and self-polymerization reaction. The weight ratio of the capsule core and the capsule wall is (16-32): 1, and a specific 385 amino resin is used to react with the active hydroxyl groups in the second shell layer to form a stable microcapsule.

Benefits of technology

The prepared perfluorohexanone microcapsules are not easy to break and reunite during drying. They have good fire extinguishing effects and can effectively extinguish fires many times.

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Abstract

The invention discloses a perfluorohexanone microcapsule as well as a preparation method and application thereof, and relates to the technical field of fire extinguishing materials. The invention provides a perfluorohexanone microcapsule which comprises a capsule core and a capsule wall which are sequentially arranged, the capsule wall comprises a first shell layer, a second shell layer and a third shell layer which are sequentially arranged, and the capsule core is adjacent to the first shell layer; the average particle size of the perfluorohexanone microcapsule is 50-400 [mu] m, and the weight ratio of the capsule core to the capsule wall is (16-32): 1; by adopting a specific core-shell structure, the prepared perfluorohexanone microcapsule is not easy to damage, not easy to agglomerate and good in fire extinguishing effect.
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Description

Technical Field

[0001] The present invention relates to the technical field of fire extinguishing materials, in particular to a perfluorhexanone microcapsule, a preparation method thereof and an application thereof. Background Art

[0002] Fire is one of the disasters in people's daily life. If not extinguished in time, it is likely to cause serious losses to people's lives and property. In theory, all fires can be extinguished. The key lies in extinguishing the fire source in time when the fire breaks out initially, which is the key control factor determining the losses of personnel and property. There are various fire extinguishing media for extinguishing the fire source, and common fire extinguishing media include water, dry ice, etc.

[0003] As an emerging fire extinguishing medium, microcapsule fire extinguishing agents have been gradually widely used in the fire protection field in recent years. In the prior art, microcapsule active fire extinguishing agents usually use high molecular resin as the shell and encapsulate halogenated hydrocarbon fire extinguishing substances inside, such as Russian Patent RU90994, Chinese Patent CN103370104A, etc. The halogenated hydrocarbon fire extinguishing substances in the core material of the microcapsules are not only costly, but also toxic to the environment and the human body to varying degrees. As an important alternative to halon fire extinguishing agents, perfluorhexanone is a compound of fluorinated ketones. In recent years, it has attracted much attention due to its good fire extinguishing ability and the characteristic of not damaging the ozone layer. However, the extremely low degree of fluorination of perfluorocarbons makes the intermolecular dispersion interaction weak. As a result, compared with hydrocarbons with the same relative molecular mass, the boiling point of perfluorocarbons is very low. The boiling point of perfluorhexanone is 49°C, which is easy to quickly gasify and volatilize, and it is difficult to store and apply. Another result caused by the extremely low degree of fluorination of perfluorocarbons is that there is a large immiscibility fault in the solvent systems of perfluorocarbons and hydrocarbons, that is, hydrocarbon liquids and fluorocarbon liquids are immiscible at room temperature, which also greatly increases the difficulty of making perfluorhexanone into a fire extinguishing material. Currently, microfluidic methods and complex coacervation methods are generally used to prepare perfluorhexanone microcapsules. The microfluidic preparation method has low production efficiency, high production cost, and is difficult to meet large-scale industrial production; although the complex coacervation preparation method can prepare wet microcapsules on a large scale, drying is a problem. Spray drying method is generally used for drying. This method is suitable for core materials that can withstand high temperatures, and is not suitable for perfluorhexanone with a low boiling point. It is easy to damage the capsules during the drying process, and the products obtained by freeze drying and natural air drying are prone to agglomeration and cannot form stable particles.

[0004] In view of this, the present application is proposed. Summary of the Invention

[0005] Based on this, the object of the present invention is to overcome the above-mentioned deficiencies of the prior art and provide a perfluorhexanone microcapsule, a preparation method thereof and an application thereof.

[0006] To achieve the above object, the technical solution adopted by the present invention is as follows: A perfluorohexanone microcapsule includes a core and a wall arranged in sequence. The wall includes a first shell layer, a second shell layer, and a third shell layer arranged in sequence. The core is adjacent to the first shell layer. The average particle size of the perfluorohexanone microcapsule is 50 - 400 μm, and the weight ratio of the core to the wall is (16 - 32):1.

[0007] The core includes perfluorohexanone. The components of the first shell layer include a polymer material. The polymer material is at least two of gelatin, sodium alginate, chitosan, gum arabic, polyglutamic acid, β-cyclodextrin, sodium dodecyl sulfate, sodium carboxymethyl cellulose, hydroxypropyl methylcellulose, octenyl succinic anhydride esterified starch. The components of the second shell layer include a curing agent. The curing agent is at least one of formaldehyde, acetaldehyde, glutaraldehyde, and glyoxal. The components of the third shell layer include 385 amino resin.

[0008] By adopting a specific core-shell structure, the perfluorohexanone microcapsules prepared by the present invention are not easily damaged and agglomerated during the drying process, and have a good fire extinguishing effect. The first shell layer of the present invention is a wall material layer. The second shell layer is formed by crosslinking the curing agent with the amino and hydroxyl groups in the first layer and self-polymerizing into the second shell layer. The components of the third shell layer are selected to react with the active hydroxyl groups in the second shell layer with a specific 385 amino resin and self-polymerize. Finally, the prepared perfluorohexanone microcapsules are not easily damaged and agglomerated during the drying process.

[0009] Further preferably, the weight ratio of the core to the wall is (17 - 25):1; more preferably, the weight ratio of the core to the wall is (18 - 22):1.

[0010] The inventors found in the actual experiment process that the weight ratio of the core to the wall in the perfluorohexanone microcapsules with a specific core-shell structure will further affect the fire extinguishing effect of the perfluorohexanone microcapsules.

[0011] Preferably, the components of the first shell layer further include an antifoaming agent. Preferably, the antifoaming agent is at least one of silicone antifoaming agent and polyether antifoaming agent. Specifically, the antifoaming agent is silicone antifoaming agent BYK-141 and polyether antifoaming agent Federal-B-0518.

[0012] Preferably, the polymer material is a mixture of gum arabic, gelatin, and sodium dodecyl sulfate. The weight ratio of the polymer material of gum arabic, gelatin, and sodium dodecyl sulfate is gum arabic:gelatin:sodium dodecyl sulfate = (20 - 40):(20 - 40):(0.2 - 0.4).

[0013] Preferably, the curing agent is glutaraldehyde.

[0014] In addition, the present invention provides a method for preparing the perfluorohexanone microcapsules, comprising the following steps:

[0015] (1) Stir the components of the first shell layer and deionized water evenly to obtain a mixed solution A; continue to stir after adding perfluorohexanone to obtain a mixed solution B;

[0016] (2) Adjust the pH of the mixed solution B to 4.5 - 5, cool down to 4 - 10°C, and then adjust the pH to 8 - 9 to obtain a mixed solution C;

[0017] (3) Add the components of the second shell layer to the mixed solution C and react for 0.5 - 2 h, then continue to react for 0.5 - 2 h after adding the components of the third shell layer, raise the temperature to 35 - 45°C, continue to react until the solution turns milky white, filter and dry to obtain the perfluorohexanone microcapsules.

[0018] Preferably, in the step (1), the mass percentage content of the mixed solution A is 1 - 2%; the defoaming agent is 0.01 - 0.02% of the absolute dry mass of the mixed solution A, and the mass of the added perfluorohexanone is 600 - 1600% of the absolute dry mass of the mixed solution A.

[0019] Preferably, the mass of the added components of the second shell layer is 70 - 200% of the absolute dry mass of the mixed solution A, and the mass of the added components of the third shell layer is 100 - 300% of the absolute dry mass of the mixed solution A.

[0020] More preferably, in the step (1), the mass percentage content of the mixed solution A is 1.3 - 2.0%; the mass of the added perfluorohexanone is 622 - 1584% of the absolute dry mass of the mixed solution A.

[0021] More preferably, the mass of the added components of the second shell layer is 75 - 198% of the absolute dry mass of the mixed solution A, and the mass of the added components of the third shell layer is 124 - 297% of the absolute dry mass of the mixed solution A.

[0022] Preferably, in the step (3), the drying temperature is 25 - 35°C and the drying time is 10 - 20 h.

[0023] In one embodiment, in the step (1), the reaction temperature of the first stirring is 35 - 45°C, the rotation speed of the first stirring is 100 - 300 rpm; the rotation speed of the second stirring is 80 - 200 rpm, and the time of the second stirring is 5 - 15 min.

[0024] In one embodiment, in the step (2), the pH of the mixed solution B is adjusted to 4.5 - 5 using a 2% acetic acid solution by mass, and then adjusted to 8 - 9 using a 5% NaOH solution by mass; the temperature is reduced to 4 - 10°C, which is achieved by using circulating coolant to rapidly cool the solution, and the time taken to reduce the temperature to 4 - 10°C is 40 - 70 min.

[0025] In one embodiment, in the step (3), the components of the second shell layer are added dropwise to the mixed solution B.

[0026] Furthermore, the present invention provides the use of the perfluorocyclohexanone microcapsules in the preparation of fireproof and / or fire extinguishing materials.

[0027] The present invention provides a fireproof and / or fire extinguishing material, in which the mass percentage content of the perfluorocyclohexanone microcapsules is 50 - 70%.

[0028] The present invention provides a fire extinguishing patch, which comprises the following components in parts by weight: 0.8 - 1 part of the perfluorocyclohexanone microcapsules and 0.7 - 1 part of a high molecular polymer.

[0029] Preferably, the method for preparing the fire extinguishing patch is as follows: the perfluorocyclohexanone microcapsules and the high molecular polymer resin are mixed evenly, coated on a release film using a coater, and after natural curing, 3M double-sided tape is attached to the front side, and then cut into the required size to obtain the fire extinguishing patch.

[0030] Preferably, the high molecular polymer is at least one of polyester, polyurethane, phenolic resin, urea-formaldehyde resin, polyurea resin, high molecular silicon, natural source polymer, acrylic resin, and epoxy resin; more preferably, the high molecular polymer is polyurea resin.

[0031] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0032] By adopting a specific core-shell structure, the perfluorocyclohexanone microcapsules prepared in the present invention are not easily damaged and agglomerated during the drying process, and have a good fire extinguishing effect. The first shell layer of the present invention is a wall material layer, the second shell layer is formed by crosslinking the curing agent with the amino and hydroxyl groups in the first layer and self-polymerizing, and the components of the third shell layer are selected to react with the active hydroxyl groups in the second shell layer using a specific 385 amino resin and self-polymerize. Finally, the perfluorocyclohexanone microcapsules prepared are not easily damaged and agglomerated during the drying process.

[0033] The present invention solves the problems in the prior art that perfluorohexanone is difficult to be solidified and loaded, has a small loading capacity, is difficult to be made into a fire extinguishing material, and is not easy to form a fire source coverage during fire extinguishing, and provides a method for preparing perfluorohexanone microcapsules; the present invention solves the technical problem that the perfluorohexanone microcapsule particles with low boiling point and dry prepared by the existing complex coacervation method agglomerate together, and provides a technology combining complex coacervation with surface modification, and prepares dry perfluoro microcapsule particles and fire extinguishing stickers. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 Optical microscope image of perfluorohexanone microcapsule-1 prepared in Example 1;

[0035] Figure 2 Figure of the combustion test chamber.

[0036] Figure 3 Fire extinguishing sticker prepared in Application Example 1. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0037] To better illustrate the purpose, technical solution and advantages of the present invention, the present invention will be further described below in conjunction with the drawings and specific embodiments. The purpose is to understand the content of the present invention in detail, rather than a limitation to the present invention. All other embodiments obtained by those of ordinary skill in the art without creative work fall within the protection scope of the present invention. The experimental reagents and instruments designed in the embodiments and comparative examples of the present invention are all common ordinary reagents and instruments unless otherwise specified, and can be obtained from commercial channels. In the embodiments and comparative examples, the experimental methods used are all conventional methods unless otherwise specified; and unless otherwise specified, the raw materials used in parallel experiments are of the same batch.

[0038] The raw materials used in the present invention are described as follows, but are not limited to the following raw materials:

[0039] 385 amino resin: Zeneca Resins (China) Co., Ltd., model CYMEL 385, content above 79%;

[0040] Polyethyleneimine: Shanghai Gaoming Chemical Co., Ltd., model 456547, content 99.8%;

[0041] Acrylic resin: Shanghai Kayin Chemical Co., Ltd., model T19-2, content 57±2%;

[0042] Epoxy resin: Guangdong Shan Jin New Materials Co., Ltd., model SJ-103, content 60%;

[0043] Silicone resin: Guangdong Lin Hua New Materials Co., Ltd., model SJ-35, content 35%;

[0044] Example 1

[0045] This embodiment provides a perfluoromethylcyclohexanone microcapsule - 1, and the preparation method is as follows:

[0046] (1) Stir the components of the first shell layer, deionized water, and defoamer (BYK - 141) evenly at 40 °C with a rotation speed of 200 rpm to obtain a mixed solution A; after adding perfluoromethylcyclohexanone, continue to stir at a rotation speed of 100 rpm for 10 min to obtain a mixed solution B;

[0047] The mass percentage of the mixed solution A is 1.3%; the defoamer is 0.01% of the absolute dry mass of the mixed solution A, and the mass of the added perfluoromethylcyclohexanone is 622% of the absolute dry mass of the mixed solution A; the components of the first shell layer are a mixture of gum arabic, gelatin, and sodium dodecyl sulfate; the weight ratio of the polymer materials of gum arabic, gelatin, and sodium dodecyl sulfate is gum arabic:gelatin:sodium dodecyl sulfate = 20:40:0.2;

[0048] (2) Adjust the pH of the mixed solution B to 4.5 - 5 with a 2% acetic acid solution, quickly cool it to 10 °C within 40 min using circulating coolant, and then adjust the pH to 8 - 9 with a 5% NaOH solution by mass to obtain a mixed solution C;

[0049] (3) Dropwise add the components of the second shell layer to the mixed solution C and react for 1 h. After adding the components of the third shell layer, continue to react for 1 h, heat up to 40 °C, continue to react until the solution turns milky white, filter, and dry at 30 °C for 15 h to obtain the perfluoromethylcyclohexanone microcapsule;

[0050] The mass of the added components of the second shell layer (curing agent - glutaraldehyde) is 75% of the absolute dry mass of the mixed solution A, and the mass of the added components of the third shell layer (385 amino resin) is 124% of the absolute dry mass of the mixed solution A.

[0051] Example 2

[0052] This embodiment provides a perfluoromethylcyclohexanone microcapsule - 2, and the difference in the preparation method from Example 1 is as follows:

[0053] The components of the first shell layer in step (1) are different. The components of the first shell layer are a mixture of gum arabic, gelatin, and sodium dodecyl sulfate; the weight ratio of the polymer materials of gum arabic, gelatin, and sodium dodecyl sulfate is gum arabic:gelatin:sodium dodecyl sulfate = 40:20:0.4.

[0054] Example 3

[0055] This embodiment provides a perfluoromethylcyclohexanone microcapsule - 3, and the difference in the preparation method from Example 1 is as follows:

[0056] In step (1), the composition of the first shell layer is different. The composition of the first shell layer is a mixture of gum arabic, chitosan, and sodium alginate. The weight ratio of the polymer materials gum arabic, chitosan, and sodium alginate is gum arabic:chitosan:sodium alginate == 20:40:0.2.

[0057] Example 4

[0058] This example provides a perfluoropentanone microcapsule - 4. The difference in the preparation method from Example 1 is as follows:

[0059] In step (1), the mass of perfluoropentanone added is different. The mass of perfluoropentanone added is 1584% of the dry mass of mixed solution A.

[0060] Example 5

[0061] This example provides a perfluoropentanone microcapsule - 5. The difference in the preparation method from Example 1 is as follows:

[0062] In step (1), the mass of perfluoropentanone added is different. The mass of perfluoropentanone added is 984% of the dry mass of mixed solution A.

[0063] Example 6

[0064] This example provides a perfluoropentanone microcapsule - 6. The difference in the preparation method from Example 1 is as follows:

[0065] In step (3), the mass of glutaraldehyde is different. The mass of the curing agent - glutaraldehyde added is 108% of the dry mass of mixed solution A.

[0066] Example 7

[0067] This example provides a perfluoropentanone microcapsule - 7. The difference in the preparation method from Example 1 is as follows:

[0068] In step (3), the mass of glutaraldehyde is different. The mass of the curing agent - glutaraldehyde added is 198% of the dry mass of mixed solution A.

[0069] Example 8

[0070] This example provides a perfluoropentanone microcapsule - 8. The difference in the preparation method from Example 1 is as follows:

[0071] In step (3), the mass of 385 amino resin added is different. The mass of 385 amino resin added is 205% of the dry mass of mixed solution A.

[0072] Example 9

[0073] This embodiment provides a perfluoromethylcyclohexanone microcapsule-9. The difference in the preparation method from that of Embodiment 1 lies in that:

[0074] In step (3), the mass of the added 385 amino resin is different, and the mass of the added 385 amino resin is 297% of the absolute dry mass of the mixed solution A.

[0075] Comparative Example 1

[0076] This comparative example provides a perfluoromethylcyclohexanone microcapsule-A. The difference in the preparation method from that of Embodiment 1 lies in that:

[0077] In step (3), the composition of the added third shell layer is different. The composition of the third shell layer is polyethyleneimine (molecular weight 400), and the mass is exactly the same.

[0078] Comparative Example 2

[0079] This comparative example provides a perfluoromethylcyclohexanone microcapsule-B. The difference in the preparation method from that of Embodiment 1 lies in that:

[0080] In step (3), the composition of the added third shell layer is different. The composition of the third shell layer is acrylic resin, and the mass is exactly the same.

[0081] Comparative Example 3

[0082] This comparative example provides a perfluoromethylcyclohexanone microcapsule-C. The difference in the preparation method from that of Embodiment 1 lies in that:

[0083] In step (3), the composition of the added third shell layer is different. The composition of the third shell layer is epoxy resin, and the mass is exactly the same.

[0084] Comparative Example 4

[0085] This comparative example provides a perfluoromethylcyclohexanone microcapsule-D. The difference in the preparation method from that of Embodiment 1 lies in that:

[0086] In step (3), the composition of the added third shell layer is different. The composition of the third shell layer is silicone resin, and the mass is exactly the same.

[0087] Comparative Example 5

[0088] This comparative example provides a perfluoromethylcyclohexanone microcapsule-E. The difference in the preparation method from that of Embodiment 1 lies in that:

[0089] In step (1), the mass of the added perfluoromethylcyclohexanone is different, and the mass of the added perfluoromethylcyclohexanone is 450% of the absolute dry mass of the mixed solution A.

[0090] Comparative Example 6

[0091] This comparative example provides a perfluoromethylcyclohexanone microcapsule - F. The difference in the preparation method from Example 1 lies in that:

[0092] In step (1), the mass of perfluoromethylcyclohexanone added is different, and the mass of perfluoromethylcyclohexanone added is 1700% of the absolute dry mass of the mixed solution A.

[0093] Performance Test - 1

[0094] The results of the morphological tests of the perfluoromethylcyclohexanone microcapsules prepared in the examples and comparative examples are shown in Table 1. Among them, Figure 1 is the optical microscope image of the perfluoromethylcyclohexanone microcapsule - 1 prepared in Example 1. It can be seen that Figure 1 the surface of the microcapsule particles is relatively smooth and plump, without damage, and there is no cross - linking between them.

[0095] Among them, the method for testing the average particle size of the perfluoromethylcyclohexanone microcapsules is as follows:

[0096] Observe whether there is agglomeration of the microcapsules with an optical microscope;

[0097] If there is no agglomeration of the microcapsules, test them by the sieving method of GB / T 21524 - 2008; if the microcapsules are agglomerated, test them by the image analysis method of GB / T 21649.1 - 2008.

[0098] The weight ratio of the core to the wall: Measured by the TGA method. Set the temperature to 200 °C. At this temperature, all the perfluoromethylcyclohexanone cores are released, while the wall remains intact. Then the remaining substance is the wall.

[0099] The test results are shown in Table 1.

[0100] Table 1

[0101]

[0102] Performance Test - 2

[0103] Application Example 1 - 9 provides a fire - extinguishing patch, which includes the following components in parts by weight: 0.8 part of the perfluoromethylcyclohexanone microcapsules described in Examples 1 - 9, and 0.7 part of polyurea resin; the preparation method is as follows: Mix the perfluoromethylcyclohexanone microcapsules and polyurea resin evenly, coat them on a release film with a coater, and after natural curing, stick 3M double - sided tape on the front side and cut them into the required size to obtain the fire - extinguishing patch.

[0104] The perfluoromethylcyclohexanone microcapsules prepared in the examples are respectively made into fire - extinguishing patches. Among them, the perfluoromethylcyclohexanone microcapsules prepared in Example 1 are applied to Application Example 1, the perfluoromethylcyclohexanone microcapsules prepared in Example 2 are applied to Application Example 2, and the perfluoromethylcyclohexanone microcapsules prepared in Example 9 are applied to Application Example 9, and so on.

[0105] To test the performance of Comparative Examples 1-4, the agglomerated microcapsules prepared in Comparative Examples 1-4 were directly cut into the size of 50mm*100mm*2mm required for testing, and were correspondingly described as Comparative Application Examples. Comparative Examples 5-6 were prepared into fire extinguishing patches consistent with the Application Examples, and were correspondingly described as Comparative Application Examples, and their performance was tested.

[0106] Test process: Stick the fire extinguishing patch (or directly cut microcapsules) with a size of 50mm*100mm*2mm on the top of a relatively enclosed 5L combustion test box (such as Figure 2 ), and place a glass dish containing 10 mL of absolute ethanol at the bottom. Close the test box, light the absolute ethanol with a lighter, record the time when the fire is extinguished and the number of times of repeated ignition and extinguishing.

[0107] Test results: As shown in Table 2.

[0108] Table 2

[0109]

[0110]

[0111] The performance test results of the Application Examples and Comparative Application Examples are shown in Table 2. Among them, Figure 3 is the fire extinguishing patch diagram of Application Example 1. The fire extinguishing patch has a flat and smooth appearance and is overall beautiful.

[0112] It can also be seen from the test results in Table 1 and Table 2 that after the microcapsules not modified by 385 amino resin are dried, they are easy to agglomerate together and it is impossible to prepare fire extinguishing patches. 385 amino resin can further crosslink with the active functional groups on the surface of the wet capsule wall material, reduce the binding force on the surface of the capsule wall material, make the capsules not easy to agglomerate during the drying process, and the fire extinguishing effect of the fire extinguishing patch is very good, and the fire can be extinguished within 5 seconds and can be extinguished multiple times.

[0113] During the multiple (within 5 times) fire extinguishing processes of the fire extinguishing patch prepared by the present invention, the fire extinguishing time difference is not large, and the fire extinguishing effect is better.

[0114] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit the protection scope of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that the technical solutions of the present invention can be modified or equivalently replaced without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. A perfluoromethylcyclohexanone microcapsule, characterized in that, It includes a core and a wall arranged in sequence. The wall includes a first shell layer, a second shell layer, and a third shell layer arranged in sequence, and the core is adjacent to the first shell layer; the average particle size of the perfluorhexanone microcapsules is 50 - 400 μm, and the weight ratio of the core to the wall is (16 - 32):1; The core includes perfluorhexanone; The components of the first shell layer include a polymer material; the polymer material is at least two of gelatin, sodium alginate, chitosan, gum arabic, polyglutamic acid, β - cyclodextrin, sodium dodecyl sulfate, sodium carboxymethyl cellulose, hydroxypropyl methyl cellulose, octenyl succinic anhydride esterified starch; The components of the second shell layer include a curing agent; the curing agent is at least one of formaldehyde, acetaldehyde, glutaraldehyde, glyoxal; The components of the third shell layer include 385 amino resin.

2. The perfluoromethylcyclohexanone microcapsule according to claim 1, wherein The components of the first shell layer also include an antifoaming agent.

3. A method for preparing a perfluoromethylcyclohexanone microcapsule according to any one of claims 1-2, characterized in that, It includes the following steps: (1) Stir the components of the first shell layer and deionized water evenly to obtain a mixed solution A; continue to stir after adding perfluorhexanone to obtain a mixed solution B; (2) Adjust the pH of the mixed solution B to 4.5 - 5, cool it to 4 - 10 °C, and then adjust the pH to 8 - 9 to obtain a mixed solution C; (3) Add the components of the second shell layer to the mixed solution C and react for 0.5 - 2 h, continue to react for 0.5 - 2 h after adding the components of the third shell layer, heat up to 35 - 45 °C, continue to react until the solution turns milky white, filter and dry to obtain the perfluorhexanone microcapsules.

4. The preparation method of the perfluorohexanone microcapsule according to claim 3, characterized in that, In the step (1), the mass percentage content of the mixed solution A is 1 - 2%; the mass of the added perfluorhexanone is 600 - 1600% of the absolute dry mass of the mixed solution A.

5. The preparation method of the perfluorohexanone microcapsules according to claim 3, characterized in that, The mass of the added components of the second shell layer is 70 - 200% of the absolute dry mass of the mixed solution A, and the mass of the added components of the third shell layer is 100 - 300% of the absolute dry mass of the mixed solution A.

6. The preparation method of the perfluorohexanone microcapsule according to claim 3, characterized in that, In the step (3), the drying temperature is 25 - 35 °C, and the drying time is 10 - 20 h.

7. Use of the perfluorhexanone microcapsules according to any one of claims 1 - 2 in the preparation of fire - prevention and / or fire - extinguishing materials.

8. A fire prevention and / or fire extinguishing material, characterized in that, In the fire - extinguishing material, the mass percentage content of the perfluorhexanone microcapsules according to any one of claims 1 - 2 is 50 - 70%.

9. A fire extinguishing patch, characterized in that, It includes the following components in parts by weight: 0.8 - 1 part of the perfluorhexanone microcapsules according to any one of claims 1 - 2, 0.7 - 1 part of a high - molecular polymer.

10. The fire extinguishing patch according to claim 9, characterized in that, The high - molecular polymer is at least one of polyester, polyurethane, phenolic resin, urea - formaldehyde resin, polyurea resin, high - molecular silicon, acrylic resin, epoxy resin.

Citation Information

Patent Citations

  • Autonomous fire-fighting agent

    CN103370104A