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Preparation method of microencapsulated pentaerythrite

A pentaerythritol and microencapsulation technology, which is applied in the preparation of microencapsulated flame retardants and microencapsulated pentaerythritol, can solve problems such as technical difficulties in microencapsulation, achieve broad market prospects, improve water resistance, and evenly disperse Effect

Inactive Publication Date: 2015-01-14
安徽长正升科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, as the carbon source pentaerythritol in the halogen-free flame retardant is an important part of the intumescent flame retardant, its microencapsulation technology is difficult, and there is no public report on its microencapsulation preparation process.

Method used

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  • Preparation method of microencapsulated pentaerythrite
  • Preparation method of microencapsulated pentaerythrite
  • Preparation method of microencapsulated pentaerythrite

Examples

Experimental program
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Effect test

Embodiment 1

[0026] (1) Preparation of melamine-formaldehyde resin prepolymer

[0027] Take 2.5mL of distilled water, 10g of melamine, and 25mL of 37% formaldehyde solution, mix them evenly, and put them into a 250mL three-neck round bottom flask, adjust the pH to 8~9 with 10% sodium carbonate solution, heat to 50°C, and keep warm for 1h; The solution system is placed in a rotary evaporator, and rotated at 40~45°C for 0.5h to remove 10% of the water to obtain a melamine-formaldehyde resin prepolymer solution for later use;

[0028] (2) Pentaerythritol microencapsulation

[0029] Weigh 12 g of pentaerythritol micron powder (about 2~10 μm), disperse in 150 mL of acetone, then add the prepolymer solution prepared above while stirring, then heat to 55 ° C, react at constant temperature for 4 h, filter, wash, and dry to obtain Microencapsulated pentaerythritol.

[0030] The solubility of microencapsulated pentaerythritol at 13°C is only 0.2 g / 100mL.

Embodiment 2

[0032] (1) Preparation of melamine-formaldehyde resin prepolymer

[0033] Take 5mL of distilled water, 10g of melamine, and 25mL of 37% formaldehyde solution, mix them evenly, and add them into a 250mL three-necked round bottom flask, adjust the pH to about 8~9 with 10% sodium carbonate solution, heat to 55°C, and keep warm for 1.5h; keep warm 1~2h; place the mixed solution system in a rotary evaporator, and rotate it at 40~45°C for 0.8h, remove 20% of the water, and obtain the melamine-formaldehyde resin prepolymer solution, which is ready for use;

[0034] (2) Pentaerythritol microencapsulation

[0035] Weigh 60g of pentaerythritol micron powder (2~10μm), disperse in 150 mL of acetone, then add it into the prepolymer solution prepared above while stirring, then heat to 50°C, react at constant temperature for 4.5h, filter, wash, and dry. Microencapsulated pentaerythritol was obtained.

[0036] The solubility of microencapsulated pentaerythritol at 13°C is only 0.6g / 100mL. ...

Embodiment 3

[0038] (1) Preparation of melamine-formaldehyde resin prepolymer

[0039] Take 4mL of distilled water, 10g of melamine, and 25mL of 37% formaldehyde solution and mix them evenly, and add them into a 250mL three-necked round-bottomed flask, adjust the pH to about 8~9 with 10% sodium carbonate solution, heat to 65°C, and keep warm for 2 hours; the mixed solution The system is placed in a rotary evaporator, and rotated at 40-45°C for 1 hour to remove 50% of the water, and the melamine-formaldehyde resin prepolymer solution is obtained, which is set aside.

[0040] (2) Pentaerythritol microencapsulation

[0041] Weigh 40g of pentaerythritol micron powder (2~10μm), disperse it in 150mL of absolute ethanol, then add it into the prepolymer solution prepared above while stirring, then heat to 60°C, react at constant temperature for 5h, filter, wash, and dry. Microencapsulated pentaerythritol was obtained.

[0042] The solubility of microencapsulated pentaerythritol at 13°C is only 0...

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Abstract

The invention provides a preparation method of microencapsulated pentaerythrite. The preparation method comprises the following steps of: adding melamine into a formaldehyde solution with the mass percentage of 36-37%, adjusting the pH value of a system to 8-9, heating to 50-65 DEG C, and keeping the temperature for 1-2hours; placing the mixed solution system in a rotary evaporator, carrying out rotary evaporation at the temperature of 40-45 DEG C for 0.5-1hour, and removing 10-50% of water to obtain a melamine and formaldehyde resin prepolymer solution; and dispersing pentaerythrite micropowder into acetone, adding the prepared prepolymer solution under stirring, heating to 50-60 DEG C, reacting at constant temperature for 4-5hours, filtering, cleaning and drying to obtain the microencapsulated pentaerythrite. The microencapsulated pentaerythrite prepared by the invention not only has the property of a carbon source of the pentaerythrite, but also has the function of an air source of the pentaerythrite. The microencapsulated pentaerythrite is applied to various expansive type flame-retardant high-polymer materials and not only can be used for improving the water resistance and the flame retardance of a composite material, but also can be used for ensuring that an additive is more uniformly dispersed in the high-polymer materials so as to have a wide market prospect.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and relates to a preparation method of a microencapsulated flame retardant, in particular to a preparation method of a microencapsulated pentaerythritol. Background technique [0002] With the rapid development of industrial technology of polymer materials, its use has penetrated into all sectors of the national economy and all areas of people's lives, and has become the four pillar materials alongside steel, wood, and cement. With the development of modern science and technology, the requirements for the fire and flame retardant properties of polymer materials are getting higher and higher. Flame retardant is an additive used to improve the flame retardancy of polymer materials. According to the type of flame retardant elements, flame retardants can be divided into halogen-based, organic-phosphorus-based, inorganic-phosphorus-based, halogen-phosphorus-based, nitrogen-based , phosphoru...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K9/10C08K5/053C08G12/32
Inventor 张哲高淑玲陶镜合赵子聪许俊魏博王小亮雷自强
Owner 安徽长正升科技有限公司