Method for preparing microencapsulation molybdenate

A technology of microencapsulation and molybdate, which is applied in the field of preparation of surface treatment of nanomaterials, can solve the problems of long cycle and achieve high yield, good modification effect and good dispersibility

Inactive Publication Date: 2009-09-30
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, there are few literature reports on the surface organic modification of molybdate, but related to it, Wang Guancai et al. published "Preparation, Characterization and Application of Microencapsulated Ammonium Phosphomolybdate in UPR" in "Fine Chemical Industry". Research on Flame Retardant and Smoke Suppressive Performance of "Phoenix", in which melamine resin is used for coating. After the prepolymer is added, it is first reacted at pH = 2.5 for 3 hours, then the pH is adjusted to 6, and the aging is continued for 12 hours. It can be said that the whole reaction process has a long cycle

Method used

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  • Method for preparing microencapsulation molybdenate

Examples

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Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1: Utilize the present invention to prepare microencapsulated calcium molybdate.

[0017] The first step: configure 1M sodium molybdate aqueous solution and 1M calcium chloride aqueous solution respectively;

[0018] Step 2: Add 50ml of 1M calcium chloride aqueous solution dropwise to 50ml of 1M sodium molybdate aqueous solution at 20°C, keep the pH at 6, and react for 15 minutes;

[0019] Step 3: Mix 2 g of melamine and 3.9 formaldehyde solution, react at pH=9-9.5, 85°C for 30 minutes, and prepare a prepolymer;

[0020] Step 4: Add 0.1 g of potassium persulfate and the above-mentioned prepolymer to the reaction product of the third step, adjust the pH value to 5.5, control the temperature at 55°C, and react for 2 hours;

[0021] Step 5: Suction filter the above reaction solution, and wash with water for 3 times;

[0022] Step 6: After washing, dry at 60°C to obtain microencapsulated calcium molybdate without grinding.

Embodiment 2

[0023] Embodiment 2: Utilize the present invention to prepare microencapsulated calcium molybdate.

[0024] The first step: configure 1M sodium molybdate aqueous solution and 1M calcium chloride aqueous solution respectively;

[0025] Step 2: Add 0.3g OP-10 to 50ml of 1M sodium molybdate aqueous solution and stir evenly;

[0026] Step 3: Slowly pour 50ml of 1M calcium chloride aqueous solution into the mixture in the second step at 60°C, keep the pH at 9, and react for 15 minutes;

[0027] Step 4: Mix 2 g of melamine and 3.9 formaldehyde solution, and react for 30 minutes at pH=9-9.5, 85°C to prepare a prepolymer;

[0028] Step 5: Add 0.1 g of potassium persulfate and the above-mentioned prepolymer to the reaction product of the third step successively, adjust the pH value to 5.5, control the temperature at 55°C, and react for 2 hours;

[0029] Step 6: Suction filter the above reaction solution, and wash with water for 3 times;

[0030] Step 7: After washing, dry at 60°C to...

Embodiment 3

[0032] Embodiment 3: Utilize the present invention to prepare microencapsulated calcium molybdate.

[0033] The first step: configure 3M sodium molybdate aqueous solution and 3M calcium chloride aqueous solution respectively;

[0034] The second step: add 0.3g polyethylene glycol 400 to 50ml of 3M sodium molybdate aqueous solution, and stir evenly;

[0035] Step 3: Slowly pour 50ml of 3M calcium chloride aqueous solution into the mixture in the second step at 60°C, keep the pH at 6, and react for 15 minutes;

[0036] Step 4: Mix 3 g of melamine and 6.0 g of formaldehyde solution, react at pH=9-9.5, 85°C for 30 minutes, and prepare a prepolymer;

[0037] Step 5: Add 0.2 g of sodium persulfate and the above-mentioned prepolymer to the reaction product of the third step successively, adjust the pH value to 5, control the temperature at 60°C, and react for 2 hours;

[0038] Step 6: Suction filter the above reaction solution, and wash with water for 3 times;

[0039] Step 7: Aft...

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Abstract

The invention discloses a method for preparing microencapsulation molybdenate, which comprises the following steps: preparing a soluble molybdenate aqueous solution and a soluble metal salt aqueous solution respectively, adding the soluble metal salt aqueous solution into the soluble molybdenate aqueous solution at a temperature of between 20 and 80 DEG C, and controlling the pH to between 6 and 9 to react for 15 minutes to 1 hour; mixing melamine and a formaldehyde solution, and reacting for 30 minutes at a temperature of 85 DEG C with the pH value being equal to 9 to 9.5 to prepare a preformed polymer; adding soluble persulfate as an initiator and the preformed polymer into reactants in the third step successively, controlling the temperature to between 55 and 80 DEG C, and carrying out reaction for 2 to 4 hours; and performing suction filtration on the reaction solution, washing the reaction solution with water repeatedly, and drying the reaction solution to obtain the microencapsulation molybdenate without grinding. The method has short preparation process cycle and high yield, the decomposition temperature of cladding resin is more than 400 DEG C, and the dispersity of the cladding resin is good. Thus, the method is applicable to processing high polymer with relatively higher temperature requirement.

Description

technical field [0001] The invention relates to a preparation method for surface treatment of nanometer materials, in particular to a preparation method for microencapsulated molybdate. Background technique [0002] Molybdenum compounds are commonly used excellent flame retardant and smoke suppressants. At present, molybdenum trioxide and ammonium octamolybdate are used in the largest amount, which have been widely used in flame retardancy and smoke suppression of PVC, rubber, fiber, etc. They can catalyze polymers to form trans polyenes in the condensed phase by a Lewis acid mechanism, so that the polymers cannot be cyclized to form aromatic ring structures, increase the amount of char formation, increase the oxygen index, reduce flammable components, and reduce smoke generation Speed ​​and density, so as to achieve the purpose of flame retardancy and smoke suppression. [0003] Since Claymarks Molybdenum Company developed α-molybdenum trioxide flame retardant and smoke s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/00B01J13/02
Inventor 汪信蒋文俊杨绪杰刘孝恒陆路德吴汾韩巧凤朱俊武江晓红郝青丽徐超杨福兴
Owner NANJING UNIV OF SCI & TECH
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