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Method for preparing compound ADC (azodicarbonamide) foaming agents with nano-particles

A technology of ADC foaming agent and nanoparticle, which is applied in the field of preparation of nanoparticle compound ADC foaming agent, can solve problems such as equipment corrosion and difficult treatment of waste water, and achieve high quality, large foaming amount, and high decomposition temperature. Effect

Inactive Publication Date: 2017-03-08
衡阳市锦轩化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of biurea by acid method and weak base method is to add a large amount of acid to the reaction system to adjust the pH value of the system, which will seriously corrode the equipment and make the waste water difficult to treat.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The preparation method of nanoparticle composite ADC blowing agent, comprises the steps:

[0026] (1) Synthesis of biurea

[0027] Add hydrazine hydrate and urea into the four-neck flask, reflux at 100 °C until white precipitates appear, and continue to react for 9 h; cool to room temperature, filter with suction, dry the filter cake at 55 °C for 25 h to obtain a white solid, and measure the filtrate by spectrophotometry Medium urea content;

[0028] (2) Synthesis of ADC

[0029] In the four-necked flask, add biurea, main catalyst sodium bromide, procatalyst V 2 o 5 , urea, EDTA, deionized water, heated to 65 ℃, with 10wt% H 2 SO 4 Adjust the pH value of the reaction system to 2, add 30wt% hydrogen peroxide dropwise at a rate of 0.24mL / min, after 1.5h, keep the reaction for 7h, cool, filter with suction, and dry the filter cake at 52°C for 25h to obtain an orange-yellow solid;

[0030] (3) Nano ZnO-SiO 2 Powder preparation

[0031] Dissolve zinc acetate dihydra...

Embodiment 2

[0035] The preparation method of nanoparticle composite ADC blowing agent, comprises the steps:

[0036] (1) Synthesis of biurea

[0037] Add hydrazine hydrate and urea into the four-neck flask, reflux at 101 °C until white precipitates appear, and continue to react for 10 h; cool to room temperature, filter with suction, and dry the filter cake at 60 °C for 25 h to obtain a white solid, and use spectrophotometry to determine the filtrate Medium urea content;

[0038] (2) Synthesis of ADC

[0039] In the four-necked flask, add biurea, main catalyst sodium bromide, procatalyst V 2 o 5 , urea, EDTA, deionized water, heated to 65 ℃, with 10wt% H 2 SO 4 Adjust the pH value of the reaction system to 3, add 30wt% hydrogen peroxide dropwise at a rate of 0.26mL / min, after 1.7 hours, keep the reaction for 7.5 hours, cool, filter with suction, and dry the filter cake at 53°C for 25-27 hours to obtain orange yellow solid;

[0040] (3) Nano ZnO-SiO 2 Powder preparation

[0041] D...

Embodiment 3

[0045] The preparation method of nanoparticle composite ADC blowing agent, comprises the steps:

[0046](1) Synthesis of biurea

[0047] Add hydrazine hydrate and urea into the four-neck flask, reflux at 102 °C until white precipitates appear, and continue to react for 10 h; cool to room temperature, filter with suction, dry the filter cake at 65 °C for 26 h to obtain a white solid, and measure the filtrate by spectrophotometry Medium urea content;

[0048] (2) Synthesis of ADC

[0049] In the four-necked flask, add biurea, main catalyst sodium bromide, procatalyst V 2 o 5 , urea, EDTA, deionized water, heated to 65 ℃, with 10wt% H 2 SO 4 Adjust the pH of the reaction system to 3, add 30wt% hydrogen peroxide dropwise at a rate of 0.27mL / min, after 2 hours, keep the reaction for 8 hours, cool, filter with suction, and dry the filter cake at 54°C for 27 hours to obtain an orange-yellow solid;

[0050] (3) Nano ZnO-SiO 2 Powder preparation

[0051] Dissolve zinc acetate ...

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PUM

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Abstract

The invention discloses a method for preparing compound ADC (azodicarbonamide) foaming agents with nano-particles. The method includes steps of (1), synthesizing biurea; (2), preparing ADC; (3), preparing ZnO-SiO2 nano-powder; (4), proportionally mixing the ZnO-SiO2 nano-powder and the ADC which is a foaming agent with each other to obtain mixtures, and sufficiently grinding the mixtures. The method has the advantages that excellent activation effects can be realized by the compound ADC foaming agents with the nano-particles, and accordingly the quality of products can be greatly improved.

Description

technical field [0001] The invention relates to the technical field of foaming agents, in particular to a method for preparing a foaming agent compounded with nanoparticles. Background technique [0002] Foaming agent ADC (chemical name: azodicarbonamide) is a non-toxic, odorless, non-polluting, orange-yellow azo foaming agent. Its biggest feature is that the molecule contains -N=N- structure, It can release a large amount of N2 when heated, and the gas generation volume can reach 200 ~ 250 mL / g. It is a widely used chemical blowing agent. The decomposition temperature of pure foaming agent ADC is 195 ~ 220 ℃, which is far beyond the plasticizing temperature of PVC resin (about 165 ~ 170 ℃), so it is necessary to add an activator to the foaming agent ADC to reduce the decomposition of the foaming agent ADC Temperature, in order to meet the processing requirements of PVC resin. Zinc ions in zinc oxide have the ability to accept lone pair electrons, and can accept lone pair ...

Claims

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Application Information

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IPC IPC(8): C08J9/10
CPCC08J9/103C08J2203/04
Inventor 罗小平张群志陈新文贺军朱志宏
Owner 衡阳市锦轩化工有限公司
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