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Supercritical carbon dioxide (CO2) foaming nucleating agent and preparation method thereof

A technology of foaming nucleating agent and carbon dioxide, which is applied in the production of bulk chemicals, etc., to achieve the effects of simple preparation process, improved nucleation efficiency, and easy control

Inactive Publication Date: 2013-02-06
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, modifying the porous material and using the CO 2 Substance modification to have dual nucleation sites as supercritical CO for polymers 2 Foaming nucleating agent, there is no research report on this aspect

Method used

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  • Supercritical carbon dioxide (CO2) foaming nucleating agent and preparation method thereof
  • Supercritical carbon dioxide (CO2) foaming nucleating agent and preparation method thereof
  • Supercritical carbon dioxide (CO2) foaming nucleating agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Synthesize ordered mesoporous silica with CTAB as a template: take 1 g CTAB and 500 mL distilled water, stir well; weigh 0.32g NaOH to adjust the pH to 12; gradually increase the temperature to 80℃, and dissolve the NaOH; 18g positive Ethyl silicate as a silicon source was added dropwise to the system. After the dropping, the hydrolysis reaction was carried out with heat preservation and stirring for 6 hours. The resulting suspension was refluxed and washed with a mixed solvent of concentrated hydrochloric acid and methanol with a volume ratio of 80:500 to remove the template, and the solid was separated and dried. 3g of mesoporous silica (such as figure 1 a) and b)).

[0035] 1g of mesoporous silica and 3g of KH550 were added to 200mL of toluene, and reacted for 24 hours under reflux conditions for modification and modification. After the reaction, the solid was obtained by centrifugation, and the modified powder was obtained after drying. Add 1g of modified powder to 200...

Embodiment 2

[0037] Hydrothermal synthesis of porous titanium dioxide: prepare a hydrochloric acid solution with a pH of 2.0, measure 350ml, add 50ml of glycerin, mix well to obtain a mixed solution with a volume ratio of 7:1, respectively measure 40ml in 10 hydrothermal reactors , Add 600mg of titanium tetrafluoride weighed to each fluorine, stir well; hydrothermally react at 155℃ for 20 hours, after which, take out the reaction solution for centrifugation, wash twice with ethanol, and vacuum dry at 60℃ for 10 hours to obtain the product Porous titanium dioxide.

[0038] 0.5 g of porous titanium dioxide and 1 g of KH550 were added to 200 mL of toluene and reacted for 24 hours under reflux conditions for modification and modification. After the reaction, the solid was obtained by centrifugation, and the modified powder was obtained after drying. Add 1g of modified powder to 300mL of dichloromethane and 20mL of triethylamine after dewatering. After stirring evenly, add 9mL of 2-bromoisobutyryl...

Embodiment 3

[0042] Take 0.15g of the nucleating agent prepared in Example 1 and 4.85g of GPPS, disperse and dissolve them in 25mL DMF, precipitate the precipitate with 300mL methanol, and filter the filter cake at 120 o Vacuum drying at C, the dried sample is mixed uniformly under the twin-screw extrusion of the micro mixer, at 200 o C extrudes the material, and obtains a spline after drawing. Spline is made into 5mm*5mm foam samples for supercritical CO 2 Foaming experiment. Place the sample in the autoclave and use supercritical CO first 2 Flush the system with fluid, purge the air, and heat up the system to 120 after sealing the device o Saturation temperature of C, injected CO 2 Saturate the fluid to a saturation pressure of 13.8 MPa for 10 hours, then quickly release the pressure and place it in an ice water room to cool and shape it to obtain a polymer foam material. Frozen and brittle the foamed material with liquid nitrogen and perform scanning electron microscopy analysis, such as ...

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Abstract

The invention discloses a preparation method of a supercritical carbon dioxide (CO2) foaming nucleating agent. The preparation method comprises the steps that porous silica or porous titania and a modifying reagent are subjected to a modification reaction in a toluene solvent under the condition of heating reflux, and modified powder is obtained after the reaction is completed; the modified powder reacts with an initiator and triethylamine in an anhydrous dichloromethane solvent at a normal temperature in a nitrogen atmosphere for 12 to 24 hours, and powder loaded with the initiator is prepared after the reaction is completed; a CuBr catalyst and a pentamethyl diethylene triamine ligand are added to the powder loaded with the initiator and ionic liquid in an anhydrous acetonitrile solvent to conduct a graft polymerization reaction at a temperature of 110 to 120 DEG C in a nitrogen atmosphere for 24 to 36 hours; and after the reaction, a reaction solution is post-processed to obtain the supercritical CO2 foaming nucleating agent. Material of the nucleating agent prepared according to the preparation method has a certain CO2-friendly substance loading amount, so that the CO2 adsorption capacity is improved, nucleation energy can be well reduced, the nucleation efficiency is improved, the cell size of a polymer foaming material is reduced, and the cell density is increased.

Description

(1) Technical field [0001] The invention relates to the synthesis of a supercritical carbon dioxide foaming nucleating agent, in particular to a method for synthesizing nano particles containing a porous structure and a carbon dioxide-philic substance. (2) Background technology [0002] The polymer supercritical carbon dioxide foaming method is an environmentally friendly method for preparing lightweight and high-strength materials. Supercritical CO 2 The fluid has the properties of non-toxic and non-flammable, clean, cheap, and easy to reach the critical state. It is a green and environmentally friendly foaming agent; but its fluid is easy to diffuse, has poor solubility in polymers, and has some disadvantages such as low nucleation efficiency. It is difficult to prepare foamed materials with high cell density and low material density. [0003] From the foaming process of the polymer (nucleation, cell growth, cell aggregation and shaping), it can be known that the nucleation proc...

Claims

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Application Information

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IPC IPC(8): C08F292/00C08F220/18C08F226/06C08J9/12C08L25/06C08L67/04C08L33/12C08L77/00
CPCY02P20/54
Inventor 杨晋涛黄凌琪陈枫钟明强
Owner ZHEJIANG UNIV OF TECH
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