Surfactant for polymerization reaction in supercritical carbon dioxide

A surfactant and polymerization reaction technology, applied in the production of bulk chemicals, chemical instruments and methods, chemical/physical processes, etc. Agent working pressure, high cost of surfactants (such as fluorine-containing surfactants and most siloxane-based surfactants, etc., to achieve the effect of ensuring low toxicity, low cost, and improving solubility

Inactive Publication Date: 2012-07-25
DALIAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these surfactants are difficult to meet the requirements for industrial polymerization
The problems faced by these surfactants in industrial production are: the cost of surfactants is expensive (such as fluorine-containing surfactants and most silicone-based surfactants), and the surfactant itself is toxic (such as fluorine-containing surfactants). Surfactants) and high working pressure (most siloxane-based surfactants and hydrocarbon surfactants, the working pressure is usually 34MPa), etc.

Method used

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  • Surfactant for polymerization reaction in supercritical carbon dioxide
  • Surfactant for polymerization reaction in supercritical carbon dioxide
  • Surfactant for polymerization reaction in supercritical carbon dioxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] (1) Synthesis of methacryloyl chloride (MAC)

[0068] Below 10°C, add 10g of methacrylic acid, 0.05g of hydroquinone and a magnetic rotor to a 100mL three-necked flask equipped with a reflux condenser, a thermometer and a constant pressure dropping funnel, and slowly add them dropwise from the dropping funnel while stirring. 9 g thionyl chloride. Slowly raise the temperature until the reaction starts, and continue to raise the temperature to 60°C until the reaction is complete after the reaction rate decreases. Use 5% NaOH solution to absorb the HCl and SO generated in the reaction 2 gas. The crude product is distilled twice, the product at 87-103°C is collected in the first distillation, and the product at 95-96°C is collected in the second distillation, which is high-purity MAC.

[0069] (2) Condensation of hydroxyl silicone oil and γ-aminopropyldimethoxymethylsilane

[0070] The reaction was carried out in a 100mL three-neck flask equipped with a reflux condenser...

Embodiment 2

[0076] In this embodiment, the polysiloxane-based surfactant of the present invention is applied to the dispersion polymerization reaction of methyl methacrylate (hereinafter referred to as MMA) in supercritical carbon dioxide.

[0077] MMA in ScCO 2 The dispersion polymerization in was carried out in a 50mL stainless steel reactor. The reactor was cleaned with DMC before the experiment. Add 5 g of MMA, 0.05 g of AIBN, 0.15 g of polysiloxane surfactant and a polytetrafluoroethylene rotor into the reactor, and seal the reactor. Slow passage of CO 2 After 5 minutes, heat and turn on the plunger pump to pressurize the system. When the experimental temperature reaches 65°C and the reaction pressure reaches 16MPa, start the stirrer and react for 4 hours. Stop heating and stirring, use an ice-water bath to cool the reaction kettle to room temperature, and slowly release the gas to normal pressure. Open the reactor to collect the white powdery product, which is the synthesized po...

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Abstract

The invention relates to a polysiloxane based surfactant for polymerization reaction in supercritical carbon dioxide, which is structurally represented as: (see the original text), wherein, p ranges from 7 to 13, q ranges from 7-13, n ranges from 12-17, and the number-average molecular weight of the surfactant ranges from 10KDa to 50KDa. The preparation method for the polysiloxane based surfactant includes the steps: firstly, carrying out a condensation reaction between low molecular weight hydroxy silicone oil and gamma-aminopropyl dimethoxymethyl-silane to generate a double-amino-terminated polysiloxane intermediate; then reacting the polysiloxane intermediate with methacryloyl chloride to generate a methacrylamide based polysiloxane macromonomer; and finally, generating the polysiloxane based surfactant under initiation of the azodiisobutyronitrile and by means of free radical polymerization.

Description

technical field [0001] The product of the invention is suitable for polymerization in supercritical carbon dioxide, and can be used for the synthesis of biological materials, high-purity polymers and other functional materials. technical background [0002] Supercritical carbon dioxide (ScCO 2 ) has the characteristics of non-toxic, non-polluting, non-combustible, inert chemical reaction and low price. Moreover, it has good solubility to non-polar organic small molecules, has good swelling effect on polymers, can lower the glass transition temperature of polymers, and is beneficial to the progress of polymerization reaction. After the reaction is completed, the CO can be decompressed 2 Separated from the system, and during decompression, ScCO 2 The unique extraction function can extract unreacted monomers, initiators and surfactants, avoiding the cumbersome post-processing procedures in traditional processes. Therefore using ScCO 2 Replacing toxic and volatile organic s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F299/08C08G77/38C08G77/388B01F17/54C08F120/14C09K23/54
CPCY02P20/54
Inventor 詹世平任建鹏
Owner DALIAN UNIV
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