Preparation method for and application of modified siloxane-based supercritical carbon dioxide thickener

Patent metadata

Field	Value
Publication number	US-12030994-B2
Application number	US-202218025666-A
Country	US
Kind code	B2
Filing date	Jul 28, 2022
Priority date	Oct 26, 2021
Publication date	Jul 9, 2024
Grant date	Jul 9, 2024

Abstract

A preparation method for and an application of a modified siloxane-based supercritical carbon dioxide thickener are disclosed. The method includes the following steps: using 1,3-diallyl-1,3,5-triazine-2,4,6-trione as a polymerization monomer, and dropwise adding 1,3,5,7-tetramethylcyclotetrasiloxane for hydrosilylation in the presence of a catalyst to obtain a modified siloxane polymer. The obtained modified siloxane polymer is directly used as a supercritical carbon dioxide thickener without purification post-treatment; when in use, the modified siloxane polymer is prepared into a solution with a concentration of 1-2%, has an excellent thickening effect with no cosolvent required, and has high solubility in carbon dioxide and high temperature resistance.

First claim

What is claimed is:

1. A preparation method for a modified siloxane-based supercritical carbon dioxide thickener, comprising the following steps:
adding 1,3-diallyl-1,3,5-triazine-2,4,6-trione into a reactor, stirring and heating to 60-120° C., adding chloroplatinic acid as a catalyst and keeping the catalyst activated for 1-3 h, wherein a catalyst activation temperature is 60-100° C.;
adding dropwise 1,3,5,7-tetramethylcyclotetrasiloxane, wherein a molar ratio of carbonyl groups of the 1,3-diallyl-1,3,5-triazine-2,4,6-trione to active hydrogens of the 1,3,5,7-tetramethylcyclotetrasiloxane is (1-4):1; and
conducting hydrosilylation at 70-110° C. to obtain a modified siloxane polymer (SBD), wherein the SBD is the modified siloxane-based supercritical carbon dioxide thickener.

2. The preparation method for the modified siloxane-based supercritical carbon dioxide thickener of claim 1 , wherein the molar ratio of the carbonyl groups of the 1,3-diallyl-1,3,5-triazine-2,4,6-trione to the active hydrogens of the 1,3,5,7-tetramethylcyclotetrasiloxane is (1-2): 1.

3. The preparation method for the modified siloxane-based supercritical carbon dioxide thickener of claim 1 , wherein:
the catalyst activation temperature is 80-90° C.; and
a hydrosilylation temperature is the same as the catalyst activation temperature.

4. The preparation method for the modified siloxane-based supercritical carbon dioxide thickener of claim 1 , wherein dose of the chloroplatinic acid as the catalyst is 25-60 ppm.

5. The preparation method for the modified siloxane-based supercritical carbon dioxide thickener of claim 1 , wherein a hydrosilylation time is 2-20 h.

6. The preparation method for the modified siloxane-based supercritical carbon dioxide thickener of claim 1 , wherein the modified siloxane polymer has a weight-average molecular weight of 8,000-11,000.

7. The modified siloxane-based supercritical carbon dioxide thickener of claim 1 , having a structure shown in formula I:

wherein n=17-24.

8. The modified siloxane-based supercritical carbon dioxide thickener of claim 2 , having a structure shown in formula I:

wherein n=17-24.

9. The modified siloxane-based supercritical carbon dioxide thickener of claim 3 , having a structure shown in formula I:

wherein n=17-24.

10. The modified siloxane-based supercritical carbon dioxide thickener of claim 4 , having a structure shown in formula I:

wherein n=17-24.

11. The modified siloxane-based supercritical carbon dioxide thickener of claim 5 , having a structure shown in formula I:

wherein n=17-24.

Assignees

• Univ China Petroleum East China

Inventors

• Wang Yanling
• Liu Bin
• Sun Baojiang
• Liang Lei
• Li Di

Classifications

• B01J23/42

  Platinum · CPC title

• Y02P20/54

  using solvents, e.g. supercritical solvents or ionic liquids · CPC title

• C09K8/885

  obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds · CPC title

• C09K8/68

  containing organic compounds · CPC title

• C08G77/50 Primary

  by carbon linkages · CPC title