Preparation method for polyhydroxy functional POSS hybrid material

A hybrid material and polyhydric technology, which is applied in the field of preparation of polyhydric functional POSS hybrid materials, can solve problems such as single functionalization, and achieve the effects of avoiding biological toxicity, simple method, and high production yield

Inactive Publication Date: 2019-01-11
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This patent only prepares a single functional organic / inorganic hybrid material

Method used

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  • Preparation method for polyhydroxy functional POSS hybrid material
  • Preparation method for polyhydroxy functional POSS hybrid material
  • Preparation method for polyhydroxy functional POSS hybrid material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032]Synthesis of POSS-PEG-styrene ratio (1:2:6): 0.3g (0.3mmol) of dry mercapto POSS was added to a 100mL three-necked flask, and 0.271g (0.6mmol) of PEG- 400 and 0.188g (1.8mmol) styrene, and add 0.0060g (0.024mmol) of 2,2-dimethoxy-2-phenylacetophenone (DMPA), as the photoinitiator of the system. Add 30mL of anhydrous tetrahydrofuran and stir rapidly to fully dissolve. Seal the mouth of the bottle with a rubber stopper, and blow the mixed solution with nitrogen for 20 min. Under the condition of room temperature, put it under the ultraviolet lamp (15W) to irradiate for 1h. After the obtained mixed solution was suction filtered to remove insoluble substances, the solvent was removed by rotary evaporation to obtain a light yellow viscous liquid, which was the target product with PEG group and benzene ring group. Yield: 90.6%. See Synthetic Route 1 for the synthetic route and molecular formula. M.P = -7.9°C. FTIR (KBr): v=3415cm -1 (-OH), 2924cm -1 (-CH 2 ), 2552cm -...

Embodiment 2

[0034] The difference between this embodiment and embodiment 1 is:

[0035] The synthesis of POSS-PEG-styrene ratio is (1:3:5): in step 1), the amount of PEG-400 that is connected to acryloyl chloride at one end is 0.407g (0.9mmol) and the amount of styrene is 0.158g ( 1.5mmol), the amount of 2,2-dimethoxy-2-phenylacetophenone added (DMPA) is 0.0038g (0.024mmol), as the photoinitiator of the system. Make it fully dissolved in 20mL of anhydrous tetrahydrofuran solution. All the other are exactly the same as Example 1. Yield: 93.9%. See Synthetic Route 1 for the synthetic route and molecular formula. M.P = -7.1°C. FTIR (KBr): V=3415cm -1 (-OH), 2924cm -1 (-CH 2 )2552cm -1 (-SH)1736cm -1 (C=O)1628, 1449cm -1 (-C 6 h 5 )1110cm -1 (Si-O-Si). 1 HNMR (600MHz, CDCl 3 , 298K, δ / ppm): δ7.63(d, 25H), 4.27(s, 2H), 3.75-3.45(m, 105H), 2.51(s, 2H), 1.65(s, 2H), 0.74(s , 2H). 13 CNMR (600MHz, CDCl 3 , 298K, δ / ppm): δ172.01, 140.67, 134.47, 128.27, 126.35, 103.92, 72.55, 66....

Embodiment 3

[0037] The difference between this embodiment and embodiment 1 is:

[0038] The synthesis of POSS-PEG-styrene ratio is (1:4:4): in step 1), the amount of PEG-400 that is connected to acryloyl chloride at one end is 0.542g (1.2mmol) and the amount of styrene is 0.125g ( 1.2mmol), the amount of 2,2-dimethoxy-2-phenylacetophenone added is 0.0062g (0.024mmol), as the photoinitiator of the system. Make it fully dissolved in 20mL of anhydrous tetrahydrofuran solution. All the other are exactly the same as Example 1. Yield: 93.5%. See Synthetic Route 1 for the synthetic route and molecular formula. M.P = -6.7°C. FTIR (KBr): v=3415cm -1 (-OH), 2924cm -1 (-CH 2 ), 2552cm -1 (-SH), 1736cm -1 (C=O), 1628, 1449cm -1 (-C 6 h 5 ), 1110cm -1 (Si-O-Si). 1 HNMR (600MHz, CDCl 3 , 298K, δ / ppm): δ7.63(d, 20H), 4.27(s, 2H), 3.75-3.45(m, 140H), 2.51(s, 2H), 1.65(s, 2H), 0.74(s , 2H). 13 CNMR (150MHz, CDCl 3 , 298K, δ / ppm): δ172.01, 140.67, 134.47, 128.27, 126.35, 103.92, 72.55, 66...

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Abstract

The invention discloses a preparation method for a polyhydroxy functional POSS hybrid material. The preparation method is characterized by the following steps: adding reactants, namely, polyethylene glycol derivative PEG (C=CH2) containing unsaturated carbon-carbon double bond at one end, olefinic organism (RHC=CH2), octa-sulfydryl POSS and dissolvent into a reactor; adding radical initiator afterthe added reactants dissolve and uniformly disperse; reacting for 40min-4h under the nitrogen shielding condition at 30-80 DEG C or under an ultraviolet light condition, thereby acquiring the POSS hybrid material; removing the remained radical initiator and unreacted reactants, and drying, thereby acquiring the polyhydroxy functional POSS hybrid material. The preparation method disclosed by the invention has the advantages of simplicity in operation, easily acquired reaction materials, fast reaction and mild reaction condition. The polyhydroxy functional POSS hybrid material prepared according to the invention has the advantages of high biocompatibility, controllable hydrophily and hydrophobicity, controllable form under condensed state, multifunctional reaction group and the like.

Description

technical field [0001] The invention relates to a preparation method of a polyhydroxy functional POSS hybrid material, in particular to a polyhedral oligomeric silsesquioxane (POSS-SH) containing polymercapto functional groups, organic alkenes, water-soluble one-end unsaturated di The invention relates to a preparation method for preparing a multi-functional POSS hybrid material with specific polyhydroxyl mercapto groups by using a mercapto-ene click polymerization reaction one-step method after stirring evenly bonded PEG derivatives, a free radical initiator and a solvent, and belongs to the technical field of polymer synthesis methods. Background technique [0002] Organic-inorganic hybrid materials combine the advantages of organic and inorganic materials as a whole, and overcome the shortcomings of both to a certain extent, so they have attracted much attention in recent years. In view of the advantages of easy shape and modification of the silicon framework, the current...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/38C08G77/388
CPCC08G77/38C08G77/388
Inventor 徐洪耀赵岗于婷光善仪
Owner DONGHUA UNIV
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