Hydrolysis resistant organomodified trisiloxane surfactants
A technology of organosilicon and composition, applied in the field of hydrolysis-resistant trisiloxane surfactants
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preparation Embodiment 1
[0143] 1,5-Di-tert-butyl-1,1,3,5,5, pentamethyltrisiloxane (Figure 1, Structure 1).
[0144] 100g tBuMe 2 SiCl and 46g MeHSiCl 2 Dissolve in 150ml isopropyl ether (IPE) and place in addition funnel. Charge 150 g of water and 250 ml of IPE with a mechanical stirrer, reflux condenser, and N 2 Imported 1 liter round bottom flask. Chlorosilane was added dropwise via addition funnel at room temperature (23° C.) over 1 h. After the addition was complete, the temperature was adjusted to 70° C. and the reaction was carried out at reflux temperature for 20 h, the progress was monitored by GC (88% yield at 20 h). At the end of the reaction, the water was drained through a separatory funnel. The liquid was washed three times with 100 g of water each time. 25g NaHCO 3 Mix with 100 g of water and slowly add to the mixture and stir for 30 minutes. The water was drained again and dried over sodium sulfate. After filtration, the IPE was stripped off in a rotary evaporator and the cru...
preparation Embodiment 2
[0150] 1,5-Bis(isopropyl)-1,1,3,5,5, pentamethyltrisiloxane (Figure 2, structure 2).
[0151] 25g iPrMe 2 SiCl (0.183 mol) and 13.1 g MeHSiCl 2 (0.114 mol) was dissolved in 80 ml isopropyl ether (IPE) and placed in the addition funnel. Charge 50 g of water and 100 ml of IPE with a mechanical stirrer, reflux condenser, and N 2 Imported 500ml round bottom flask. The chlorosilane was added dropwise via the addition funnel at room temperature (23° C.) over 40 minutes. After the addition was complete, the temperature was adjusted to 80° C. and the reaction was carried out at reflux temperature for 4 h, the progress was monitored by GC (75% yield at 4 h). At the end of the reaction, the water was drained through a separatory funnel. The liquid was washed three times with 80 g of water each time. 25g NaHCO 3 Mix with 100 g of water and slowly add to the mixture and stir for 30 minutes. The water was drained again and dried over sodium sulfate. After filtration, the IPE was s...
preparation Embodiment 3
[0157] The hydride intermediates of Examples 1-2 were further modified with various allyl polyoxyalkylenes to obtain organomodified trisiloxane surfactant compositions of the present invention (Table 1), as well as comparative trisilicon Oxylkane surfactants (from Table 2).
[0158] The organomodified trisiloxane surfactant compositions of the present invention are prepared by the conventional method of platinum-mediated hydrosilylation reactions, as described in US Patent 3,299,112 to Bailey, which is incorporated herein by reference.
[0159] Table 1 provides a description of the compositions of the present invention. Some of these compositions are described by the following structures:
[0160] m * D'M *
[0161] where M * = R 1 Si(CH 3 ) 2 o 0.5 ;
[0162] D'=OSi(CH 3 )CH 2 CH(R 32 )CH 2 O-(CH 2 CH 2 O) r -(CH 2 CH 2 O) s R 33
[0163] where R 1 , R 32 , R 33 , the subscripts r and s are as described in Table 1.
[0164] Table 1 - Description of o...
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