Preparation of Organosilicon Copolymer Surfactant

Mar 25, 2021

The embodiments of the present invention will be described in detail below in conjunction with examples, but those skilled in the art will understand that the following examples are only used to illustrate the present invention and should not be regarded as limiting the scope of the present invention. If specific conditions are not indicated in the examples, it shall be carried out in accordance with the conventional conditions or the conditions recommended by the manufacturer. The reagents or instruments used without the manufacturer's indication are all conventional products that can be obtained on the market.
Example 1 Preparation of organosilicon copolymer surfactant
In a 500ml four-neck flask with a fixed device, constant temperature function, mechanical stirring, thermocouple and nitrogen gas, 350g of butanol is added to the allyl chloride terminated with an average molecular weight of 2100 allyl polyoxyethylene Ether, the polyoxyethylene ether contains 45% by mole of ethylene oxide group and 55% by mole of propylene oxide, and then 150g of low hydrogen polysiloxane (0.15% of hydrogen) Put it into a four-necked flask, start stirring, use a heating mantle to heat to 80°C, stir for 5 minutes, add chloroplatinic acid ethanol solution, add chloroplatinic acid ethanol solution, make the concentration of chloroplatinic acid in the entire reaction system 15ppm. After reacting for 3 hours, a clear and transparent light yellow liquid is obtained, which is a silicone copolymer surfactant. The hydroxyl value is 0 according to the test of GB/T 7383-2007.

In a 500ml four-necked flask with a fixed device, constant temperature function, mechanical stirring, thermocouple and nitrogen gas, add 350g of triethylene glycol methyl ether and start with methallyl chloride with an average molecular weight of 1,900. Polyoxyethylene ether, polyoxyethylene ether contains 40% mole percent of ethylene oxide groups and 60% mole percent of propylene oxide groups, and then 150g of low hydrogen-containing polysiloxane (with a hydrogen content of 0.15 %) into a four-necked flask, start stirring, use a heating mantle to heat to 80 ℃, stir for 5 minutes, add chloroplatinic acid ethanol solution, after adding chloroplatinic acid ethanol solution, so that the concentration of chloroplatinic acid in the entire reaction system is 15ppm. After reacting for 3 hours, a clear and transparent light yellow liquid is obtained, which is a silicone copolymer surfactant. The hydroxyl value is 0 according to the test of GB/T 7383-2007.

The silicone copolymer surfactants prepared in Examples 1-4 were used to prepare rigid polyurethane foams as Groups 1-4; at the same time, commercially available silicones L-6900 and B-8545 were used as controls 1-2 to prepare rigid polyurethane foams. High-quality polyurethane foam, the raw materials used are shown in Table 1
Table 1 Preparation of rigid polyurethane foam
Among them, PIR board combination polyether contains polyether polyol, polyester polyol, catalyst, water, flame retardant and physical blowing agent; its viscosity is 400-600mPa.s, hydroxyl value is 200-300mgKOH/g, water The content is 1.5-2.5%, and the physical foaming agent content is 10-20%;
PIR board combination polyether contains the following components in mass fraction: 4 parts of polyether polyol NJ6207, 6 parts of polyester polyol PS-2412, 4.0 parts of catalyst, 2.0 parts of H2O, 15 parts of flame retardant TCPP, physical blowing agent 15 parts of n-pentane.
According to the above formula, the ingredients are added into the stainless steel mixing kettle, stirred at 500 rpm at room temperature for 1 hour, and the material is discharged to obtain the combined polyether.

In a 500ml four-necked flask with a fixed device, constant temperature function, mechanical stirring, thermocouple and nitrogen gas, 350g of ethylene glycol butyl ether is added to start polyoxyethylene with an average molecular weight of 2200 and an average molecular weight of 2200. Ether, polyoxyethylene ether contains 45% by mole of ethylene oxide group and 55% by mole of propylene oxide, and then 150g of low hydrogen polysiloxane (with hydrogen content of 0.15%) is added In the four-neck flask, start stirring, use a heating mantle to heat to 80°C, stir for 5 minutes, add chloroplatinic acid ethanol solution, after adding chloroplatinic acid ethanol solution, make the concentration of chloroplatinic acid in the entire reaction system 15ppm. After reacting for 3 hours, a clear and transparent light yellow liquid is obtained, which is a silicone copolymer surfactant. The hydroxyl value is 0 according to the test of GB/T 7383-2007.