1. Classification: Conventional hydrogen containing silicone oil includes end hydrogen containing silicone oil and side hydrogen containing silicone oil (dangling hydrogen based silicone oil).
2. Synthesis:
The synthesis method of hydrogen terminated silicone oil: Tetramethyldihydrodisiloxane is used as the hydrogen terminated end capping agent, and DMC, D4 and other cyclic compounds are used as chain extenders. Under the catalysis of acidic catalysts, ring opening polymerization is carried out to generate hydrogen terminated silicone oil of various molecular weights.
Synthesis method of side hydrogen containing silicone oil:
① Ring opening polymerization is carried out by the D4H ring, D4, DMC, etc. under the action of a broken catalyst.
② Ring opening polymerization is carried out using high hydrogen containing silicone oil, D4, DMC, etc. under the action of a broken catalyst.
③ Co hydrolysis and condensation of methyldichlorosilane and trimethylchlorosilane, followed by equilibrium polymerization under the action of acidic catalyst.
3. Application:
① Hydrogen containing silicone oil can be used as a raw material for linear modified silicone oil, and can be used to prepare polyether modified silicone oil, ternary block copolymer silicone oil, and other products. It is applied as a textile softener, leather finishing agent, etc.
② Hydrogen containing silicone oil can generally be used as a curing agent for silicone resins and rubber. Common products include silicone adhesives, silicone release agents, silicone rubber products, etc.
4. Hydrogen content detection:
① Chemical method 1: By utilizing the activity of silicon hydrogen bonds, a dehydrogenation reaction is carried out with a base to generate hydrogen gas, which is used to calculate its hydrogen content. The specific method is as follows:; First, weigh 0.5-1.0g of hydrogen containing silicone oil standard and place it in a 250mL single mouthed reaction bottle. Then, measure 60-80mL of potassium hydroxide solution with a mass fraction of 30-40% and add it to a 100mL constant pressure dropping funnel. Collect hydrogen gas using alkaline hydrolysis method and seal it carefully; Turn on the magnetic stirrer and add the potassium hydroxide solution from the constant pressure dropping funnel to the single necked flask at a constant speed. Collect the produced hydrogen gas through the drainage method; When the liquid is clear and the gas volume reading no longer changes (approximately 5 minutes), record the amount of hydrogen gas produced and convert it into the volume of hydrogen gas released per gram of sample. Measure three times and take the average value VA; Measure the hydrogen gas accumulation VB generated by the test sample through the same steps; Under the same measurement environment, the hydrogen content of A and B can be obtained; The hydrogen content of the sample to be tested can be calculated; Among them, A is a standard with known hydrogen content, and B is the sample to be tested.
Chemical method 2 involves the consumption of known bromine through the substitution reaction of silicon hydrogen bonds with bromoacetic acid, followed by the reaction of residual bromine with potassium iodide to generate iodine. Finally, the generated iodine is chemically titrated with sodium thiosulfate to obtain the final measurement value. The sample weighing should be accurate to four decimal places.
② Infrared detection method,
The absorption peak of silicon hydrogen bonds is in the range of 2000-2100. By configuring a standard concentration solution for infrared detection, a standard spectrum of concentration and absorption peak area is drawn, and then the concentration of silicon hydrogen bonds is detected for unknown samples.
③ Nuclear magnetic resonance hydrogen spectroscopy,
Using the standard reagent benzene as the internal standard reference, the active hydrogen in Si-H was quantitatively calculated using the classical internal standard method.
Based on the characteristics of silicon hydrogen bond nuclear magnetic resonance hydrogen spectrum, identify the silicon hydrogen peak. Then, according to the integrated area of the hydrogen proton peak of benzene and the hydrogen proton peak in Si-H, as well as the mass fraction of hydrogen in benzene, the mass fraction of active hydrogen in hydrogen containing silicone oil can be calculated by the following formula:
WH%=AsAr × mrms × 71743%, where wH is the mass fraction of active hydrogen in hydrogen containing silicone oil,%;
As and Ar are the integral values of hydrogen in the sample and internal standard, respectively; MS and MR represent the mass of the sample and internal standard, respectively, in grams;
71743% is the mass fraction of hydrogen in the internal standard benzene,%.

Methyl Low Hydrogen silicone oil MY 203