Synthetic formulation of ice-sensitive silicone oil
Production of smooth amino silicone oil
Smooth crude oil generally uses linear body as raw material. First, pump the linear body into the kettle, turn on the stirring, add piperazine-based coupling agent, the coupling agent generally does not need to be hydrolyzed, raise the temperature to 70-80℃, add the catalyst, the catalyst is tetramethylammonium hydroxide, potassium hydroxide, lithium hydroxide, according to the different viscosity, choose different catalyst, the amount of addition is about one ten thousandth. Continue to heat up to 110-120℃, keep warm for 1 hour and then evacuate, the vacuum time depends on the viscosity of the oil, generally 10-60 minutes. After the viscosity of the oil reaches the requirement, cool down to below 80℃ and discharge the material and set aside.
Use linear system to make several kinds of silicone oil as follows.
0.03-0.05N, viscosity at 500-1 million CP.
0.1-0.15N with viscosity in the range of 50-100,000 CP.
0.4-0.45N, viscosity in the range of 20-50,000 CP.
Usually means 0.1N per 100kg of linear body with 1kg of coupling agent.
Production of loose and soft amino silicone oil
Loose and soft crude oil is generally made from D4 or DMC. The production methods for making amino silicone oil with D4 or DMC are.
1、Hydrolysis of coupling agent
First, put 100kg of piperazine-based coupling agent into the reactor, add 20kg of deionized water, turn on the stirring, open the evacuation valve of the receiver, raise the temperature to 80℃, turn on the cooling water of the condenser, continue to raise the temperature to 130℃, close the evacuation valve, turn on the vacuum, raise the temperature of the material to 150℃ in the process of evacuation, cool to below 80℃, discharging and weighing.
Yield = weight after dehydration / input quantity (generally at 0.8)
2、Synthesis of amino silicone oil
Pump 200kg of DMC into the reaction kettle, add (20g potassium hydroxide + 180g water) when the temperature rises to 80℃, raise the temperature to 145~150℃, keep warm for 1 hour, measure the viscosity at 2000~5000CP. no need to lower the temperature, add thoroughly hydrolyzed piperazinyl coupling agent, such as do 0.6N (12kg * yield), then add potassium hydroxide (20g potassium hydroxide + 20g of water ), at 145 + 150 ℃, holding 1 hour, viscosity above 5000. That can be cooled to below 80 ℃, the discharge if the viscosity requirements of high can be before cooling, pumping vacuum reaction, pumping to the required viscosity. If the viscosity requirement is small, you can add MM or MDM capping agent before cooling, and then add catalyst, the viscosity will be reduced.
The oil produced with D4 or DMC has: 0.6N viscosity of 5000 to 1000CP, 0.9N viscosity of 1000CP.
Production of ice-sensitive silicone oil
A、Smooth type
0.03-0.05N crude oil.
Viscosity 500-1,000,000CP 40kg
0.1-0.15N crude oil.
Viscosity 5-10 million CP 40kg
0.4-0.45N crude oil.
Viscosity 20-50,000 CP 20kg
Emulsifier T05 10kg
T07 10kg
Glacial acetic acid 0.8kg
Glycerol 100-200kg
Water 150kg
Mix the various crude oils in the formula, add the emulsifier, stir for 5-10 minutes, add acid water, add glycerin, stir and disperse at high speed for 30-60 minutes, then add the remaining water slowly until all the water is added, adjust the pH value to 5-6, filter and pack.
B. Loose and soft type
Loose soft type add high ammonia value silicone oil, also can’t add too much, otherwise the cotton feeling is too strong, reference formula as follows.
0.03-0.05N crude oil.
Viscosity 50-1 million CP 40kg
0.1-0.15N crude oil.
Viscosity 5-10 million CP 30kg
0.4-0.45N crude oil.
Viscosity 20-50,000 CP 20kg
Emulsifier T05 10kg
T07 15kg
Glacial acetic acid 1kg
Glycerol 100-200kg
Water 150kg
Emulsification process.
First add 10-20kg of water to the high-speed stirring kettle, add T05, T07, stir evenly, add various amino silicone oils to the kettle, stir at high speed for 20 minutes, add glacial acetic acid, then add glycerin in several times, stir at high speed for 40-60 minutes, add water slowly until all water is added, adjust pH 6-7, stand still, filter and pack.
The applicable range of different ammonia value of amino silicone oil for reference
0.02-0.1N Suitable for making deepening agent
0.1-0.2N Suitable for smoothing agent
0.2-0.3N For polyester nylon softener
0.3-0.4N Softener for cotton
0.4-0.6N Cotton, wool loosening and softening finishing agent
0.6-0.9N acrylic, cotton loosening finishing
Triamine piperazine 0.3-0.5N cotton, human cotton, acrylic loosening finishing
Piperazine 0.3-0.5N cotton, human cotton soft finishing
The influence of coupling agent on the quality of synthetic amino silicone oil
1、602 coupling agent
602 is the most commonly used silane coupling agent, the advantages of good feel, versatility for all types of fabrics, the disadvantages of yellowing, the application of a large constraint.
2、KH550
Used in the production of amino silicone oil coupling agent can not add water, usually used in large quantities in emulsion polymerization, the advantages of small yellowing with high resilience since the cross-linking, used for smooth rebound stiff finishing.
3、Piperazine-based coupling agent
Due to the piperazine-based coupling agent in the amino group is not exposed, with small yellowing, semi-hydrophilic properties, a large number of cotton fabrics and acrylic, cotton finishing.
4、Triamcinolone piperazine
Tri-ammonia piperazine than piperazine-based coupling agent more than one group, so more fluffy performance, a large number of cotton, cotton fluffy finishing.
5、560 coupling agent
560 coupling agent is with epoxy group of self-crosslinking coupling agent, fabric finishing without yellowing, most of the emulsion polymerization used in the finishing of the fabric with dry, slippery, elastic.
Choice of emulsifier 1, TO isomeric tridecanol series
As TO series has a strong emulsification penetration performance, a large number of emulsifiers used as smoothing agent wool mercerizing softener, etc., the disadvantage of emulsification with TO series of amino silicone oil cation of strong polarity, easy to bo color, sticky rollers, in the long car finishing agent used sparingly.
2、XL isomeric decanol series
Emulsification permeability is moderate, used in large quantities in cotton and chemical fiber finishing agent.
3、Aliphatic alcohol AEO series
Emulsification penetration is poor, especially for cotton fabric softener can reduce the phenomenon of sticky rollers.
4, the choice of emulsifier in the smooth softener is crucial, generally in a smooth softener in the use of two series of more ideal results.
Ice-sensitive silicone oil ice additive
Ice feeling silicone oil ice feeling from where, is the silicone oil emulsion added non-volatile, boiling point of 200 ℃ above the solvent, such as and ethylene glycol monobutyl ether, boiling point at 230 ℃; white oil, alias paraffin oil, white oil, mineral oil, boiling point ≥ 250 ℃; glycerin is generally used industrial glycerin, industrial glycerin to propylene as raw material synthesis method, the resulting glycerin called synthetic glycerin, boiling point of 290 ℃. Add one or more non-volatile solvents in the silicone oil emulsion, used in the finishing of the fabric, the surface of the fabric adsorbed silicone oil emulsion after high temperature setting, and the fiber surface hydroxyl reaction, combined with the film, the adsorbed solvent still remains on the surface of the fiber, thus reflecting the cold feeling. When the fiber is washed, this feeling is gone, so it is not washable.
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