The production method for making amino silicone oil with D4 or DMC is as follows.
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, in the process of evacuation, raise the temperature of the material to 150℃, cool to below 80℃, discharge and weigh.
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 1000 CP, 0.9N viscosity of 1000 CP.
Reference of the applicable range of different ammonia values of amino silicone oil
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 advantage is good feel, versatility for all kinds of fabrics, the disadvantage is that the yellowing is large, the application is subject to great constraints.
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 advantage is that the yellowing is small, with a self-crosslinking high resilience, used for smooth rebound stiff finishing.
3、Piperazine-based coupling agent
Because 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 acrylics, 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, no yellowing of fabric finishing, most of the emulsion polymerization used in the finishing of the fabric with dry, smooth, elastic.
Choice of emulsifier
1, TO isomeric tridecanol series
As TO series has a strong emulsification penetration performance, a large number of emulsifier used as a smoothing agent, wool mercerizing softener, etc., the disadvantage is that with TO series emulsification 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 to use two series, the effect is more desirable.
The production of mercerized silicone oil
The recipe is as follows.
The formula of various amino silicone oil and hydroxy silicone oil into the emulsifying kettle with high-speed dispersion, scraping wall device, high-speed stirring for 2 hours, the temperature of the material will rapidly warm up, the temperature will reach about 90 ℃. At this time, the amino silicone oil and hydroxy silicone oil will have a reaction and redistribute the structure, the amino group in the amino silicone oil will be transferred to the hydroxy silicone oil, and the hydroxyl group of the hydroxy silicone oil has partly combined with the amino group. After the material is mixed and degraded, cool down to below 40℃, add the cross-linking agent, add the emulsifier, stir for 10-20 minutes, add 1kg of glacial acetic acid to 10kg of water, which is said to be acid water, slowly add it to the emulsifying kettle, stir for 10-20 minutes, then add glycerin in batches, and then add the water slowly. Static, filter and pack.
The role of hydroxy silicone oil and cross-linking agent
Hydroxy silicone oil determines the style and refractive index of fabric finishing, which is specifically expressed in the thickness, resilience, glossiness and smoothness of fabric.
The fabric’s fleshiness, thickness, mirror feeling, smoothness lies in the use of 5 million viscosity of hydroxy silicone oil; fabric’s smoothness, brightness, depth lies in the use of 1 million viscosity of hydroxy silicone oil; and low ammonia value of amino silicone oil; fabric’s dryness or non-sticky silicone oil, lies in the cross-linking agent, cross-linking agent commonly used are high hydrogen silicone oil, KH550, KH560, methyl triethoxy, etc. The soft, fluffy hand style of fabric lies in the medium ammonia value and high ammonia value of amino silicone oil.
Application of mercerized silicone oil
In principle, mercerized silicone oil is ice-sensitive silicone oil, mainly used for mercerized cotton, cotton pulling frame, imitation mercerization, woolen sweater, woolen thread, tweed, leather feel agent, denim finishing.
