Method for producing potassium carboxymethylcellulose by using ultrasonic
A technology of carboxymethyl cellulose and ultrasound, applied in the field of production of carboxymethyl cellulose potassium, can solve the problems of low viscosity, low utilization rate of etherification agent, difficult to dissolve, etc., and achieve simple equipment cleaning and operation, batch production The effect of stable quality and expanding the scope of use
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Embodiment 1
[0027] In the first step, 51 g of food-grade sodium carboxymethylcellulose (FH6 type, DS=0.62, 1% aqueous solution viscosity (Brookfield) 250 mPa, purity 98.8%) was degassed for 5 minutes at a vacuum of 0.05 MPa, and filled with nitrogen. Add 10% H 2 SO 4 Aqueous solution 816mL;
[0028] The second step is ultrasonic treatment for 1 minute, the ultrasonic treatment frequency is 15kHz, and the power density is 1.5kW / m 3 , ultrasonic treatment twice for 3 minutes at intervals, 0.5 minutes each time, kept at 10°C for 1 hour, separated, kept at 10°C for 10 hours, separated, the solid was washed with water at pH = 1, and separated at 0°C to obtain a water content of 55%. solid;
[0029] The third step The solid obtained in the second step is subjected to ultrasonic treatment for 0.1 minutes under nitrogen protection, the ultrasonic treatment frequency is 15kHz, and the power density is 0.1kW / m 3 , temperature 25°C, add K 2 CO 3 99 copies, (NH 4 ) 2 CO 3 1.5 parts of alkali...
Embodiment 2
[0034] The first step will produce 65g of food-grade sodium carboxymethylcellulose (FH6 type, DS=0.62, 2% aqueous solution viscosity (Brookfield) 50mPa, purity 85.0%) without purification, and a vacuum degree of 0.10MPa is degassed for 20 minutes, Fill with nitrogen, add H with a mass concentration of 40% 2 SO 4 260mL aqueous solution;
[0035] The second step is ultrasonic treatment for 15 minutes, the ultrasonic treatment frequency is 104kHz, and the power density is 0.1kW / m 3 ;Sonicate 3 times with 1 minute interval, 5 minutes each time, keep warm at 40°C for 1 hour, separate, wash the solid with pH=3, 30°C, 80% ethanol water, and separate to obtain a solid with a water content of 65%;
[0036] The third step The solid obtained in the second step is subjected to ultrasonic treatment for 15 minutes under nitrogen protection, the ultrasonic treatment frequency is 104kHz, and the power density is 0.1kW / m 3 , temperature 35°C, add K 2 CO 3 99.5 parts, (NH 4 ) 2 CO 3 8.1...
Embodiment 3
[0041]In the first step, 40 g of food-grade sodium carboxymethylcellulose (FH9 type, DS=1.0, 1% aqueous solution viscosity (Brookfield) 400 mPa, purity 98.8%) was degassed for 10 minutes at a vacuum of 0.05 MPa, and filled with argon , adding 15% mass concentration of H 2 SO 4 300mL aqueous solution;
[0042] The second step is ultrasonic treatment for 10 minutes, the ultrasonic treatment frequency is 25kHz, and the power density is 0.5kW / m 3 ;Sonicate 5 times for 1.5 minutes intermittently, 2 minutes each time, keep warm at 10°C for 0.5 hours, separate, wash the solid with pH=1, 10°C, 80% methanol water, and separate to obtain a solid with a water content of 60%;
[0043] The third step The solid obtained in the second step is subjected to ultrasonic treatment for 10 minutes under the protection of argon, the ultrasonic treatment frequency is 252kHz, and the power density is 0.25kW / m 3 , temperature 30°C, add, K 2 CO 3 99.5 parts, (NH 4 ) 2 CO 3 1 part of alkali mixtu...
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