A kind of preparation method of homogeneous spinning solution
A technology of spinning solution and keratin protein, which is applied in the preparation of spinning solution, artificial filament in cellulose solution, single-component protein rayon, etc., can solve the complex, large structure of vacuum dehydration and dissolution equipment, which is not conducive to industrialization Production and other issues, to avoid excessive degradation, to avoid the effect of entrained air bubbles
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[0029] Specifically, the invention provides a method for preparing a homogeneous spinning solution of a mixture of low-temperature molten salt and cellulose, keratin or cellulose keratin, comprising:
[0030] a) Premix low-temperature molten salt at a temperature of t1 with cellulose, keratin or cellulose-keratin mixture to obtain a fluffy premix A with a ratio of bulk density to compacted density of 0.29 to 0.32, and t1 is 5~50℃;
[0031] b) Fully mix the premix A with the low-temperature molten salt at a temperature of t2 until a homogeneous and transparent solution is obtained, wherein t1
[0032] The low-temperature molten salt suitable for the present invention is selected from 1-ethyl-3-methylimidazole diethyl phosphate ([EMIM]DEP), 1-methyl-3-methylimidazole phosphate ([MMIM]DMP), 1-Ethyl-3-methylimidazole acetate, 1-propyl-3-methylimidazole acetate, 1-butyl-3-methylimidazole acetate, 1-allyl-3- Methylimidazole acetate, 1-methylallyl-3-methylimidazole acetat...
Embodiment 1
[0048] 1) First shape 20g to about 1cm 2 The cellulose pulp was added to the mixing tank A, and vacuumed to -0.1MPa. Then 80 g of 1-allyl-3-methylimidazolium chloride salt ([AMIM]Cl) with a water content of about 1200 ppm was added to mixing tank A at a temperature of about 40°C. Stir for 20 minutes at a stirring speed of approximately 80 rpm to obtain a bulk density of approximately 0.286 g / cm 3 , The compacted density is about 0.923g / cm 3 The premix has a looseness of about 0.3099.
[0049] 2) Under the condition of keeping the vacuum degree of the system at about -0.1MPa, add 135g of [AMIM]Cl at a temperature of about 121°C into the mixing tank A to fully mix it with the premix to obtain a viscosity of about 968Pa • A homogeneous transparent cellulose solution of s.
Embodiment 2
[0051] 1) First, 18g of cellulose powder (DP=1000) and 2g of keratin protein pulverized into fine powder (the bulk density of the mixed powder of cellulose and keratin protein is about 0.33g / cm 3 ) into the mixing tank A, and vacuum to -0.09MPa. Then add 70g of 1-ethyl-3-methylimidazolium diethyl phosphate ([EMIM]DEP) with a water content of about 6000ppm into mixing tank A at a temperature of about 38°C at a stirring speed of about 60 rpm Stir for 20 minutes to obtain a bulk density of about 0.283g / cm 3 , The compacted density is about 0.962g / cm 3 The premix has a looseness of about 0.2942.
[0052] 2) Under the condition of keeping the vacuum degree of the system at about -0.09MPa, add 120g of [EMIM]DEP at a temperature of about 121°C into the mixing tank A to fully mix it with the premix to obtain a viscosity of about 4180Pa Homogeneous transparent solution of s.
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