Carbodylated cellulose esters
A technology of cellulose ester and oxidized cellulose, used in cellulose coatings, inks, coatings, etc.
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Embodiment 1
[0044]A 20 g sample of oxidized cellulose containing 77 meq / kg carboxyl groups was crushed into small pieces and soaked in demineralized water overnight. The impregnated cellulose was broken into smaller pieces by processing it in an EBERBACH(R) industrial blender. After draining the water using a vacuum glass filter, the water-activated oxidized cellulose was washed several times with acetic acid and then several times with butyric acid.
[0045] The esterification reagent was prepared by mixing 47 grams of butyric acid including a residual amount of water activated oxidized cellulose, 6.2 grams of acetic anhydride and 50.6 grams of butyric anhydride. 0.68 g of 8% sulfuric acid was added as catalyst. The esterification reagent and catalyst were added to water-activated oxidized cellulose and injected into a stirred round bottom flask. Place the flask in an ice bath that maintains the bath temperature near zero. After keeping the temperature of the water bath close to zero ...
Embodiment 2
[0052] Carboxylated cellulose ester was prepared using 20 g of the same oxidized cellulose used in Example 1. The procedure was similar to that described in Example 1, but the esterification reagent was prepared by mixing 80 grams of butyric acid including residual cellulose, 8.3 grams of acetic anhydride and 62.7 grams of butyric anhydride. The bath temperature of the reaction bath was maintained at zero degrees for two hours and then gradually increased to 35°C. The remaining steps of the method are the same as in Example 1. This cellulose ester is referred to as sample No. 2.
[0053] Cellulose acetate-butyrate was prepared using PLACETATE F(R) regular grade cellulose in the same manner as the above samples were prepared from oxidized cellulose. After neutralization the solution was filtered through a medium frit filter to remove excess fibers. This cellulose ester is referred to as sample No.3.
[0054] The analytical results of the two cellulose acetate-butyrates are ...
Embodiment 3
[0058] Carboxylated cellulose acetate-butyrate was prepared by using the same oxidized cellulose in Example 1. 150 grams of oxidized cellulose was reacted with an esterification reagent consisting of a total of 352.5 grams of butyric acid, 46.5 grams of acetic anhydride, and 379.5 grams of butyric anhydride. 6.18 g of 98% sulfuric acid were added as catalyst. The reaction was maintained at about zero degrees for five hours, and then the temperature was gradually increased to 40°C to complete the esterification. After completion of esterification, a mixture of 142.5 grams of acetic acid and 142.5 grams of water was added for hydrolysis. Hydrolysis was carried out at 60°C for 15 hours. The solution was filtered through a coarse frit filter and precipitated in 10% acetic acid solution. This cellulose ester is referred to as sample No.4. The analysis results of this carboxylated cellulose ester are shown in Table 4.
[0059] Sample №4
Carboxyl content (meq / k...
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