Cellulose acylate film, saturated norbornene resin film, and process for producing these
A technology of cellulose acylate, manufacturing method, applied in the direction of flat products, applications, coatings, etc., can solve problems such as film streak failure, and achieve the effect of suppressing streak failure
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Synthetic example 1
[0188] Synthesis example 1 (synthesis of cellulose acetate propionate)
[0189] 150 g of cellulose (hardwood pulp) and 75 g of acetic acid were taken in a 5 L separable flask with a reflux device as a reaction vessel, and vigorously stirred for 2 hours while heating in an oil bath adjusted to 60°C. The cellulose subjected to such a pretreatment is swollen and pulverized into flakes. The reaction vessel was placed in an ice-water bath at 2°C for 30 minutes to cool.
[0190] Separately, a mixture of 1545 g of propionic anhydride and 10.5 g of sulfuric acid was prepared as an acylating agent, and after cooling to -30° C., it was added at once to the reaction container containing the pretreated cellulose. After 30 minutes had passed, the temperature of the external device was gradually raised, and after 2 hours had passed after the addition of the acylating agent, the internal temperature was adjusted to 25°C. Cool the reaction container with an ice-water bath at 5°C, adjust the...
Synthetic example 2
[0192] Synthesis example 2 (synthesis of cellulose acetate butyrate)
[0193] 100 g of cellulose (hardwood pulp) and 135 g of acetic acid were taken in a 5 L separable flask with a reflux device as a reaction vessel, and heated in an oil bath adjusted to 60° C. for 1 hour. It was then heated with an oil bath adjusted to 60° C. while stirring vigorously for 1 hour. The cellulose subjected to such a pretreatment is swollen and pulverized into flakes. The reaction vessel was placed in an ice-water bath at 5°C for 1 hour to sufficiently cool the cellulose.
[0194] Separately, a mixture of 1080 g of butyric anhydride and 10.0 g of sulfuric acid was prepared as an acylating agent, and after cooling to -20° C., it was added all at once to the reaction vessel containing the pretreated cellulose. After 30 minutes, the peripheral temperature was gradually raised to 20° C. and reacted for 5 hours. The reaction container was cooled with a 5° C. ice-water bath, and 2,400 g of 12.5% b...
Embodiment
[0499] 1. Film production of cellulose acylate film or saturated norbornene-based resin film
[0500] (1) Preparation of cellulose acylate
[0501] prepare Figure 5 The cellulose acylate described in Table 1. Sulfuric acid (7.8 parts by weight per 100 parts by weight of cellulose) was added as a catalyst, carboxylic acid as a raw material of an acyl substituent was added, and an acylation reaction was performed at 40°C. At this time, the type and degree of substitution of the acyl group are adjusted by adjusting the type and amount of the carboxylic acid. Moreover, aging at 40 degreeC after acylation was performed, and the sample was prepared (the degree of polymerization was lowered by prolonging aging time). The degree of polymerization of the cellulose acylate thus obtained was determined by the following method.
[0502] (Polymerization Determination Method)
[0503] Accurately weigh about 0.2 g of completely dry cellulose acylate, and dissolve it in 100 ml of a mixe...
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