• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    An alkali-soluble cellulose derivative is produced by treating cellulose with liquid ammonia having urea dissolved therein, removing the ammonia, resulting in cellulose having urea distributed therethrough, and heating the thus obtained cellulose-urea to cause reaction between the urea and cellulose and form alkali-soluble cellulose carbamate. This cellulose carbamate can be precipitated from alkaline solution in the form of cellulose carbamate film or fibre.
    公开号:SU1306478A3
    申请号:SU823381944
    申请日:1982-01-26
    公开日:1987-04-23
    发明作者:И.Хуттунен Еоко；Турунен Олли；Мандел Пео；Еклунд Видар；Екман Курт
    申请人:Несте Ой (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to chemical technology, specifically to the preparation of ketchullose carbamate, which can be used to prepare solutions for forming hydrated cellulose articles.
    The purpose of the invention is to obtain an alkali-soluble carbamate cellulose.
    Example 1. Cellulose is treated with alkali to reduce the polymerisation rate (SP) to 300, neutralized with acetic acid and washed with water, dried and crushed in a hammer mill. 40 g of cellulose thus cleaned at -40 are impregnated with 500 ml of liquid ammonia containing 36 g of urea (molar ratio of urea and cellulose of 2.5). The cellulose is kept in this solution at a temperature below the boiling point of ammonia for 6 hours, after which the temperature is slowly raised to room temperature. After the ammonia is evaporated, the cellulose containing urea is kept under vacuum at 135 ° C for 3 hours. All this time, a stream of air ejected through the furnace passes through the furnace.
    The reaction product was washed with methanol, three times with water, and again with methanol. Air-dry product has
    Low thickening numbers indicate that the solutions are suitable for molding.
    Example 3. Two portions of cellulose (30 g each), treated analogously to example 1, having SP 430 and 350, are impregnated with PEN-40 with 500 ml of ammonia, in which urea is dissolved (7.8 and 6.2 g, respectively), the ratio of urea and cellulose is 0.7 and 0.5. After impregnation for 6 h, the temperature of cellulose samples 341 and contains 1.7% nitrogen. The product is dissolved at -5 ° C in an aqueous solution containing 10% NaOH and 2% ZnO. Ball viscosity
    is 50 s,
    the number of cellulose thickening in rast
    1485, thief content 5.5%.
    Example 2. Three portions of cellulose 30 g each process
    as in example 1, it is passed at 500 ml of ammonia, in which 11.1, respectively, is dissolved; 22.2 and 33.3 g of urea, with a molar ratio of urea and cellulose of 1.2 and 3. The impregnation time is 5.5, respectively; 6 and 6 o'clock
    The temperature of the cellulose samples is raised to room temperature after the impregnation and removal of ammonia stage. Then
    Cellulose samples are placed in a vacuum furnace and kept for 3 hours at 136-137 s.
    The obtained cellulose carbamate samples are washed after termination of the reaction with methanol, three times with water and again with methanol. The degree of polymerization and the nitrogen content of the products are determined. The cellulose urea is dissolved in a solution containing 10% NaOH and 2% zinc oxide to give viscosity ball 50 s.
    The results of the experiment are given in table.1.
    Table D
    the vines are raised to room temperature and the ammonia is evaporated.
    50 Heat treatment is carried out as in Example 1 in a vacuum oven with PE-IO C. The products are washed with methanol and water.
    The characteristics of the products and their solubility are determined analogously to example 2.
    The results of the experiment are given in table 2.
    55
    table 2
    Soko and can not be determined.
    The results of experiments indicate that when the content of nitrogen is low, the solutions contain a significant amount of insoluble particles.
    Examples 4-8. The cellulose derivative, split with alkali to SP 300, is neutralized with acetic acid and washed with water, dried and crushed in a hammer mill, 40 g of the thus treated cellulose is impregnated at -40 ° C with 450 ml of liquid ammonia, in which urea is dissolved. The cellulose is kept in this solution at the boiling point of ammonia below for 3 to 6 hours, after which the ammonia is evaporated at room temperature. Heat treatment is carried out in a vacuum oven at 140-150 ° C in those
    Example 10. 40 g of cellulose with an average SP 355 are ground in a hammer mill, impregnated in a liquid Shz (400 ml), in which the precursor
    4-6 hours. During this period, an air flow of 20 liters per minute is passed through the oven, supplied by a nozzle for irrigation with water.
    The reaction product is washed with methanol, three times with water and again with methanol. The SP of these air-dry products is determined using the standard S CAN-C15: 62 in copper ethylenediamine. The nitrogen content and the solubility, expressed as a thickening number, in a 10% solution at -5 s are then determined.
    15
    20
    Example 9. The experiment was carried out according to Example 4. The cellulose was hydrolyzed to SP 300 and neutralized with acetic acid, washed with water and dried. The thus obtained 440 g of cellulose is impregnated at -40 ° C with 500 ml of ammonia in which urea is dissolved (the ratio of urea and cellulose is 3). The cellulose is soaked with this solution for 3 hours, after which the ammonia is evaporated at room temperature. The pulp thus treated is heated in a vacuum oven at 132 ° C for 6.5 h.
    30 as in example 4.
    The data obtained are given in table.3t
    Table3
    but 40 g of urea is dissolved, the ratio of urea and cellulose is 2.7. Ammonia is evaporated at room temperature. After that, the mixture of urea and cellulose is heated for 16 hours at, washed three times in 1 liter and finally in 1 liter of methanol. After evaporation of methanol, the product yield is 40.3 g, SP 230, N content is 2.3%,
    , "" °. ball viscosity 97 s (conditional
    viscosity), carbamate content of cellulose is 8.5%,
    Example 11. 40 g of pulp with an average SP of 355 are crushed in a hammer mill, impregnated in liquid NHj (400 ml), in which 40 g of urea is pre-dissolved in a ratio of urea and cellulose of 2.7. Ammonia is evaporated at room temperature. the mixture of urea and cellulose is heated for 32 hours at 110 ° C, washed three times in 1 liter of H, 0
    and finally washed in 1 liter of the formula of the invention
    The method of producing cellulose carbamate by treating cellulose with urea followed by heat treatment, which is the case in order to obtain an alkali-soluble compound Composer L, Abramova Editor O, Golovach Tekhred I. Popovich Corrector L, Patay
    1470/58
    Circulation 438. Subscription
    VNIIPI USSR State Committee
    for inventions and discoveries 113035, Moscow, Zh-35, Raushsk nab ,, d, 4/5
    Production and printing company, Uzhgorod, Proektna st, 4
    tanola. After methanol was evaporated, the product yield was 40.5 g, SP 240, N content 2.2%, eo 1200, Viscosity per ball (nominal viscosity 100 s, 5 content of carbamate cellulose 8.5%,

    Example 12 40 g of pulp with an average DP of 300 are ground in a hammer mill, impregnated in liquid NHg (400 ml), in which 40 g of urea are pre-dissolved in a ratio of urea and cellulose of 2.7. Ammonia is evaporated at room temperature. After that, the mixture of urea and cellulose is heated for 2.5; 3.0; 3.5 and 4.0 hours at 150 ° C and the product is washed and dried as in Examples 10 and 1 1,
    The properties of the product are given in Table 4.
    Table 4
    40
    chi of the target product, urea treatment. CONDUCTED in a liquid ammonia environment with a molar ratio of urea and cellulose 0.5-3.0 3-6 h, followed by evaporation of ammonia, and heat treatment is carried out 2.5-232 h at 110-150 .
    权利要求:
    Claims (1)
    [1]
    Claim
    A method of producing cellulose carbamates by treatment of cellulose with urea, followed by heat treatment, characterized in that, to produce the alkali-soluble target product chi υ fault handling urine .provodyat in liquid ammonia at a molar ratio of urea and cellulose 0.5-3.0 3 -6 hours, followed by evaporation of ammonia, and heat treatment is carried out 2.5 45 32 hours at 110-150 ° C.
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    引用文献:
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    FI810226A|FI62318C|1981-01-27|1981-01-27|FORM OF CELLULOSE DERIVATIVES OF FRAMSTAELLNING AV ETT ALKALILOESLIGT|
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