CN1199757A - 彩色感光材料用聚合品红成色剂 - Google Patents

彩色感光材料用聚合品红成色剂 Download PDF

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CN1199757A
CN1199757A CN 97112086 CN97112086A CN1199757A CN 1199757 A CN1199757 A CN 1199757A CN 97112086 CN97112086 CN 97112086 CN 97112086 A CN97112086 A CN 97112086A CN 1199757 A CN1199757 A CN 1199757A
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CN1091784C (zh
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黄振国
郑定洪
侯建国
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CHINA LEKAI FILM Co
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Abstract

本发明涉及卤化银彩色照相材料,特别涉及卤化银照相材料用品红成色剂。本发明为新型聚合品红成色剂,其结构通式为上式,该品红成色剂采用两个发色基团,既可以调整品红染料的色光,又可以调节解像力和均方根颗粒度。

Description

彩色感光材料用聚合品红成色剂
本发明涉及卤化银彩色照相材料，更确切说，涉及卤化银照相材料用品红成色剂。
众所周知，聚合成色剂可减薄涂层，提高涂层的机械强度。美国专利4128427中提到一种四元聚品成色剂，其中两元是共聚不饱和化合物，一元是无色成色剂基团，另一元是品红发色基团。由于只有一个品红发色基团，无法调整品红染料的色光，也无法调节解像力和均方根颗粒度。
本发明目的在于通过一种新型聚合品红成色剂，采用两个品红发色基团，既可以调整品红染料的色光，又可以调节解像力和均方根颗粒度。
本发明的聚合品红成色剂结构通式如下：
R1、R2为带有不同取代基的吡唑酮：
Figure A9711208600072
Figure A9711208600091
Figure A9711208600111
R3为：-CH3、-C4H9、-C2H4OCH3、-C2H4OC2H5R4为：
R5、R6为：H、-CH3
聚合性成色剂的制备：首先合成带有吡唑酮的发色单体，其分子结构如下：
Figure A9711208600122
Figure A9711208600131
Figure A9711208600151
聚合性品红成色剂的具体结构如下：成色剂  R1   R2  R3      R4     R5   R6   x     y     z     p1       I     II   -C4H9
Figure A9711208600162
-CH3-CH31     1     62       I     II   -C4H9    同上    同上  同上  2     3     153       I     II   -C4H9    同上    同上  同上  2     3     204       I     II   -C4H9    同上    同上  同上  0.35  0.65  35       I     II   -C4H9    同上    同上  同上  1     1     86       I     II   -C4H9    同上    同上  同上  0.45  0.55  3.57       I     II   -CH3      同上    同上  同上  0.35  0.65  48       I     II   -C2H5    同上    同上  同上  0.45  0.55  4  9    III   VI    -C4H9同上      H       H      1    3      1210    同上  同上  同上    同上      H       H      1    3      12   211    XV    VI    同上    同上      H       H      1    3      12   212    VII   VI    同上    同上      H       H      1    3      12   213    VIII  VI    同上    同上      H       H      1    3      12   214    IX    VI    同上    同上      H       H      1    3      12   215    X     VI    同上    同上      H       H      1    3      12   216    X     VI    -       同上      H       H      1    3      12   2
               CH2CH2
               OCH317    X     VI    -       同上      H       H      1    3      12   2
               CH2CH2
               OCH3
成色剂的制备方法：
例1：成色剂1的合成
在500毫升三口烧瓶中加入单体I110克、单体II168克、无水乙醇200毫升，搅拌下升温至75℃，再加入580毫升丙烯酸丁酯与4.8克偶氮异丁氰，继续回流搅拌3小时，然后加入35.8克氢氧化钠(事先溶于500毫升蒸馏水中)，溶液呈透明状，冷却至40℃，再加入2000毫升蒸馏水，搅拌均匀，倒入由18升冰水与100毫升冰乙酸组成的溶液中，析出沉淀，过滤，水洗，真空下干燥。
GPC分析结果：数均分子量＝14236；重均分子量＝89704；Z均分子量＝690845；粘均分子量＝52616；峰位分子量＝37154；10％分子量＝154651；90％分子量＝9869；分布系数＝5.6；特性粘度＝0.35954
例2  成色剂13的合成：
A液  在1000毫升三口烧瓶中加入400毫升蒸馏水、3.2克乳化剂，搅拌下升温至95～100℃。
B液  在另一只250毫升三口烧瓶中加入单体IV6.65克，单体V17.82克，丙烯酸丁酯30.8克，乙醇120毫升，搅拌、加热至75～80℃，得一透明溶液。
将A液慢慢加入B溶液，一小时内添加完毕，再加入2％的过硫酸钾溶液100毫升，搅拌回流2小时，蒸出剩余丙烯酸丁酯和水组成的共沸混合物，直至无丙烯酸丁酯味为止，冷却至室温，用4％的氢氧化钠溶液调PH至5.5，过滤，乳液装入容器，乳液含固量在10％～13％之间，重量为450～500克。
对此高分子化合物进行GPC分析，得结果如下：数均分子量＝20536；重均分子量＝100534；Z均分子量＝908865；粘均分子量＝72216；峰位分子量＝33654；10％分子量＝194441；90％分子量＝9665；分布系数＝4.9；特性粘度=0.43084应用实例1：A液：在5升三口烧瓶中加入1千克成色剂1，无水乙醇3000毫升，水浴升温至75℃，搅拌下加入350毫升8.2％的氢氧化钾，在70～75℃下搅拌备用。B液：在20升搪瓷桶内加入8立升水，20克十二烷基硫酸钠，升温至70～75℃，搅拌至完全溶解。
将B液搅拌下惭惭加入A液，并用少量无水乙醇冲洗A容器后一起加入B液中，补加蒸馏水至12.5升，冷却至30℃，用滤纸过滤，得8％浓度乳液。
将上述分散成色剂用于油彩正品层：涂布银量1.51克/米2；成色剂用量：1.6克/米2，将涂布好的胶片用CD-2配方加工，所得性能数据见下表：成色剂    照相性能               光谱性能
      D°             γ              S      λmax   对黄     对红对比1     0.18    3.0     5       542     29％     11.7％对比2     0.12    2.15    2.8     538     33％     10％15        0.14    2.51    2.20    540     30％     14％16        0.12    3.3     2.4     540     29％     9％3    0.12    3.3    3.0    535    32.2％  10％6    0.12    3.0    3.0    535    33％    10％4    0.15    3.5    3.0    540    32.2％  10.3％5    0.11    3.6    3.0    540    36％    11.4％
由以上数据可见，本发明成色剂可以调节色光与性能。
对比成色剂1：
Figure A9711208600191
对比成色剂2：
对比成色剂3：
应用例2：
将对比成色剂1、2、3和发明成色剂13、14加入彩色胶卷品层乳剂，制成样片，经C-41彩色显影液加工，其结果见下表：成色剂       D。       γ          S      Dmax  λmax Rp    RMS对比成色剂2  0.20    0.77    125    1.16   550    81    10.8对比成色剂1  0.14    1.05    127    1.15   550    90    9.5对比成色剂3  0.18    1.0     130    1.33   550    95    8.5成色剂13     0.20    1.1     130    1.25   550    95    7.0成色剂14     0.20    1.1     131    1.27   550    100   6.5
从以上数据可以看出，与对比成色剂相比，本发明成色剂具有较好的照相性能。

Claims (7)

1、一种聚合品红成色剂，其通式如下：
Figure A9711208600021
2、根据权利要求1所述的成色剂，其特征在于：R3为-CH3、-C4H9、-C2H4OCH3、-C2H4OC2H5。
3、根据权利要求2所述的成色剂，其特征在于：R4为
4、根据权利要求3所述的成色剂，其特征在于：R5、R6为H、-CH3。
5、根据权利要求4所述的成色剂，其特征在于：R1、R2为：
Figure A9711208600031
Figure A9711208600051
6、根据权利要求5所述的成色剂，其特征在于：X∶Y∶Z∶P＝1～2∶3∶3～12∶0～2；
7、根据权利要求5所述的成色剂，其特征在于：X∶Y∶Z∶P＝1∶3∶12∶2。
CN97112086A 1997-05-21 1997-05-21 彩色感光材料用聚合品红成色剂 Expired - Fee Related CN1091784C (zh)

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