CN112281257A - 一种负载纳米氯化银的海洋纤维的制备方法 - Google Patents
一种负载纳米氯化银的海洋纤维的制备方法 Download PDFInfo
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Abstract
本发明公开了一种负载纳米氯化银的海洋纤维的制备方法,以海洋资源海藻酸钠为原料,通过原位法工艺制备海藻酸钙/纳米氯化银溶胶纺丝液,并采用平均分子量≥12万的聚乙烯吡咯烷酮K90辅助控制氯化银晶核生长,再用湿法纺丝设备喷丝于锌、钙非氯化物凝固浴中获得纤维,确保纤维制造过程中氯化银呈纳米级尺寸,从而获得纳米氯化银高阻燃强抗菌海洋纤维;该纤维极限氧指数大于60%,抑菌率大于99%,特别适合于对防火和防疫要求很高的装饰材料和家纺用品的规模化生产。
Description
技术领域
本发明属于海洋生物质阻燃纤维技术领域,具体涉及一种负载纳米氯化银的海洋纤维的制备方法。
背景技术
目前,在日常生活中,火灾引发的财产生命安全已备受重视,为了降低火灾危害,社会各界极度关心阻燃材料及其技术的发展,海洋生物质阻燃纤维备受关注;海洋生物质阻燃纤维主要包括类纤维素结构的海洋生物质基阻燃剂、具有金属离子的海藻纤维、卡拉胶纤维、甲壳素纤维、壳聚糖纤维,虽然海洋生物质阻燃纤维可有效避免或减轻火灾起数和损失,比如海藻酸钙,其是一种本体阻燃材料且属于环境友好材料,但它也是一种多糖材料,阻燃性能有限,抗菌性能弱,不能满足对阻燃和抗菌功能都很高的纺织品及其装饰材料的要求。
同时除了火灾危险外,传染性疾病对人类的威胁也是巨大的,比如肆虐全球的新冠冠状病毒就造成了全球数百万人感染,几十万人死亡,且严重阻碍了经济发展,所以开发兼具阻燃和抗菌性能的海洋生物质纤维具有重要意义。在纤维中加入具有抗菌性的金属离子或者天然抗菌剂得到抗菌海藻纤维是时下流行的方式之一。
在海藻酸纤维中载银的方法有多种,主要分为喷涂浸渍法、离子交换法、共混纺丝法。其中,喷涂浸渍法是直接将纳米银浆喷涂在纤维上或者将纤维浸渍在纳米银浆中,再经过干燥等工序得到载银海藻酸钙纤维,虽然简便快捷,但是存在易板结、处理均匀性差的问题;离子交换法是利用海藻酸钙纤维浸渍在硝酸银溶液中,纤维中的钙离子或氢离子与溶液中的银离子之间的离子交换作用在纤维中载银,由于海藻酸中的羧基组既要与钙离子交联,又要封闭银离子,这直接使得纤维的力学性能和稳定性下降。共混纺丝法是在原纺丝液中混合银盐或纳米银,经过湿法纺丝或静电纺丝得到载银海藻酸钙纤维,但由于加入PVA、戊二醛或魔芋葡甘聚糖等物质,改变了纯海藻酸盐纤维在生理盐水中完全溶解的性能,甚至会发生粘连,且银浆容易出现团聚现象而导致喷丝孔堵塞,不适合于纺丝工艺。加之,纳米级氯化银制备的困难新,这使得要简便地制备一种高阻燃、强抗菌的纳米氯化银/海洋生物质复合纤维,在工艺方法备受挑战。
发明内容
本发明就是为了克服上述现有技术存在的缺陷而提出的解决方案。其技术解决方案是:
一种负载纳米氯化银的海洋纤维的制备方法,包括以下步骤:
(1)配制溶液A:先将去离子水加热至30-50℃,在超声波作用下,再依次将聚乙烯吡咯烷酮K90、氯化物和海藻酸钠溶于其中,维持反应30-60min后即得;
(2)配制溶液B:称取与氯化物等摩尔的硝酸银,在常温下将硝酸银溶解于去离子水中,然后在搅拌下将氨水滴加至溶液中,再维持搅拌反应3-5min,即得;
(3)制备结晶物C:在35-50℃水浴加热、搅拌条件下将溶液B滴加到溶液A中,然后,见到反应液变成乳白色时终止搅拌,并40-50℃恒温养护10-20min,即得;
(4)按照结晶物C与可溶性非卤化物盐溶液为1:5-10的质量比,将结晶物C在湿法纺丝设备中喷丝成形后于可溶性非卤化物盐溶液中交联反应10-15min,制得纤维后,用硼盐溶液喷洗1-3次,再用去离子水浸洗3-5次,再蒸汽干燥、热拉伸,冷却至常温,即得负载纳米氯化银的海洋纤维。
所述氯化物为氯化钠、氯化钾、氯化铵中任意一种或多种组合;进一步优选氯化钠。
所述溶液A中氯化物、聚乙烯吡咯烷酮、海藻酸钠、去离子水的质量比为1:(0.1-0.3):(15-25):(400-500)。
所述聚乙烯吡咯烷酮,其平均分子量≥12万。
所述可溶性非卤化物盐为硝酸钙、醋酸钙、乳酸钙、硝酸锌、醋酸锌、乳酸锌中任意一种或多种组合;优选为乳酸钙或乳酸锌。
所述溶液B中硝酸银、氨水、去离子水的质量比为1:(5-6):(5-7)。
所述氨水,其体积浓度为25%。
所述水浴加热,其温度为35-50℃。
所述恒温养护,其温度为40-50℃。
所述结晶物C,其粒径为5-50nm。
所述可溶性非卤化物盐溶液,其质量浓度为1-3%。
所述交联反应中结晶物C与可溶性非卤化物盐溶液的质量比是1:5-10。
所述硼盐溶液,其质量浓度为0.1-0.3%。
所述硼盐由硼酸与硼砂按质量比4:1组成。
所述负载纳米氯化银的海洋纤维,其极限氧指数大于60%,抗菌率大于99%。
上述技术方案直接带来的技术效果是,以海洋资源海藻酸钠为原料,通过粒径可控技术制备纳米氯化银溶胶,用湿法纺丝设备喷丝于二价金属离子的凝固浴中发生离子交换反应,继而通过硼元素表面修饰,制备了负载极限氧指数大于60%,抗菌率大于99%的纳米氯化银的海洋纤维,该纤维可满足敬老院、幼儿园、娱乐场合、军事装备、汽车、动车、客轮等场合的装饰材料等对高阻燃强抗菌性能的功能需求。
有益效果:
1、原工艺是海藻酸钠和银氨离子溶胶进入氯化钙凝固浴中直接一步生成氯化银和海藻酸钙复合纤维。本专利申请是先通过预混氯化银生成体氯离子于溶胶体中,改氯化银和海藻酸钙一步生成工艺为先后生成氯化银和海藻酸钙的两步工艺,克服了原工艺不能调控氯化银粒径的弊端。
2、在纺丝溶胶中预混了平均分子量≥12万的聚乙烯吡咯烷酮模型剂,实验证明起到了氯化银晶粒调控作用,确保了氯化银微粒在纳米尺寸,更有利于湿法纺丝不会堵塞喷丝孔。
3、氯化银的原位生成-复合过程,克服了在海藻酸盐中直接添加氯化银容易团聚不易喷丝的缺陷,使得纳米氯化银在海藻大分子本体内分布均匀,均一性好,流体性能好,不会堵塞喷丝孔,特别适合于湿法纺丝。
4、可溶性非卤化物钙盐和锌盐的选用,避免了过量氯离子能促进纳米氯化银团聚增大而失去纳米尺寸的弊端。
5、用硼盐溶液(硼酸:硼砂=4:1)喷洗初生钙化纤维,表面生成少量硼化钙,具有耐盐、耐洗涤剂作用,克服了海藻酸盐不耐盐、不耐洗涤剂的缺陷。
6、蒸汽干燥消除了纤维的内应力,克服了纤维的脆性,使纤维具有良好的弹性,易于织造成布或者制造无纺布。
7、该工艺简单,可操作性强,无污染,材料环境友好,适合大批量工业化生产。
附图说明
图1:实施例1中成品材料的电镜图;
图2:实施例4中成品材料的电镜图;
图3:实施例2中成品材料的电镜图;
图4:实施例5中成品材料的电镜图;
图5:实施例3中成品材料的电镜图;
图6:实施例6中成品材料的电镜图。
具体实施方式
下面对本发明的具体实施方式作进一步详细的说明,但本发明并不局限于这些实施方式,任何在本实施例基本精神上的改进或代替,仍属于本发明权利要求所要求保护的范围。
实施例1
一种负载纳米氯化银的海洋纤维的制备方法,包括以下步骤:
(1)分别将氯化钠、平均分子量≥12万的聚乙烯吡咯烷酮K90、海藻酸钠、去离子水按照1:0.2:20:450的质量比配成溶液A;具体是:先将去离子水加热至40℃,在超声波作用下,再依次将聚乙烯吡咯烷酮K90、氯化物和海藻酸钠溶于其中,维持反应50min后即得;
(2)称取与氯化钠等摩尔的硝酸银,再分别将硝酸银、25%氨水、去离子水按照1:5.5:6的质量比配成溶液B;具体是:先在常温条件下将硝酸银溶解于水中,后在搅拌条件下将25%氨水滴加入硝酸银溶液中,再维持搅拌反应4min,即得;
(3)在40℃水浴加热以及搅拌下将溶液B滴加到溶液A中,至反应液变成乳白色时终止搅拌,并在40℃下恒温静置养护15min,即得结晶物C;
(4)按照结晶物C与2%的乳酸钙溶液为1:7的质量比,将结晶物C在湿法纺丝设备中喷丝成形后于2%的乳酸钙溶液中交联反应12min,制得纤维后,用0.2%硼盐溶液喷洗2次,再用去离子水浸洗4次,最后蒸汽干燥、热拉伸,冷至常温即为成品;
所述硼盐由硼酸与硼砂按质量比4:1组成。
实施例2
一种负载纳米氯化银的海洋纤维的制备方法,包括以下步骤:
(1)分别将氯化钾、平均分子量≥12万的聚乙烯吡咯烷酮K90、海藻酸钠、去离子水按照1:0.1:15:400的质量比配成溶液A;先将去离子水加热至30℃,在超声波作用下,再依次将聚乙烯吡咯烷酮K90、氯化物和海藻酸钠溶于其中,维持反应60min后即得;
(2)称取与氯化钾等摩尔的硝酸银,再分别将硝酸银、25%氨水、去离子水按照1:5:5的质量比配成溶液B;具体是:先在常温条件下将硝酸银溶解于水中,后在搅拌条件下将25%氨水滴加入硝酸银溶液中,再维持搅拌反应3min,即得;
(3)在50℃水浴加热以及搅拌下将溶液B滴加到溶液A中,至反应液变成乳白色时终止搅拌,并在45℃下恒温静置养护10min,即得结晶物C;
(4)按照结晶物C与1%硝酸锌溶液为1:10的质量比,将结晶物C在湿法纺丝设备中喷丝成形后于1%硝酸锌溶液中交联反应10min,制得纤维后,用0.1%硼盐溶液喷洗1次,再用去离子水浸洗5次,最后蒸汽干燥、热拉伸,冷至常温即为成品;
所述硼盐由硼酸与硼砂按质量比4:1组成。
实施例3
一种负载纳米氯化银的海洋纤维的制备方法,包括以下步骤:
(1)分别将氯化铵、平均分子量≥12万的聚乙烯吡咯烷酮K90、海藻酸钠、去离子水按照1:0.3:25:500的质量比配成溶液A;具体是:先将去离子水加热至50℃,在超声波作用下,再依次将聚乙烯吡咯烷酮K90、氯化物和海藻酸钠溶于其中,维持反应30min后即得;
(2)称取与氯化铵等摩尔的硝酸银,再分别将硝酸银、25%氨水、去离子水按照1:6:7的质量比配成溶液B;具体是:先在常温条件下将硝酸银溶解于水中,后在搅拌条件下将25%氨水滴加入硝酸银溶液中,再维持搅拌反应5min,即得;
(3)在35℃水浴加热以及搅拌下将溶液B滴加到溶液A中,至反应液变成乳白色时终止搅拌,并在50℃下恒温静置养护20min,即得结晶物C;
(4)按照结晶物C与3%醋酸钙和醋酸锌等质量比混合溶液为1:5的质量比,将结晶物C在湿法纺丝设备中喷丝成形后于3%醋酸钙和醋酸锌等质量比混合溶液中交联反应15min,制得纤维后,用0.3%硼盐溶液喷洗3次,再用去离子水浸洗3次,最后蒸汽干燥、热拉伸,冷至常温即为成品;
所述硼盐由硼酸与硼砂按质量比4:1组成。
实施例4
一种负载纳米氯化银的海洋纤维的制备方法,包括以下步骤:
(1)分别将海藻酸钠、去离子水按照20:450的质量比配成溶液A;具体是先将去离子水加热到40℃,在超声作用下再慢慢将海藻酸钠加入其中溶解完全,维持45min即得;
(2)称取海藻酸钠质量5%的硝酸银,再分别将硝酸银、25%氨水、去离子水按照1:5.5:6的质量比配成溶液B;具体是:在常温条件下将硝酸银溶解于去离子水中,然后在搅拌下将25%氨水滴加入硝酸银溶液中,再维持搅拌反应4min,即得;
(3)在40℃水浴加热,搅拌条件下,将溶液B滴加到溶液A中,然后在40℃恒温下反应15min得到结晶物C;
(4)按照结晶物C与2%氯化钙溶液为1:7的质量比,将结晶物C在湿法纺丝设备中喷丝成形后于2%氯化钙溶液中交联反应12min,反应中会同时生成海藻酸钙和氯化银,制得纤维后,用0.2%硼盐溶液喷洗2次,再用去离子水浸洗4次,最后蒸汽干燥,冷至常温即为成品;
所述硼盐由硼酸与硼砂按质量比4:1组成。
实施例5
一种负载纳米氯化银的海洋纤维的制备方法,包括以下步骤:
(1)分别将氯化钾、海藻酸钠、去离子水按照1:15:400的质量比配成溶液A;具体是先将氯化钾溶解于去离子水中,加热到30℃,在超声作用下再慢慢将海藻酸钠加入其中溶解完全,维持60min即得;
(2)称取与氯化钾等摩尔的硝酸银,再分别将硝酸银、25%氨水、去离子水按照1:5:5的质量比配成溶液B;具体是:在常温条件下将硝酸银溶解于去离子水中,然后在搅拌下将25%氨水滴加入硝酸银溶液中,再维持搅拌反应3min,即得;
(3)50℃水浴加热,在搅拌下将溶液B滴加到溶液A中,见到反应液变成乳白色时终止搅拌,并在45℃下恒温静置养护10min得结晶物C;
(4)按照结晶物C与1%硝酸钙溶液为1:10的质量比,将结晶物C在湿法纺丝设备中喷丝成形后于1%硝酸钙溶液中交联反应10min,制得纤维后,用0.1%硼盐溶液喷洗1次,再用去离子水浸洗5次,最后蒸汽干燥、热拉伸,冷至常温即为成品;
所述硼盐由硼酸与硼砂按质量比4:1组成。
实施例6
(1)分别将氯化铵、平均分子量≥12万的聚乙烯吡咯烷酮K90、海藻酸钠、去离子水按照1:0.3:25:500的质量比配成溶液A;具体是:先将氯化铵溶于去离子水中,然后将其加热到50℃,在超声作用下再慢慢将高分子量聚乙烯吡咯烷酮K90和海藻酸钠依次加入其中溶解完全,维持30min即得;
(2)称取与氯化铵等摩尔的硝酸银,再分别将硝酸银、25%氨水、去离子水按照1:6:7的质量比配成溶液B;具体是:先在常温条件下将硝酸银溶解于水中,后在搅拌条件下将25%氨水滴加入硝酸银溶液中,再维持搅拌反应5min,即得;
(3)在35℃水浴加热以及搅拌下将溶液B滴加到溶液A中,至反应液变成乳白色时终止搅拌,并在50℃下恒温静置养护20min,即得结晶物C;
(4)按照结晶物C与3%氯化钙溶液为1:5的质量比,将结晶物C在湿法纺丝设备中喷丝成形后于3%氯化钙溶液中交联反应15min,反应中会同时生成海藻酸钙和氯化银,制得纤维后,用0.3%硼盐溶液喷洗3次,再用去离子水浸洗3次,最后蒸汽干燥、热拉伸,冷至常温即为成品;
所述硼盐由硼酸与硼砂按质量比4:1组成。
图1:实施例1中成品材料的电镜图;即氯化银和海藻酸钙两步法生成负载纳米氯化银的海洋纤维的电镜图;
图2:实施例4中成品材料的电镜图;即氯化银和海藻酸钙一步法生成载银的海洋纤维的电镜图;
通过比较图1和图2,可知:一步法生成工艺中的氯化银为微米级,团聚现象明显,两步法生成工艺中的氯化银为纳米级,粒径在5-50纳米之间;由此说明:本发明创造中两步法克服了一步法工艺不易得到纳米氯化银的缺陷。
图3:实施例2中成品材料的电镜图;即本发明创造保护范围内工艺生产的负载纳米氯化银的海洋纤维的电镜图;
图4:实施例5中成品材料的电镜图;即与本发明创造性保护范围的工艺区别在于未添加PVP K90条件下生产的负载纳米氯化银的海洋纤维的电镜图;
通过比较图3和图4,可知:未添加PVP时氯化银有超过1200纳米的微米级颗粒;而添加高分子量聚乙烯吡咯烷酮K90两步法工艺中的氯化银为纳米级,粒径在5-20纳米之间;由此说明:PVP K90起到了有效控制氯化银晶核生长的作用,从而克服了一步法工艺不易得到纳米氯化银的缺陷;
图5:实施例3中成品材料的电镜图;
图6:实施例6中成品材料的电镜图;
由图5和图6可知:图5是采用以醋酸钙和醋酸锌混合溶液为交联剂,凝固浴两步法生产的载银海洋纤维的电镜图,而图6是采用以氯化钙为交联剂,凝固浴两步法生产的负载纳米氯化银的海洋纤维的电镜图,图6中存在大量超过1000纳米的微米级氯化银颗粒,说明氯离子起到了促进氯化银团聚增长的作用,而采用非氯离子钙盐和锌盐,能够维持氯化银为纳米级,粒径在50纳米以下。
表1海藻酸钙纤维材料和实施例1纤维材料的阻燃数据对比
UL-94:垂直燃烧实验阻燃材料级别;LOI:极限氧指数;PHRR:释热速率;THR:总释热量;TSR:总释烟量;Residue:热分解残渣量。
测试条件:
极限氧指数(LOI)根据ISO 4589-1:1996标准方法,在LFY-606B型数字极限氧指数测定仪上进行了LOI测试。所有样品的尺寸均为130mm×10mm。
垂直燃烧(UL-94)数据采用ANST/UL-94-1985标准方法,在LFY-601A型垂直燃烧速率测试仪上进行试验。所有样品的尺寸均为130mm×13mm×5mm。
燃烧性能PHRR、THR、TSR、Residue等数据由CONE试验获得:使用FTT-0242锥形量热仪(英国),根据ISO 5660标准,在50kW/m2的外部热通量下检查燃烧行为。所有样品的尺寸为100mm×100mm×2mm。
表1为海藻酸钙纤维材料和实施例1纤维材料的阻燃数据对比。尽管两者均达到UL-94标准中的V-0阻燃等级,但实施例1的极限氧指数超过了60%,耐火性能得到大幅度提高。并且实施例1的热释放速率、总热释放量都显著低于海藻酸钙纤维材料。
尤其是,说表1中的实施例1的负载纳米氯化银的海洋纤维材料的总释烟量特低,仅是海藻酸钙纤维材料的3.5%,实现了海藻多糖纤维材料的超低发烟量目标。
表2海藻酸钙纤维材料和实施例1-3纤维材料的抗菌性数据对比
E.coli:大肠杆菌(革兰氏阴性菌);S.aureus:金黄色葡萄球菌(革兰氏阳性菌)。
抗菌性能测试依据标准和方法:
采用圆盘扩散法和菌落形成计数法检测纯CA和实施例CA/AgCl复合材料的抗菌活性。在溶源性肉汤培养基中培养大肠杆菌(ATCC25922),在37%的氯化钠肉汤培养基中将金黄色葡萄球菌(ATCC6538)培养过夜。
在圆盘扩散法中,抑制区测试基于AATCC-90(光晕测试)。将灭菌的平板琼脂倒入培养皿中并冷却。将50μL的大肠杆菌和金黄色葡萄球菌细菌悬浮液铺展在琼脂表面并均匀铺展。然后将水凝胶置于平板琼脂表面,并在37℃黑暗中孵育24h。抑制带的作用可以通过初步观察来判断。使用以下方法评估样品的抗菌活性:抗菌作用的等级为“好”(抑制区>1mm),“相当好”(抑制区≤1mm),“足够”(生长)。直至(但不是在水凝胶上),“有限”(在水凝胶上有限的生长)或“差”(水凝胶中细菌≥50%长满)。抑制区域表示为无细菌生长的直径减去水凝胶的直径。抑制区直接显示了复合纤维材料的抗菌特性。
在菌落形成计数方法中,将CA/AgCl颗粒溶解在磷酸盐缓冲盐水(PBS)中,以获得10mg/L的溶液。将细菌悬浮液稀释至102-103CFU mL-1,然后移取50μL与溶解溶液混合的溶液。孵育后,移取50μL,在37℃下培养过夜。最后,计算菌落数,抑制率的百分比表示为以下等式:
抗菌率=(对照组-实验组)/(对照组)×100%
实验前将所有材料在高压釜中灭菌。每个样品重复三次,结果取平均值。
表2为实施例1-3制备的负载纳米氯化银的海洋纤维材料和海藻酸钙纤维材料的抗菌性能对比。可见纯海藻酸钙纤维材料的抑菌率为0,实施例1-3制备的负载纳米氯化银的海洋纤维材料对大肠杆菌和金黄色葡萄球菌抑菌率的抑菌率均大于99%。
Claims (10)
1.一种负载纳米氯化银的海洋纤维的制备方法,其特征在于,包括以下步骤:
(1)配制溶液A:先将去离子水加热至30-50℃,在超声波作用下,再依次将聚乙烯吡咯烷酮K90、氯化物和海藻酸钠溶于其中,维持反应30-60min后即得;
(2)配制溶液B:称取与氯化物等摩尔的硝酸银,在常温下将硝酸银溶解于去离子水中,然后在搅拌下将氨水滴加至溶液中,再维持搅拌反应3-5min,即得;
(3)制备结晶物C:在35-50℃水浴加热、搅拌条件下将溶液B滴加到溶液A中,然后,见到反应液变成乳白色时终止搅拌,并40-50℃恒温养护10-20min,即得;
(4)按照结晶物C与可溶性非卤化物盐溶液为1:5-10的质量比,将结晶物C在湿法纺丝设备中喷丝成形后于可溶性非卤化物盐溶液中交联反应10-15min,制得纤维后,用硼盐溶液喷洗1-3次,再用去离子水浸洗3-5次,再蒸汽干燥、热拉伸,冷却至常温,即得负载纳米氯化银的海洋纤维。
2.如权利要求1所述一种负载纳米氯化银的海洋纤维的制备方法,其特征在于,所述氯化物为氯化钠、氯化钾、氯化铵中任意一种或多种组合。
3.如权利要求1或2所述一种负载纳米氯化银的海洋纤维的制备方法,其特征在于,所述氯化物为氯化钠。
4.如权利要求1所述一种负载纳米氯化银的海洋纤维的制备方法,其特征在于,所述溶液A中氯化物、聚乙烯吡咯烷酮、海藻酸钠、去离子水的质量比为1:(0.1-0.3):(15-25):(400-500)。
5.如权利要求1所述一种负载纳米氯化银的海洋纤维的制备方法,其特征在于,所述聚乙烯吡咯烷酮,其平均分子量为≥12万。
6.如权利要求1所述一种负载纳米氯化银的海洋纤维的制备方法,其特征在于,所述可溶性非卤化物盐为硝酸钙、醋酸钙、乳酸钙、硝酸锌、醋酸锌、乳酸锌中任意一种或多种组合。
7.如权利要求1所述一种负载纳米氯化银的海洋纤维的制备方法,其特征在于,所述溶液B中硝酸银、氨水、去离子水的质量比为1:(5-6):(5-7)。
8.如权利要求1所述一种负载纳米氯化银的海洋纤维的制备方法,其特征在于,所述氨水,其体积浓度为25%。
9.如权利要求1所述一种负载纳米氯化银的海洋纤维的制备方法,其特征在于,所述硼盐溶液,其质量浓度为0.1-0.3%。
10.如权利要求1或9所述一种负载纳米氯化银的海洋纤维的制备方法,其特征在于,所述硼盐由硼酸与硼砂按质量比4:1组成。
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