CN116905263A - 一种高均匀聚合度特种精制棉生产方法 - Google Patents
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Abstract
本发明公开了一种高均匀聚合度特种精制棉生产方法,其方法包括以下步骤:选料、开棉、除杂,配碱、浸渍、蒸煮、前除杂、洗涤、打浆精浆、预漂白、碱处理、漂白、脱氯、后除杂,最后烘干制得絮状成品,所述选料、开棉、除杂:选取成熟度≥85%的二级棉短绒,新疆北疆,通过将短绒撕松、除杂,经旋风分离送至预浸,优选的,所述配碱、浸渍:将质量浓度3.0~3.5%的NaOH溶液蒸煮剂加热至75~80℃,将0.5~1.0%蒸煮渗透剂与蒸煮剂充分混合形成蒸煮液,蒸煮液比1:3.0~4.0,本发明优点是:控制精制棉成熟度达到75%,纤维饱满,在有限的硝化时间内,硝化程度趋于均匀,保障精制棉在硝化工艺中制备高氮量NC均匀性高,有利于提高纤维聚合度的均匀性。
Description
技术领域
本发明涉及一种精制棉生产方法的技术领域,更具体地说是涉及一种特种精制棉生产方法的技术领域。
背景技术
精制棉是以棉花副产品棉短绒经蒸煮、漂白而生产的一种棉纤维素基础材料,也是生产军火炸药唯一材料。由于精制棉采用棉短绒原料,其杂质多、纤维一致性差,以及原料品质不稳定、蒸漂过程降解剧烈,产品的聚合度难以有效控制,同一规格产品聚合度波动范围达到200~300,在2023年5月发布实施的精制棉(GB/T9107~2023)同规格产品聚合度范围仍然定在200~300。聚合度范围宽,生产的精制棉难以满足衍生加工军工发射药对硝化棉的加工性能和力学性能要求,以致于生产的军火炸药在使用时,火炸药燃烧不充分,产生烟雾等重大质量问题,严重影响战斗力。聚合度波动范围大,是生产精制棉共性卡脖子瓶颈。
同时,精制棉原料棉短绒品质及成熟度直接关系精制棉产品品质,包括聚合度控制。经过有关军工企业和高校大量研究表明,控制精制棉成熟度,事关后续硝化工艺对高氮量 NC 硝化均匀性的影响,高成熟度的精制棉也是控制关键。
发明内容
本发明的目的在于提供一种高均匀聚合度特种精制棉生产方法,本申请的生产方法产品聚合度波动范围控制在100以内、成熟度超过75%,符合生产特种用精制棉的质量要求。
一种高均匀聚合度特种精制棉生产方法,其方法包括以下步骤:选料、开棉、除杂,配碱、浸渍、蒸煮、前除杂、洗涤、打浆精浆、预漂白、碱处理、漂白、脱氯、后除杂,最后烘干制得絮状成品。
优选的,所述选料、开棉、除杂:选取成熟度≥85%的二级棉短绒,新疆北疆,通过将短绒撕松、除杂,经旋风分离送至预浸。
优选的,所述配碱、浸渍:将质量浓度3.0~3.5%的NaOH溶液蒸煮剂加热至75~80℃,将0.5~1.0%蒸煮渗透剂与蒸煮剂充分混合形成蒸煮液,蒸煮液比1:3.0~4.0,再通过螺旋压榨将蒸煮液均匀渗浸棉短绒纤维中。所述蒸煮渗透剂由绿氧、乙二胺四乙酸组成,按1.8:1复配;
优选的,所述蒸煮:相对短绒原料绝干浆量,在蒸煮器中加入EC-C-纤维保护剂0.2~0.5%、蒸煮复合助剂0.05~0.1%、HB稳定剂0.3~0.5%、27.5%双氧水0.5~1.0%;蒸煮分三段进行,一段蒸煮升温100~120 min ,温度升至118~120℃,恒温30min;二段蒸煮升温20~30min,温度升至130~135℃,恒温60min,小放汽;三段蒸煮升温50~60 min,温度升至140℃,恒温100~120min,温度保持在140±1℃。所述蒸煮复合助剂由质量分数0.01~0.03%的三氧化硫和0.04~0.07%的单乙醇胺组成,三氧化硫的浓度为99.0%,单乙醇胺的纯度为99.0%。
优选的,所述前除杂:将浆料浓缩至3~4%,循环除杂60~90 min。
优选的,所述洗涤:将浆料加热至60~70℃,循环洗涤50~60min。
优选的,所述打浆精浆:槽式打浆机进行打浆,电流控制在100~130A,叩解70~80min,纤维长度3.8~4.0mm;精浆机循环精浆110~120min,电流300~320A,纤维长度 3.1~3.3mm。
优选的,所述预漂白:浆料浓缩至4~5%后,加热至40~45℃;漂白机内加入0.1%-0.2%二氧化氯,0.01~0.1%FSA螯合分散剂,反应30~40 min。
优选的,所述碱处理:将浆料浓缩至4~5%后,用1~1.2%的30%NaOH溶液和0.02~0.5%碳酸镁溶液进行碱处理,反应30~40 min,浆料温度控制在30℃±1℃。
优选的,所述漂白:浆料浓缩至4~5%后,加热至50~55℃;漂白机内加入0.3%-0.5%二氧化氯,0.01~0.5%FSA螯合分散剂,反应50~60 min。
优选的,所述脱氯:漂白结束后,浆料浓缩至4~5%加入0.3~0.5%硫代硫酸钠进行脱氯处理,反应10~20 min。
优选的,所述后除杂:浆料浓度调整到2~3%,用水洗涤40~60 min,浆料浓度调整到0.5~0.6%进行低浓后除杂,进浆压力2.0~3.0MPa。
本发明取得的有益效果:
1、控制精制棉成熟度达到75%,纤维饱满,在有限的硝化时间内,硝化程度趋于均匀,保障精制棉在硝化工艺中制备高氮量NC均匀性高;
2、打浆和精浆结合使用,既提升纤维韧性和纤维长度一致性,有利于提高纤维聚合度的均匀性;
3、对蒸煮剂、碱处理与漂白前的浆料进行加热,促进纤维充分反应,提高反应性能;
4、蒸漂过程将由传统的单一的蒸漂助剂改进为蒸漂复合助剂,有利于保护纤维,控制蒸漂过程无序降聚,有利控制聚合度波动。同时,结合前后除杂洗涤,进一步降低杂质等含量。
实验表明,本发明中的生产方法得到的产品,聚合度1400~1500±50,成熟度75%,灰分含量0.05%,硫酸不溶物0.06%,白度88%,吸湿度156g,杂质3个/625cm2,反应性能良好,符合生产特种精制棉的质量要求。
实施方式
为了进一步说明本发明,以下结合实施例对本发明提供的一种高均匀聚合度特种精制棉生产方法进行详细描述,但不能将其理解为对本发明保护范围的限定。
实施例
一种高均匀聚合度特种精制棉生产方法,其方法包括以下步骤:
选料、开棉、除杂:选取成熟度85%的二级棉短绒,新疆北疆,通过将短绒撕松、除杂,经旋风分离送至预浸;
配碱、浸渍:将质量浓度3.0%的NaOH溶液蒸煮剂加热至80℃,将0.5%蒸煮渗透剂与蒸煮剂充分混合形成蒸煮液,蒸煮液比1:3.0,再通过螺旋压榨将蒸煮液均匀渗浸棉短绒纤维中。所述蒸煮渗透剂由绿氧、乙二胺四乙酸组成,按1.8:1复配;
蒸煮:相对短绒原料绝干浆量,在蒸煮器中加入EC-C-纤维保护剂0.5%、蒸煮复合助剂0.1%、HB稳定剂0.5%、27.5%双氧水1.0%;蒸煮分三段进行,一段蒸煮升温100min ,温度升至118℃,恒温30min;二段蒸煮升温30min,温度升至135℃,恒温60min,小放汽;三段蒸煮升温50min,温度升至140℃,恒温120min,温度保持在140℃;
前除杂:将浆料浓缩至4%,循环除杂90min;
洗涤:将浆料加热至70℃,循环洗涤50min;
打浆精浆:槽式打浆机进行打浆,电流控制在130A,叩解70min,纤维长度4.0mm;精浆机循环精浆120min,电流300A,纤维长度 3.1mm;
预漂白:浆料浓缩至4%后,加热至40℃;漂白机内加入0.1%二氧化氯,0.01%FSA螯合分散剂,反应40 min;
碱处理:将浆料浓缩至5%后,用1.2%的30%NaOH溶液和0.5%碳酸镁溶液进行碱处理,反应40 min,浆料温度控制在30℃;
漂白:浆料浓缩至4%后,加热至55℃;漂白机内加入0.3%二氧化氯,0.5%FSA螯合分散剂,反应60 min;
脱氯:漂白结束后,浆料浓度再4%加入0.3%硫代硫酸钠进行脱氯处理,反应10min;
后除杂:浆料浓度调整到3%,用水洗涤60 min,浆料浓度调整到0.5%进行低浓后除杂,进浆压力2.0Mpa;
最后烘干制得絮状产品。经检测,产品聚合度1457,聚合度波动范围87,成熟度74%,灰分含量0.05%,硫酸不溶物0.05%,白度87%,吸湿度153g,杂质3个/625cm2。
实施例2:
一种高均匀聚合度特种精制棉生产方法,其方法包括以下步骤:
选料、开棉、除杂:选取成熟度85%的二级棉短绒,新疆北疆,通过将短绒撕松、除杂,经旋风分离送至预浸;
配碱、浸渍:将质量浓度3.5%的NaOH溶液蒸煮剂加热至75℃,将1.0%蒸煮渗透剂与蒸煮剂充分混合形成蒸煮液,蒸煮液比1:4.0,再通过螺旋压榨将蒸煮液均匀渗浸棉短绒纤维中。所述蒸煮渗透剂由绿氧、乙二胺四乙酸组成,按1.8:1复配;
蒸煮:相对短绒原料绝干浆量,在蒸煮器中加入EC-C-纤维保护剂0.2%、蒸煮复合助剂0.05%、HB稳定剂0.3%、27.5%双氧水0.5%;蒸煮分三段进行,一段蒸煮升温120 min ,温度升至120℃,恒温30min;二段蒸煮升温20min,温度升至130℃,恒温60min,小放汽;三段蒸煮升温60 min,温度升至140℃,恒温100min,温度保持在139℃;
前除杂:将浆料浓缩至3%,循环除杂60min;
洗涤:将浆料加热至60℃,循环洗涤60min;
打浆精浆:槽式打浆机进行打浆,电流控制在100A,叩解80min,纤维长度3.8mm;精浆机循环精浆110min,电流320A,纤维长度 3.3mm;
预漂白:浆料浓缩至5%后,加热至45℃;漂白机内加入0.15%二氧化氯,0.1%FSA螯合分散剂,反应30 min;
碱处理:将浆料浓缩至4%后,用1%的30%NaOH溶液和0.02%碳酸镁溶液进行碱处理,反应30 min,浆料温度控制在31℃;
漂白:浆料浓缩至5%后,加热至50℃;漂白机内加入0.4%二氧化氯,0.01%FSA螯合分散剂,反应50 min;
脱氯:漂白结束后,浆料浓度再5%加入0.5%硫代硫酸钠进行脱氯处理,反应20min;
后除杂:浆料浓度调整到2%,用水洗涤40 min,浆料浓度调整到0.6%进行低浓后除杂,进浆压力3.0Mpa;
最后烘干制得絮状产品。经检测,产品聚合度1471,聚合度波动范围73,成熟度75%,灰分含量0.04%,硫酸不溶物0.06%,白度88%,吸湿度157g,杂质2个/625cm2。
实施例3:
一种高均匀聚合度特种精制棉生产方法,其方法包括以下步骤:
选料、开棉、除杂:选取成熟度85%的二级棉短绒,新疆北疆,通过将短绒撕松、除杂,经旋风分离送至预浸;
配碱、浸渍:将质量浓度3.2%的NaOH溶液蒸煮剂加热至78℃,将0.9%蒸煮渗透剂与蒸煮剂充分混合形成蒸煮液,蒸煮液比1:3.3,再通过螺旋压榨将蒸煮液均匀渗浸棉短绒纤维中。所述蒸煮渗透剂由绿氧、乙二胺四乙酸组成,按1.8:1复配;
蒸煮:相对短绒原料绝干浆量,在蒸煮器中加入EC-C-纤维保护剂0.35%、蒸煮复合助剂0.08%、HB稳定剂0.36%、27.5%双氧水0.85%;蒸煮分三段进行,一段蒸煮升温116 min ,温度升至120℃,恒温30min;二段蒸煮升温28min,温度升至135℃,恒温60min,小放汽;三段蒸煮升温55min,温度升至140℃,恒温110min,温度保持在141℃;
前除杂:将浆料浓缩至3.5%,循环除杂85 min;
洗涤:将浆料加热至66℃,循环洗涤55min;
打浆精浆:槽式打浆机进行打浆,电流控制在120A,叩解75min,纤维长度3.8mm;精浆机循环精浆115min,电流310A,纤维长度 3.2mm;
预漂白:浆料浓缩至4.5%后,加热至45℃;漂白机内加入0.2%二氧化氯,0.06%FSA螯合分散剂,反应35min;
碱处理:将浆料浓缩至4.5%后,用1.2%的30%NaOH溶液和0.25%碳酸镁溶液进行碱处理,反应35min,浆料温度控制在30℃;
漂白:浆料浓缩至4%后,加热至55℃;漂白机内加入0.5%二氧化氯,0.3%FSA螯合分散剂,反应56min;
脱氯:漂白结束后,浆料浓度再4.6%加入0.45%硫代硫酸钠进行脱氯处理,反应15min;
后除杂:浆料浓度调整到2.6%,用水洗涤50 min,浆料浓度调整到0.55%进行低浓后除杂,进浆压力2.5Mpa;
最后烘干制得絮状产品。经检测,产品聚合度1451,聚合度波动范围82,成熟度77%,灰分含量0.04%,硫酸不溶物0.05%,白度89%,吸湿度155g,杂质3个/625cm2。
上述具体实施方式中,EC-C-纤维保护剂、HB稳定剂、FSA螯合分散剂为现有产品;所述蒸煮复合助剂的成份如下:所述蒸煮复合助剂由质量分数0.01~0.03%的三氧化硫和0.04~0.07%的单乙醇胺组成,三氧化硫的浓度为99.0%,单乙醇胺的纯度为99.0%。
精制棉(GB/T9107-2023)中可适宜生产军工的特种精制棉的规格有30号、60号、100号。其中30号(聚合度801~1000)、60号(聚合度1001~1300)、100号(聚合度1301~1600),聚合度范围都在200~300。墨西哥ALFA CELULOSA DE ME MEXICO,S.A.deC.V.其火炸药用精制棉产品标准黏度为100~250mPa.s(1.0%铜氨溶液),其相对应聚合度约为1400~1800,聚合度波动范围近400。
通过采用本发明和以上实施例中制备的特种精制棉生产方法,经对比可知,本申请制备的高均匀聚合度特种精制棉生产方法聚合度波动范围小,均控制在100以内,而且各项技术性能优越。同时,从原料纤维到产品纤维,均控制其成熟度,更有利于保障精制棉在军工特种领域的运用。
以上所述仅是本发明的优选实施方式,应当指出,所属本技术领 域的技术人员对所描述的具体实施例进行的改进和优化,但在本发明原理的范围内,均应属于本发明的保护范围。
Claims (9)
1.一种高均匀聚合度特种精制棉生产方法,其特征在于:包括以下步骤:选料、开棉、除杂,配碱、浸渍、蒸煮、前除杂、洗涤、打浆精浆、预漂白、碱处理、漂白、脱氯、后除杂,最后烘干制得絮状产品,产品聚合度波动范围控制在100以内、成熟度超过75%,符合生产特种用精制棉的质量要求。
2.根据权利要求1所述的一种高均匀聚合度特种精制棉生产方法,其特征在于:所述选料、开棉、除杂,选取成熟度≥85%的二级棉短绒,新疆北疆。
3.根据权利要求1所述的一种高均匀聚合度特种精制棉生产方法,其特征在于:所述配碱、浸渍,将质量浓度3.0~3.5%的NaOH溶液蒸煮剂加热至75~80℃,将0.5~1.0%蒸煮渗透剂与蒸煮剂充分混合形成蒸煮液。
4.根据权利要求1所述的一种高均匀聚合度特种精制棉生产方法,其特征在于:所述蒸煮,相对短绒原料绝干浆量,在蒸煮器中加入EC-C-纤维保护剂0.2~0.5%、蒸煮复合助剂0.05~0.1%、HB稳定剂0.3~0.5%、27.5%双氧水0.5~1.0%;蒸煮分三段进行,一段蒸煮升温100~120 min ,温度升至118~120℃,恒温30min;二段蒸煮升温20~30min,温度升至130~135℃,恒温60min,小放汽;三段蒸煮升温50~60 min,温度升至140℃,恒温100~120min,温度保持在140±1℃。
5.根据权利要求4所述的一种高均匀聚合度特种精制棉生产方法,所述蒸煮复合助剂由质量分数0.01~0.03%的三氧化硫和0.04~0.07%的单乙醇胺组成,三氧化硫的浓度为99.0%,单乙醇胺的纯度为99.0%。
6.根据权利要求1所述的一种高均匀聚合度特种精制棉生产方法,其特征在于:所述洗涤,将浆料加热至60~70℃,循环洗涤50~60min。
7.根据权利要求1所述的一种高均匀聚合度特种精制棉生产方法,其特征在于:所述打浆精浆,槽式打浆机进行打浆,电流控制在100~130A,叩解70~80min,纤维长度3.8~4.0mm;精浆机循环精浆110~120min,电流300~320A,纤维长度 3.1~3.3mm。
8.根据权利要求1所述的一种高均匀聚合度特种精制棉生产方法,其特征在于:所述预漂白,浆料浓缩至4~5%后,加热至40~45℃;漂白机内加入0.1%-0.2%二氧化氯,0.01~0.1%FSA螯合分散剂,反应30~40 min。
9.根据权利要求1所述的一种高均匀聚合度特种精制棉生产方法,其特征在于:所述漂白,浆料浓缩至4~5%后,加热至50~55℃;漂白机内加入0.3%-0.5%二氧化氯,0.01~0.5%FSA螯合分散剂,反应50~60 min。
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