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CN104003565B - Method for recovering multi-component waste liquid in production process of high-performance aramid fiber - Google Patents

Method for recovering multi-component waste liquid in production process of high-performance aramid fiber Download PDF

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CN104003565B
CN104003565B CN201410230638.4A CN201410230638A CN104003565B CN 104003565 B CN104003565 B CN 104003565B CN 201410230638 A CN201410230638 A CN 201410230638A CN 104003565 B CN104003565 B CN 104003565B
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waste liquid
extraction agent
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aramid fiber
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CN104003565A (en
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钟彤
钟向华
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Dongguan Cansen New Materials Co ltd
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Abstract

本发明公开了一种高性能芳纶纤维生产过程中多组份废液的回收方法,本发明采用先萃取后蒸馏的办法,同时通过蒸发器对第一塔的塔顶出来的液体进行浓缩处理,可以达到纤维生产循环使用的要求,解决了普通蒸馏处理能耗高的问题,达到循环使用的经济目的,提高经济效益,降低生产成本,同时不会污染环境,环保节能。

The invention discloses a method for recovering multi-component waste liquid in the production process of high-performance aramid fiber. The invention adopts the method of first extracting and then distilling, and at the same time, the liquid coming out of the top of the first tower is concentrated by an evaporator, so as to meet the requirements of fiber production recycling, solve the problem of high energy consumption of ordinary distillation treatment, achieve the economic purpose of recycling, improve economic benefits, reduce production costs, and at the same time will not pollute the environment, and is environmentally friendly and energy-saving.

Description

一种高性能芳纶纤维生产过程中多组份废液的回收方法A method for recycling multi-component waste liquid in the production process of high-performance aramid fibers

技术领域technical field

本发明涉及一种高性能芳纶纤维生产过程中多组份废液的回收方法,具体涉及一种高性能聚间苯二甲酰间苯二胺纤维生产过程中的多组份废液的回收方法。The invention relates to a recovery method of multi-component waste liquid in the production process of high-performance aramid fiber, in particular to a recovery method of multi-component waste liquid in the production process of high-performance polym-phenylene isophthalamide fiber method.

背景技术Background technique

现有技术中,聚间苯二甲酰间苯二胺聚合物经过中和、过滤和脱泡处理,通过喷头在凝固液里面凝固成型,再通过牵伸、水洗、烘干和定型,最终得到的高性能聚间苯二甲酰间苯二胺纤维,高性能聚间苯二甲酰间苯二胺纤维的强度很高,其截面不是规则的圆形或者椭圆形,而是不规则的宽带状或者腰豆状。在高性能聚间苯二甲酰间苯二胺纤维的生产过程中会产生废液,废液的组成成分有:酰胺溶剂、盐和分散剂等,聚间苯二甲酰间苯二胺纤维生产过程产生的废水的组份繁多,废水的组份比较复杂,对其废水的回收处理和循环利用技术目前国内外少有介绍其技术。用一般的精馏技术很难把各组份分离干净,分离过程所需要的能耗很高,耗能严重,对废液的处理成本很高,经济效益非常低。因此,有必要给予改进。In the prior art, the polym-phenylene isophthalamide polymer is neutralized, filtered and defoamed, solidified and formed in the coagulation liquid through the nozzle, and then stretched, washed, dried and shaped to finally obtain The high-performance polym-phenylene isophthalamide fiber, the high-performance polym-phenylene isophthalamide fiber has high strength, and its cross-section is not a regular circle or oval, but an irregular broadband shape or kidney bean shape. In the production process of high-performance polym-phenylene isophthalamide fiber, waste liquid will be produced. The components of waste liquid are: amide solvent, salt and dispersant, etc., polym-phenylene isophthalamide fiber The wastewater produced in the production process has many components, and the components of the wastewater are relatively complex. At present, there are few domestic and foreign introductions to the recycling and recycling technology of the wastewater. It is difficult to separate the various components by general rectification technology, the energy consumption required for the separation process is high, the energy consumption is serious, the cost of waste liquid treatment is high, and the economic benefit is very low. Therefore, it is necessary to give improvement.

发明内容Contents of the invention

针对现有技术存在的不足,本发明的目的是提供一种高性能芳纶纤维生产过程中多组份废液的回收方法,它以更加节省能耗的方法达到可以循环使用、降低生产成本、保护生产环境的目的。In view of the deficiencies in the prior art, the purpose of the present invention is to provide a recovery method for multi-component waste liquid in the production process of high-performance aramid fiber, which can be recycled, reduce production cost, The purpose of protecting the production environment.

为了实现上述目的,本发明所采用的技术方案是。In order to achieve the above object, the technical solution adopted in the present invention is.

一种高性能芳纶纤维生产过程中多组份废液的回收方法,包括以下步骤:A method for recycling multi-component waste liquid in the production process of high-performance aramid fibers, comprising the following steps:

废液收集步骤,把高性能聚间苯二甲酰间苯二胺纤维生产过程中的多组份废液收集到废液贮罐;The waste liquid collection step is to collect the multi-component waste liquid in the high-performance polym-phenylene isophthalamide fiber production process to the waste liquid storage tank;

中和步骤,通过泵把废液贮罐中的废液输到中和贮罐,废液和中和贮罐内的中和剂中和,废液的PH值调到6.8~7.2;In the neutralization step, the waste liquid in the waste liquid storage tank is transported to the neutralization storage tank through a pump, the waste liquid is neutralized with the neutralizing agent in the neutralization storage tank, and the pH value of the waste liquid is adjusted to 6.8-7.2;

压缩过滤步骤,把中和贮罐中的废液经过压滤机过滤,把其中的悬浮物过滤干净,通过泵输送到中间贮罐;In the compression filtration step, the waste liquid in the neutralization storage tank is filtered through a filter press, and the suspended solids are filtered out, and then pumped to the intermediate storage tank;

萃取步骤,中间贮罐中的废液通过泵输送进第一塔的下部,同时从第一塔的上部按照设定的比例输送萃取剂,第一塔里面填充具有高混合效果的填料,废液和萃取剂在第一塔里面进行充分的混合,从塔底出来的萃取相存放在第四贮罐中,In the extraction step, the waste liquid in the intermediate storage tank is pumped into the lower part of the first tower, and at the same time, the extraction agent is delivered from the upper part of the first tower according to the set ratio. The first tower is filled with packing with high mixing effect, and the waste liquid Fully mixed with the extractant in the first tower, and the extract phase from the bottom of the tower is stored in the fourth storage tank.

浓缩处理步骤,从第一塔的塔顶出来的液体,输送到蒸发器进行浓缩处理,输出达到纤维生产循环使用的要求第一成品含少量丙三醇的氯化钙;In the concentration treatment step, the liquid coming out from the top of the first tower is transported to the evaporator for concentration treatment, and the output meets the requirements of fiber production and recycling. The first product contains a small amount of calcium chloride of glycerol;

萃取剂脱出步骤,第四贮罐的混合液通过泵输送进第二塔的上部,在第二塔中进行萃取剂的脱出处理,从第二塔的顶部输出达到循环使用要求的第二成品萃取剂,萃取剂通过冷凝器冷凝后进入第五贮罐,第五贮罐的萃取剂通过泵输送到第一塔的上部,循环使用萃取剂;Extraction agent removal step, the mixed liquid in the fourth storage tank is pumped into the upper part of the second tower, the extraction agent is removed from the second tower, and the second product extraction that meets the recycling requirements is output from the top of the second tower The extraction agent enters the fifth storage tank after being condensed by the condenser, and the extraction agent in the fifth storage tank is transported to the upper part of the first tower by a pump, and the extraction agent is recycled;

脱水步骤,第二塔的釜底料通过泵输送到第三塔的上部,进行脱水处理;In the dehydration step, the bottom material of the second tower is transported to the upper part of the third tower by a pump for dehydration treatment;

精馏步骤,第三塔的釜底液通过泵输送到第四塔的上部,进行精馏处理;In the rectification step, the bottom liquid of the third tower is transported to the upper part of the fourth tower by a pump for rectification treatment;

成品,纯净的、聚合级的酰胺溶剂从第四塔的上部输出,酰胺溶剂通过塔顶的冷凝器冷凝后,收集得到能够重新投入生产循环使用的酰胺溶剂成品,第四塔的釜底重组份通过泵输送到废水贮罐或者焚烧处理。Finished product, pure, polymerization-grade amide solvent is output from the upper part of the fourth tower. After the amide solvent is condensed by the condenser at the top of the tower, the finished product of amide solvent that can be put into production and recycled is collected. The heavy component of the bottom of the fourth tower Pumped to waste water storage tank or incineration.

进一步的技术方案中,所述废液收集步骤中,废液包含有10~40%二甲基乙酰胺、5~20%氯化钙或氯化镁、0~10%丙三醇或者乙二醇、余量为水。In a further technical solution, in the waste liquid collection step, the waste liquid contains 10-40% dimethylacetamide, 5-20% calcium chloride or magnesium chloride, 0-10% glycerol or ethylene glycol, The balance is water.

进一步的技术方案中,所述中和步骤中,中和剂选用氢氧化钙或者氢氧化钠。In a further technical solution, in the neutralization step, the neutralizer is calcium hydroxide or sodium hydroxide.

进一步的技术方案中,所述萃取步骤中,萃取剂选用氯仿,从第一塔的上部输送萃取剂的比例为萃取剂:废水中二甲基乙酰胺有效含量=5~10:1。In a further technical solution, in the extraction step, chloroform is selected as the extractant, and the ratio of extractant delivered from the upper part of the first tower is extractant: effective content of dimethylacetamide in waste water = 5-10:1.

进一步的技术方案中,所述萃取步骤中,萃取剂选用氯仿,从第一塔的上部输送萃取剂的比例为萃取剂:废水中二甲基乙酰胺有效含量=6~8:1。In a further technical solution, in the extraction step, chloroform is selected as the extractant, and the ratio of extractant delivered from the upper part of the first tower is extractant: effective content of dimethylacetamide in waste water = 6-8:1.

进一步的技术方案中,所述萃取剂脱出步骤中,第二塔选用均一直径的常压蒸馏塔,塔釜的温度控制在105~120度,塔顶的温度通过回流控制在60~80度。In a further technical solution, in the step of extracting the extractant, the second tower is an atmospheric distillation tower with a uniform diameter, the temperature of the tower bottom is controlled at 105-120 degrees, and the temperature at the top of the tower is controlled at 60-80 degrees by reflux.

进一步的技术方案中,所述第三塔选用均一直径的减压蒸馏塔,塔釜的温度控制在115~130度,塔顶的温度控制在60~80度,真空度控制在-0.07Mpa~-0.09Mpa。In a further technical solution, the third tower is a vacuum distillation tower with a uniform diameter, the temperature of the tower kettle is controlled at 115-130 degrees, the temperature of the tower top is controlled at 60-80 degrees, and the vacuum degree is controlled at -0.07Mpa~ -0.09Mpa.

进一步的技术方案中,所述第四塔选用均一直径的减压蒸馏塔,塔釜的温度控制在120~130度,塔顶的温度控制在110~120度,真空度控制在-0.07Mpa~-0.09Mpa。In a further technical solution, the fourth tower is a vacuum distillation tower with a uniform diameter, the temperature of the tower bottom is controlled at 120-130 degrees, the temperature of the tower top is controlled at 110-120 degrees, and the vacuum degree is controlled at -0.07Mpa~ -0.09Mpa.

采用上述结构后,本发明和现有技术相比所具有的优点是:本发明采用先萃取后蒸馏的办法,同时通过蒸发器对第一塔的塔顶出来的液体进行浓缩处理,可以达到纤维生产循环使用的要求,解决了普通蒸馏处理能耗高的问题,达到循环使用的经济目的,提高经济效益,降低生产成本,同时不会污染环境,环保节能。After adopting the above-mentioned structure, the advantages of the present invention compared with the prior art are: the present invention adopts the method of extraction first and then distillation, and at the same time concentrates the liquid coming out of the top of the first tower through the evaporator, so that the The requirement of production recycling solves the problem of high energy consumption in ordinary distillation, achieves the economic purpose of recycling, improves economic benefits, reduces production costs, and at the same time does not pollute the environment, is environmentally friendly and energy-saving.

附图说明Description of drawings

下面结合附图和实施例对本发明进一步说明。The present invention will be further described below in conjunction with the accompanying drawings and embodiments.

图1是本发明的流程示意图。Fig. 1 is a schematic flow chart of the present invention.

具体实施方式detailed description

以下所述仅为本发明的较佳实施例,并不因此而限定本发明的保护范围。The following descriptions are only preferred embodiments of the present invention, and therefore do not limit the protection scope of the present invention.

实施例Example

一种高性能芳纶纤维生产过程中多组份废液的回收方法,包括以下步骤:A method for recycling multi-component waste liquid in the production process of high-performance aramid fibers, comprising the following steps:

废液收集步骤,把高性能聚间苯二甲酰间苯二胺纤维生产过程中的多组份废液收集到废液贮罐,废液包含有10~40%二甲基乙酰胺、5~20%氯化钙或氯化镁、0~10%丙三醇或者乙二醇、余量为水;The waste liquid collection step is to collect the multi-component waste liquid in the production process of high-performance polym-phenylene isophthalamide fiber to the waste liquid storage tank. The waste liquid contains 10-40% dimethylacetamide, 5 ~20% calcium chloride or magnesium chloride, 0~10% glycerol or ethylene glycol, and the balance is water;

中和步骤,通过泵把废液贮罐中的废液输到中和贮罐,废液和中和贮罐内的中和剂中和,中和剂选用氢氧化钙或者氢氧化钠,废液的PH值调到6.8~7.2;In the neutralization step, the waste liquid in the waste liquid storage tank is transported to the neutralization storage tank through the pump, and the waste liquid is neutralized with the neutralizing agent in the neutralization storage tank. The neutralizing agent is calcium hydroxide or sodium hydroxide, and the waste liquid is neutralized. Adjust the pH value of the liquid to 6.8-7.2;

压缩过滤步骤,把中和贮罐中的废液经过压滤机过滤,把其中的悬浮物过滤干净,通过泵输送到中间贮罐;In the compression filtration step, the waste liquid in the neutralization storage tank is filtered through a filter press, and the suspended solids are filtered out, and then pumped to the intermediate storage tank;

萃取步骤,中间贮罐中的废液通过泵输送进第一塔的下部,同时从第一塔的上部按照设定的比例输送萃取剂;萃取剂选用氯仿,从第一塔的上部输送萃取剂的比例为萃取剂:废水中二甲基乙酰胺有效含量=5~10:1,其中,输送萃取剂的较佳比例范围为萃取剂:废水中二甲基乙酰胺有效含量=6~8:1。第一塔里面填充具有高混合效果的填料,废液和萃取剂在第一塔里面进行充分的混合,从塔底出来的萃取相存放在第四贮罐中;In the extraction step, the waste liquid in the intermediate storage tank is pumped into the lower part of the first tower, and at the same time, the extraction agent is delivered from the upper part of the first tower according to the set ratio; the extraction agent is chloroform, and the extraction agent is delivered from the upper part of the first tower The ratio of extraction agent: effective content of dimethylacetamide in wastewater = 5 ~ 10: 1, wherein, the optimal ratio range for transporting extraction agent is extraction agent: effective content of dimethylacetamide in wastewater = 6 ~ 8: 1. The first tower is filled with fillers with high mixing effect, the waste liquid and extractant are fully mixed in the first tower, and the extract phase from the bottom of the tower is stored in the fourth storage tank;

浓缩处理步骤,从第一塔的塔顶出来的液体,输送到蒸发器进行浓缩处理,输出达到纤维生产循环使用的要求第一成品含少量丙三醇的氯化钙;In the concentration treatment step, the liquid coming out from the top of the first tower is transported to the evaporator for concentration treatment, and the output meets the requirements of fiber production and recycling. The first product contains a small amount of calcium chloride of glycerol;

萃取剂脱出步骤,第二塔选用均一直径的常压蒸馏塔,塔釜的温度控制在105~120度,塔顶的温度通过回流控制在60~80度;第四贮罐的混合液通过泵输送进第二塔的上部,在第二塔中进行萃取剂的脱出处理,从第二塔的顶部输出达到循环使用要求的第二成品萃取剂,萃取剂通过冷凝器冷凝后进入第五贮罐,第五贮罐的萃取剂通过泵输送到第一塔的上部,循环使用萃取剂;In the extracting agent extraction step, the second tower is an atmospheric distillation tower with a uniform diameter, the temperature of the tower kettle is controlled at 105-120 degrees, and the temperature at the top of the tower is controlled at 60-80 degrees by reflux; the mixed liquid in the fourth storage tank is passed through the pump It is transported into the upper part of the second tower, and the extraction agent is removed in the second tower, and the second finished product extractant that meets the requirements of recycling is output from the top of the second tower, and the extractant enters the fifth storage tank after being condensed by the condenser , the extractant in the fifth storage tank is transported to the upper part of the first tower by a pump, and the extractant is recycled;

脱水步骤,第三塔选用均一直径的减压蒸馏塔,塔釜的温度控制在115~130度,塔顶的温度控制在60~80度,真空度控制在-0.07Mpa~-0.09Mpa;第二塔的釜底料通过泵输送到第三塔的上部,进行脱水处理;In the dehydration step, the third tower uses a vacuum distillation tower with a uniform diameter, the temperature of the tower kettle is controlled at 115-130 degrees, the temperature of the tower top is controlled at 60-80 degrees, and the vacuum degree is controlled at -0.07Mpa to -0.09Mpa; The bottom material of the second tower is pumped to the upper part of the third tower for dehydration;

精馏步骤,第四塔选用均一直径的减压蒸馏塔,塔釜的温度控制在120~130度,塔顶的温度控制在110~120度,真空度控制在-0.07Mpa~-0.09Mpa;第三塔的釜底液通过泵输送到第四塔的上部,进行精馏处理;In the rectification step, the fourth tower is a vacuum distillation tower with a uniform diameter, the temperature of the tower kettle is controlled at 120-130 degrees, the temperature of the tower top is controlled at 110-120 degrees, and the vacuum degree is controlled at -0.07Mpa to -0.09Mpa; The bottom liquid of the third tower is pumped to the upper part of the fourth tower for rectification treatment;

成品,纯净的、聚合级的酰胺溶剂从第四塔的上部输出,酰胺溶剂通过塔顶的冷凝器冷凝后,收集得到能够重新投入生产循环使用的酰胺溶剂成品,第四塔的釜底重组份通过泵输送到废水贮罐或者焚烧处理。Finished product, pure, polymerization-grade amide solvent is output from the upper part of the fourth tower. After the amide solvent is condensed by the condenser at the top of the tower, the finished product of amide solvent that can be put into production and recycled is collected. The heavy component of the bottom of the fourth tower Pumped to waste water storage tank or incineration.

以下结合实验数据进一步说明本发明。The present invention is further described below in conjunction with experimental data.

废液通过第一塔处理后,其实验数据如表1~3所示。After the waste liquid is treated in the first tower, the experimental data are shown in Tables 1-3.

废液组份为:含二甲基乙酰胺7%和氯化钙10%,实验数据如表1所示。The components of the waste liquid are: containing 7% of dimethylacetamide and 10% of calcium chloride. The experimental data are shown in Table 1.

表1Table 1

废液组份为:含二甲基乙酰胺10%,氯化钙12%和丙三醇2%,实验数据如表2所示。The components of the waste liquid are: containing 10% of dimethylacetamide, 12% of calcium chloride and 2% of glycerol. The experimental data are shown in Table 2.

表2Table 2

废液组份为:含二甲基乙酰胺20%和氯化钙22%,实验数据如表2所示。The components of the waste liquid are: containing 20% of dimethylacetamide and 22% of calcium chloride. The experimental data are shown in Table 2.

表3table 3

从上述数据可以看出,随着萃取剂的比例增加,萃余相的数据向好的方向,但是过高的比例也是不可取的,因为过高的比例会导致后面脱萃取剂的量要增加,能耗也就有所增加,通常萃取剂:废水中二甲基乙酰胺有效含量=5~10:1;更加可取的是萃取剂:废水中二甲基乙酰胺有效含量=6~8:1。It can be seen from the above data that as the proportion of extractant increases, the data of the raffinate phase is in a good direction, but too high a proportion is not advisable, because too high a proportion will lead to an increase in the amount of extractant removed later , the energy consumption will also increase, usually extractant: effective content of dimethylacetamide in waste water = 5 ~ 10: 1; it is more desirable to extractant: effective content of dimethyl acetamide in waste water = 6 ~ 8: 1.

本发明对于混合液的分离处理,把第一塔萃取塔釜出来的混合液分别通过第二塔、第三塔和第四塔处理,其实验数据如表4~6所示。For the separation and treatment of the mixed liquid in the present invention, the mixed liquid from the extraction tower kettle of the first tower is processed through the second tower, the third tower and the fourth tower respectively, and the experimental data are as shown in Tables 4-6.

第二塔second tower 进料量Feed amount 塔釜出料Tower kettle discharge 出料数据Output data 塔顶温度Top temperature 塔釜温度Tower kettle temperature 回流reflow 11 2500kg/h2500kg/h 600kg/h600kg/h DMAC:88.65%,DMAC: 88.65%, 6868 117117 200kg/h200kg/h 22 4500kg/h4500kg/h 1000kg/h1000kg/h DMAC:85.26%,DMAC: 85.26%, 7070 122122 400kg/h400kg/h

表4Table 4

第三塔third tower 塔釜出料Tower kettle discharge 出料数据Output data 塔顶温度Top temperature 塔釜温度Tower kettle temperature 回流reflow 塔真空tower vacuum 11 520kg/h520kg/h 水份150ppmMoisture 150ppm 7474 120120 5050 -0.082mpa-0.082mpa 22 830kg/h830kg/h 水份260ppmMoisture 260ppm 8686 127127 8080 -0.085mpa-0.085mpa

表5table 5

表6Table 6

从第四塔的数据可以看出,本发明得到的产品无色透明,并且水分极低,溶剂的产品质量处于同行的领先水平。由于间位芳纶的合成中,水分的影响很大,所以溶剂的处理质量好坏与芳纶的产品质量密切相关。It can be seen from the data of the fourth tower that the product obtained by the present invention is colorless and transparent, and has extremely low moisture content, and the product quality of the solvent is at the leading level in the industry. Due to the great influence of moisture in the synthesis of meta-aramid fibers, the quality of solvent treatment is closely related to the quality of aramid fibers.

以上内容仅为本发明的较佳实施例,对于本领域的普通技术人员,依据本发明的思想,在具体实施方式及应用范围上均会有改变之处,本说明书内容不应理解为对本发明的限制。The above content is only a preferred embodiment of the present invention. For those of ordinary skill in the art, according to the idea of the present invention, there will be changes in the specific implementation and application scope. limits.

Claims (8)

1. the recovery method organizing part waste liquid in a high-performance aramid fiber production process more, it is characterised in that, comprise the following steps:
Waste collection step, the many groups part waste collection in high-performance polyisophthaloyl metaphenylene diamine fiber production process to waste liquor storage tank;
Neutralization step, is passed to neutralization basin by pump the waste liquid in waste liquor storage tank, waste liquid and the neutralizing agent neutralization neutralized in basin, and the pH value of waste liquid is transferred to 6.8��7.2;
Compression filtration step, filters the waste liquid in neutralization basin through pressure filter, suspended substance wherein is filtered clean, by pump delivery to middle vessel;
Extraction step, waste liquid in middle vessel enters the bottom of the first tower by pump delivery, simultaneously from the top of the first tower according to the ratio conveying extraction agent of setting, the filler with high mixed effect is filled inside first tower, waste liquid and extraction agent mix fully inside the first tower, leave in the 4th basin from extraction phase out at the bottom of tower
Concentration step, from the tower top of the first tower liquid out, is transported to vaporizer and carries out concentration, exports the calcium chloride reaching requirement first finished product that fiber production recycles containing a small amount of glycerol;
Step deviate from by extraction agent, the mixed solution of the 4th basin enters the top of the 2nd tower by pump delivery, what carry out extraction agent in the 2nd tower deviates from process, export from the top of the 2nd tower and reach the 2nd finished product extraction agent recycling requirement, extraction agent is by entering the 5th basin after condenser condenses, the extraction agent of the 5th basin, by the top of pump delivery to the first tower, recycles extraction agent;
Dehydrating step, the bottom material of the 2nd tower, by the top of pump delivery to the 3rd tower, carries out processed;
Rectification step, the kettle base solution of the 3rd tower, by the top of pump delivery to the 4th tower, carries out rectification process;
Finished product, amide solvent pure, polymerization-grade exports from the top of the 4th tower, amide solvent by, after the condenser condenses of tower top, collecting the amide solvent finished product obtaining can again putting into production and recycling, the bottom heavy component of the 4th tower by pump delivery to waste water basin or burning disposal.
2. the recovery method organizing part waste liquid in a kind of high-performance aramid fiber production process according to claim 1 more, it is characterized in that: in described waste collection step, waste liquid includes 10��40% N,N-DIMETHYLACETAMIDEs, 5��20% calcium chloride, 0��10% glycerol, surplus are water, wherein, the content of described glycerol is not 0.
3. the recovery method organizing part waste liquid in a kind of high-performance aramid fiber production process according to claim 1 more, it is characterised in that: in described neutralization step, neutralizing agent selects calcium hydroxide or sodium hydroxide.
4. the recovery method organizing part waste liquid in a kind of high-performance aramid fiber production process according to claim 1 more, it is characterized in that: in described extraction step, chloroform selected by extraction agent, is extraction agent from the ratio of the top of the first tower conveying extraction agent: N,N-DIMETHYLACETAMIDE effective content=5��10:1 waste water.
5. the recovery method organizing part waste liquid in a kind of high-performance aramid fiber production process according to claim 1 more, it is characterized in that: in described extraction step, chloroform selected by extraction agent, is extraction agent from the ratio of the top of the first tower conveying extraction agent: N,N-DIMETHYLACETAMIDE effective content=6��8:1 waste water.
6. the recovery method organizing part waste liquid in a kind of high-performance aramid fiber production process according to claim 1 more, it is characterized in that: described extraction agent is deviate from step, the atmospheric distillation tower of mono-disperse selected by 2nd tower, the temperature of tower reactor controls at 105��120 degree, and the temperature of tower top is controlled at 60��80 degree by backflow.
7. the recovery method organizing part waste liquid in a kind of high-performance aramid fiber production process according to claim 1 more, it is characterized in that: the vacuum still of mono-disperse selected by described 3rd tower, the temperature of tower reactor controls at 115��130 degree, the temperature of tower top controls at 60��80 degree, and vacuum degree control is at-0.07Mpa��-0.09Mpa.
8. the recovery method organizing part waste liquid in a kind of high-performance aramid fiber production process according to claim 1 more, it is characterized in that: the vacuum still of mono-disperse selected by described 4th tower, the temperature of tower reactor controls at 120��130 degree, the temperature of tower top controls at 110��120 degree, and vacuum degree control is at-0.07Mpa��-0.09Mpa.
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CN105646271A (en) * 2015-12-08 2016-06-08 长春工业大学 Method for recovering N,N-dimethyl acetamide from waste liquid generated in cefuroxime acid production through extraction
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CN109134339B (en) * 2018-09-13 2020-05-22 清华大学 Method for recovering solvent for para-aramid fiber production
CN111807593B (en) * 2020-07-23 2023-07-18 河南神马芳纶技术开发有限公司 Salt-containing organic wastewater treatment and utilization integrated device and process for para-aramid solvent working section
CN114436359B (en) * 2020-10-19 2023-05-02 中国石油化工股份有限公司 Method for extracting and recovering N, N-dimethylacetamide in wastewater
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