WO2019033806A1 - 活性染料染色残液回收系统及回收方法 - Google Patents

活性染料染色残液回收系统及回收方法 Download PDF

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WO2019033806A1
WO2019033806A1 PCT/CN2018/087413 CN2018087413W WO2019033806A1 WO 2019033806 A1 WO2019033806 A1 WO 2019033806A1 CN 2018087413 W CN2018087413 W CN 2018087413W WO 2019033806 A1 WO2019033806 A1 WO 2019033806A1
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extraction
reactive dye
organic solvent
stripping
extractant
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PCT/CN2018/087413
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English (en)
French (fr)
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韦节彬
李世琪
刘奎东
张佐平
李华
陈超
张庆娟
禹辉
陈仰孚
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新疆如意纺织服装有限公司
新疆鲁意纺织科技有限公司
新疆神邦环境工程有限公司
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Publication of WO2019033806A1 publication Critical patent/WO2019033806A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/26—Treatment of water, waste water, or sewage by extraction
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/308—Dyes; Colorants; Fluorescent agents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry

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  • the invention relates to the field of textile printing and dyeing, in particular to the treatment and recycling of textile printing and dyeing wastewater.
  • the annual discharge of printing and dyeing wastewater in China is 2 billion tons, of which active dyeing wastewater accounts for about 20%, and the total amount is about 400 million tons.
  • the reactive dye is dyed with a large amount of hydrolyzed dye, in order to obtain good washing fastness, the hydrolyzed dye should be thoroughly washed out. For this reason, the parent structure of the reactive dye is designed to have a lower affinity for the fiber while being active. In the dyeing process, it is necessary to add 1-10% salt to promote dyeing, so as to increase the dye uptake rate. For some deep color, the dosage is up to 1 ton of salt per ton of fiber. These salts have no loss in dyeing, and directly stained from sewage. All of them are discharged. Many factories have more than tens of tons of salt per day. The annual average amount of salt used in the country is 1 million tons. This kind of discharge for many years has caused serious damage to the ecology of the surrounding soil and rivers.
  • the invention realizes the continuous decolorization of the reactive dyeing residue and the reuse of the reclaimed brine under the premise of changing the existing production mode, equipment, experience and operation method as little as possible.
  • the present invention provides a reactive dye staining residue recovery system and a recovery method.
  • a reactive dye staining residue recovery system comprising an extraction system and a stripping system; the extracting system extracts the reactive dye in the residual liquid into an organic solvent, and the extracted residual liquid is used for dyeing; and the The extraction system strips the reactive dye in the organic solvent extracted with the reactive dye from the extraction system into an aqueous solution, and the stripped organic solvent is returned to the extraction system as an extracting agent; wherein the extraction system and the stripping system are both For tubular membrane extraction.
  • the extractant in the extraction system is a mixture of trioctylamine, n-octanol and diesel in a volume ratio of 1-2:1-2:3-5.
  • the aqueous phase extractant in the stripping system is an alkaline solution having a pH of 10-11.
  • a method for recovering a reactive dyeing residue comprising the steps of: S1, extracting a residual liquid, extracting the hydrolyzed reactive dye in the residual liquid into an organic solvent, and extracting the salt-containing aqueous solution for dyeing again; S2, passing Stripping extracts the reactive dye from the organic solvent extracted with the reactive dye to the aqueous phase; and S3, and reuses the organic solvent as the extractant by stripping; wherein the extraction system and the stripping system are both tubular membrane extraction .
  • step S1 Also included before the step S1 is a pretreatment step of adjusting the pH of the dye residue to 2-3 with acid.
  • the acid is at least one of sulfuric acid, formic acid, and acetic acid.
  • the extracted extractant is a mixture of trioctylamine, n-octanol and diesel in a volume ratio of 1-2:1-2:3-5.
  • the stripped aqueous phase extractant is an alkaline solution having a pH of 10-11.
  • the invention adopts a reactive dye dyeing residual liquid recycling system with a tubular membrane extraction decoloring device as the core, realizes the recycling of salt and water in the dyeing residual liquid at low cost, and removes more than 95% of hydrolyzed dyes and the like, and uses the same.
  • the extractant can be recycled and recycled, and realizes industrial application.
  • the regenerated bleaching reactive dye dyeing process technology has been developed to solve the problem of high chroma and high salinity wastewater treatment of reactive dyeing, and the dye residue is realized.
  • the resource utilization of water and water has broken through the ecological and environmental constraints of the existing reactive dye dyeing production methods.
  • Figure 1 is a schematic diagram of a reactive dyeing residue recovery system of the present invention
  • Figure 2 is a schematic illustration of a recovery system utilizing a tubular membrane of the present invention
  • Figure 3 is a schematic illustration of a reactive dye staining residue recovery system of the present invention.
  • 1,11-storage tank 1,12-pressurized pump; 3,13-pressure gauge; 4,14-membrane assembly; 5,15-pressure gauge; 6,16-backpressure valve; 7,17-safety valve .
  • the reactive dye staining residue recovery system of the present invention comprises an extraction system and a stripping system.
  • the extraction system extracts the reactive dye in the raffinate into an organic solvent, and the extracted residue is used for dyeing.
  • the stripping system strips the reactive dye in the organic solvent extracted with the reactive dye from the extraction system into the aqueous solution, and the stripped organic solvent is returned to the extraction system as an extractant.
  • the method for recovering the reactive dyeing residue of the present invention comprises the following steps: S1, extracting the residual liquid, extracting the reactive dye in the residual liquid into an organic solvent, and extracting the salt-containing aqueous solution for dyeing again; S2, by stripping The reactive dye in the organic solvent extracted with the reactive dye is extracted to the aqueous phase; and S3, the organic solvent after the stripping is reused as an extractant.
  • a pretreatment step is also included prior to the S1 step, which is to adjust the pH of the raffinate to 2-3 with an acid.
  • the acid-removing treatment of the residual liquid is for the purpose of extracting the dye from the residual liquid by converting the extracting agent from a non-ionic state to a cation during the extraction process to complex the anion formed by hydrolysis of the reactive dye in the residual liquid.
  • the acid to be used may be an inorganic acid or an organic acid.
  • the inorganic acid may be sulfuric acid or the like
  • the organic acid may be formic acid, acetic acid or the like.
  • the extractant of the extraction system When extracting the extractant of the extraction system, it is generally required that the extractant is not miscible with the residual liquid, the solubility of the reactive dye is much larger than that of the reactive dye in the residual liquid, or is not easy to volatilize and the residual liquid cannot react.
  • a nonvolatile organic solvent is usually used as an extractant, and an appropriate organic solvent should be selected according to the kind of the reactive dye.
  • a complexing agent, a cosolvent, and a diluent may be included in the extractant of the present invention.
  • the complexing agent in the extractant is converted from a non-ionic state to a cation under acidic conditions, and the anion formed by the hydrolysis of the reactive dye in the complex liquid is used to achieve the purpose of extracting the dye from the residual liquid.
  • the co-solvent is a good solvent for the selected complexing agent and complexing product to facilitate the formation and phase transfer of the complex.
  • the diluent is used to improve the viscosity, surface tension, etc. of the mixed extractant, and to improve the extraction ability.
  • One skilled in the art can select a suitable co-solvent and diluent as needed based on the selected complexing agent.
  • a reactive dye is a water-soluble dye with a reactive group, which can be covalently bonded to a hydroxyl group on a cellulose fiber, an amino group on a protein fiber, an amino group on a polyamide fiber, and a carboxy hydroxyl group.
  • Reactive dyes are distinguished by different reactive groups. There are mainly nine types, namely, dichlorotriazine type, monochlorotriazine type, vinyl sulfone type, monochlorotriazine and vinyl sulfone double active group, and double chlorinated three.
  • the complexing agent in the extractant is selected from organic solvents capable of forming cations under acidic conditions, such as tertiary amines or mixtures thereof, which may be mixed in different ratios.
  • a mixed extractant R 3 N containing a polyamine is formed. The following is an example of the use of sulfuric acid in the acid treatment to illustrate the extraction process of the hydrolysis dye in the extraction residue by the extractant containing the polyamine:
  • the polyamine is converted from a nonionic state to a cation under acidic conditions.
  • the extractant may be, but is not limited to, a mixture of trioctylamine, n-octanol and diesel in a volume ratio of 1-2:1-2:3-5.
  • One skilled in the art can suitably select other suitable extractants in accordance with the teachings of the present invention.
  • the stripping system is the stripping of the dye extracted into the organic solvent into the aqueous phase.
  • the aqueous phase extracting agent may be an alkaline aqueous solution to which a pH of 10 to 11 is added, and the alkaline aqueous solution may be an aqueous sodium hydroxide solution.
  • the complex formed in the oil phase removes H + under alkaline conditions, and the extractant returns to a non-ionic state, separating the hydrolyzed dye from the oil phase, and then entering the aqueous phase to dissolve, completing the back extraction.
  • the stripping process is as shown in equation (3):
  • the stripped organic solvent is returned to the extraction system as an extractant.
  • Both extraction and stripping can be performed by tubular membrane extraction.
  • the membrane module of the tubular membrane mainly functions as a filtration separation.
  • the film may be an oleophobic material such as PDVF or ceramic.
  • Figure 1 is a schematic diagram of a reactive dye staining residue recovery system.
  • the dyeing machine removes the residual liquid, collects and adjusts the residual liquid, and then supplies the collected residual liquid to the tubular membrane extraction device for extraction.
  • the extracted residual liquid is a saline solution, which can be returned to the dyeing machine for reuse; then the extraction dye is used.
  • the organic solvent is stripped, the dye therein is stripped to the aqueous phase, and the stripped organic solvent is supplied to the tubular membrane extraction apparatus as an extractant for reuse.
  • FIG. 2 is a schematic illustration of a recovery system utilizing a tubular membrane.
  • a mixture of the reactive dye dye residue and the organic solution as the extractant adjusted in advance (the pH of the residual liquid is adjusted to 2-3) is stored in the storage tank 1, and the extractant extracts the residue. dye.
  • the mixed liquid is sent to the tubular membrane module 4 by the pressurizing pump 2 to be separated, and when the pressure exceeds a certain pressure, the safety valve 7 automatically opens the mixed liquid and returns to the storage tank 1. After separation of the tubular membrane module 4, the aqueous phase and the oil phase are separated.
  • the aqueous phase separated by the tubular membrane module 4 is the residual liquid after the extraction, and is a salt-containing aqueous solution, that is, decolorized saline. After the decolorized brine has flowed out of the tubular membrane module 4, the decolorized brine can be treated, first adjusted to neutrality, and then adjusted to the desired brine concentration for reuse for dyeing.
  • the oil phase separated by the tubular membrane module 4, that is, the organic solvent extracted with the dye, is returned to the storage tank 1.
  • the storage tank 1 mixture in the extraction system (primarily the oil phase also contains a small amount of aqueous phase) is supplied to the storage tank 11 of the stripping system for back extraction.
  • the aqueous phase extractant used for the stripping is an aqueous solution of sodium hydroxide having a pH of 10-11.
  • the organic solvent extracted with the dye in the storage tank 11 is extracted, and the dye enters the aqueous phase.
  • the mixed liquid is sent to the tubular membrane module 14 by the pressurizing pump 12 to be separated, and the safety valve 17 automatically opens the mixed liquid back to the storage tank 11 when the pressure exceeds a certain pressure.
  • the aqueous phase and the oil phase are separated, and the aqueous solution extracted with the dye is discharged from the tubular membrane module 14 and then treated.
  • the oil phase separated by the tubular membrane module 14 is an organic solvent from which the dye is extracted.
  • the organic solvent discharged from the tubular membrane module 14 can be returned to the storage tank 11 for further stripping process until the dye content in the organic solvent reaches a predetermined level, and the organic solvent can be recovered and used as an extraction system for extraction.
  • the agent realizes the recycling of the extractant.
  • the extraction system and the stripping system also include pressure gauges 3, 5, 13, 15 and back pressure valves 6, 16 for detecting and controlling the flow.
  • the extraction system and the stripping system in Fig. 2 are exemplified by providing a tubular membrane module, but the invention is not limited to a tubular membrane, and those skilled in the art can provide a plurality of tubular membranes in series according to actual needs.
  • the tubular membrane extraction and separation technology used in the invention is a polar organic chemical extraction and separation method based on reversible reaction, and a closed loop of water, salt and extractant is formed in the process of dyeing the residual liquid.
  • the interaction in the tubular membrane extraction device continuously extracts the hydrolyzed dye in the dye residue, thereby allowing the high salinity residue to be recycled, thereby avoiding a large amount of salt discharge. It not only reduces environmental pollution, but also reduces production costs. At the same time, more than 95% of the hydrolyzed dyes and other contaminants are removed, the extractant used can be recycled and reused, and industrial application is realized.
  • the regeneration dyeing process of reactive dyes is developed to solve the high chroma and high dyeing of reactive dyes.
  • the problem of salinity wastewater treatment has realized the resource utilization of dye residue liquid and water, which has broken through the ecological and environmental constraints of the existing reactive dye dyeing production methods.

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Abstract

一种活性染料染色残液回收系统，包括萃取系统和反萃系统；萃取系统将残液中的活性染料萃取至有机溶剂中，经过萃取后的残液用于染色；以及反萃系统将萃取系统中萃取有活性染料的有机溶剂中的活性染料反萃至水溶液中，经过反萃后的有机溶剂回至萃取系统作为萃取剂；其中萃取系统和反萃系统均为管式膜萃取。还公开一种活性染料染色残液的回收方法。

Description

活性染料染色残液回收系统及回收方法 技术领域
本发明涉及纺织印染领域，具体涉及纺织印染废水处理及回收。
背景技术
我国年排放印染废水量为20亿吨，其中活性染色废水占20％左右，总量约4亿吨。
由于活性染料染色过程中伴有大量的水解染料生成，为获得良好的水洗牢度，要彻底洗除水解染料，为此，活性染料的母体结构设计成为对纤维具有较低的亲和力，同时在活性染色过程中必需加入1-10％的盐促染，以提高染料的上染率，对有些深浓颜色用量多达1吨盐/吨纤维，这些盐在染色中无损耗，染色后直接从污水中全部排出，很多工厂日排盐量超过数十吨，全国年排放量化用盐量100万吨，长年累月的这样排放，给周围的土壤、河流的生态造成严重危害。
本发明尽可能的少改变现有生产方式、设备、经验、操作方法的前提下，实现活性染料染色残液连续脱色与再生盐水回用。
发明内容
为了克服上述缺陷，本发明提供一种活性染料染色残液回收系统及回收方法。
提供一种活性染料染色残液回收系统，包括萃取系统和反萃系统；所述萃取系统将残液中的活性染料萃取至有机溶剂中，经过萃取后的残液用于染色；以及所述反萃系统将所述萃取系统中萃取有活性染料的有机溶剂中的活性染料反萃至水溶液中，经过反萃后的有机溶剂回至萃取系统作为萃取剂；其中所述萃取系统和反萃系统均为管式膜萃取。
所述萃取系统中的萃取剂是按体积比为1-2:1-2:3-5的三辛胺、正辛醇和柴油的混合物。
所述反萃系统中的水相萃取剂是pH为10-11的碱性溶液。
还提供一种活性染料染色残液回收方法，包括如下步骤：S1，萃取残液，将残液中的水解活性染料萃取至有机溶剂中，萃取后含盐的水溶液再次用于染色；S2，通过反萃将萃取有活性染料的有机溶剂中活性染料萃取至水相；以及S3，将通过反萃后的有机溶剂作为萃取剂再利用；其中所述萃取系统和反萃系统均为管式膜萃取。
在所述S1步骤之前还包括预处理步骤，所述预处理步骤是用酸将染色残液的pH调整到2-3。
所述酸为硫酸、甲酸、乙酸中的至少一种。
所述萃取的萃取剂是按体积比为1-2:1-2:3-5的三辛胺、正辛醇和柴油的混合物。
所述反萃的水相萃取剂是pH为10-11的碱性溶液。
本发明以管式膜萃取脱色装置为核心的活性染料染色残液回用系统，低成本地实现了 染色残液中盐和水的循环使用，同时去除95％以上的水解染料等污染物，所用的萃取剂能够再生循环利用，并实现了产业化应用；开发了再生盐水回用活性染料染色工艺技术，解决了活性染料染色的高色度、高盐度废水处理难题，实现了染色残液盐和水的资源化利用，突破了现有活性染料染色生产方式的生态与环境制约。
附图说明
通过参照附图详细描述其示例实施方式，本发明的上述和其它特征及优点将变得更加明显。
图1是本发明的活性染料染色残液回收系统示意图；
图2是本发明的利用管式膜的回收系统的示意图；以及
图3是本发明的活性染料染色残液回收系统示意图。
其中，附图标记说明如下：
1,11-存储罐；2,12-加压泵；3,13-压力表；4,14-膜组件；5,15-压力表；6,16-背压阀；7,17-安全阀。
具体实施方式
下面结合具体实施方式对本发明作详细说明。
本发明的活性染料染色残液回收系统，包括萃取系统和反萃系统。萃取系统将残液中的活性染料萃取至有机溶剂中，经过萃取后的残液用于染色。反萃系统将萃取系统中萃取有活性染料的有机溶剂中的活性染料反萃至水溶液中，经过反萃后的有机溶剂回至萃取系统作为萃取剂。
本发明的活性染料染色残液回收方法，包括如下步骤：S1，萃取残液，将残液中的活性染料萃取至有机溶剂中，萃取后含盐的水溶液再次用于染色；S2，通过反萃将萃取有活性染料的有机溶剂中活性染料萃取至水相；以及S3，将通过反萃后的有机溶剂作为萃取剂再利用。
在S1步骤之前还包括预处理步骤，预处理步骤是用酸调整残液的pH值为2-3。对残液调酸处理是为了在萃取过程中，将萃取剂由非离子状态转变为阳离子，以络合残液中活性染料水解形成的阴离子实现从残液中萃取染料的目的。所用的酸可以是无机酸，也可以是有机酸，例如无机酸可以是硫酸等，有机酸可以是甲酸、乙酸等。在选取萃取系统的萃取剂时，一般要求萃取剂不能与残液互溶、对活性染料的溶解度远大于活性染料在残液中的溶解度、要不易于挥发并且不能残液发生反应。考虑以上因素，通常采用不易挥发的有机溶剂作为萃取剂，同时应当根据活性染料的种类选择适当的有机溶剂。本发明中萃取剂中可以包括络合剂、助溶剂和稀释剂。萃取过程中萃取剂中的络合剂在酸性条件下由非离子状态转变为阳离子，以络合残液中活性染料水解形成的阴离子实现从残液中萃取染料的目的。助溶剂是所选络合剂和络合产物的良溶剂，以利于络合物的形成与相转移。稀释剂 用于改善混合萃取剂的黏度、表面张力等，提高萃取能力的作用。本领域技术人员可以根据所选络合剂按需要选择合适的助溶剂和稀释剂。活性染料是一种带有活性基团的水溶性染料，能与纤维素纤维上的羟基、蛋白质纤维上的氨基、聚酰胺纤维上的氨基和羧羟基发生共价键结合，故又称为反应性染料。活性染料以不同反应基来区分，主要有九种类型，即二氯三嗪型、一氯均三嗪型、乙烯砜型、一氯均三嗪与乙烯砜双活性基、双一氯均三嗪A型、双一氯均三嗪B型、膦酸其型、二氟一氯嘧啶型和吡啶羧酸三嗪基型。由于不同类型的活性染料在水解后都是带负电性的，因此萃取剂中的络合剂选用在酸性条件下能形成阳离子的有机溶剂，例如叔胺类或其混合物，可以是不同的比例混合形成含有多元胺的混合萃取剂R 3N。以下以调酸处理时采用硫酸为例，说明包含多元胺的萃取剂对萃取残液中水解染料的萃取过程：
如式(1)所示，多元胺在酸性条件下由非离子状态转变为阳离子。
Figure PCTCN2018087413-appb-000001
如式(2)所示，阳离子与水解的染料R ’SO 3络合。
Figure PCTCN2018087413-appb-000002
从而实现染料从残液中萃取到萃取剂中目的。
萃取剂可以是，但不限于，按体积比为1-2:1-2:3-5的三辛胺、正辛醇和柴油的混合物。本领域技术人员可以根据本发明的构思适当选择其他适合的萃取剂。
反萃剂系统是将萃取到有机溶剂中的染料反萃到水相中。水相萃取剂可以是加入pH值为10-11的碱性水溶液，碱性水溶液可以是氢氧化钠水溶液。经过萃取过程后，油相中形成的络合物在碱条件下去除H +，萃取剂回复为非离子状态，使水解染料与油相分离，进入水相溶解，完成反萃取。反萃取过程如式(3)：
Figure PCTCN2018087413-appb-000003
经过反萃后的有机溶剂回至萃取系统作为萃取剂。
萃取和反萃均可以采用管式膜萃取。管式膜的膜组件主要起过滤分离作用。膜可以是PDVF或陶瓷等疏油类材料。
图1是活性染料染色残液回收系统示意图。染色机排除残液，对残液进入收集调酸，然后将收集的残液供给管式膜萃取装置进行萃取，萃取后的残液为含盐水溶液，可以返回染色机再次利用；然后将萃取染料的有机溶剂进行反萃，将其中的染料反萃至水相，被反萃的有机溶剂提供给管式膜萃取装置作为萃取剂再次利用。
图2是利用管式膜的回收系统示意图。在萃取系统中，将预先调整酸度(调整残液的pH为2-3)的活性染料染色残液和作为萃取剂的有机溶液的混合液存储于存储罐1中，萃取剂萃取残液中的染料。然后，通过加压泵2将混合液送入管式膜组件4进行分离，被当压力超过一定的压力后安全阀7自动打开混合液回到存储罐1中。经过管式膜组件4的分离，水相和油相分离。被管式膜组件4分离的水相为萃取后的残液，为含盐的水溶液即脱色盐水。脱色盐水从管式膜组件4中流出后，可以对脱色盐水进行处理，先调pH到中性， 再调至预期的盐水浓度，以再次用于染色。被管式膜组件4分离的油相，即萃取有染料的有机溶剂回复到存储罐1中。萃取系统中存储罐1混合物(主要是油相还包含少量的水相)供给反萃系统的存储罐11，以进行反萃取。用于反萃的水相萃取剂为氢氧化钠水溶液，pH值为10-11。在存储罐11中萃取有染料的有机溶剂被萃取，染料进入水相。然后，通过加压泵12将混合液送入管式膜组件14进行分离，被当压力超过一定的压力后安全阀17自动打开混合液回到存储罐11中。经过管式膜组件14的分离，水相和油相分离，萃取有染料的水溶液从管式膜组件14中排出，然后进行处理。被管式膜组件14分离的油相是染料被萃取出去的有机溶剂。从管式膜组件14排出的有机溶剂可以重新回到存储罐11，进行进一步的反萃过程，直到有机溶剂中的染料含量达到预定含量之下后，可以回收有机溶剂再用作萃取系统的萃取剂，实现萃取剂的循环利用。萃取系统和反萃系统还包括用于检测和控制液流的压力表3,5,13,15和背压阀6,16。
图2中的萃取系统和反萃系统以设置一个管式膜组件为例，但本发明并不限定为一个管式膜，本领域技术人员可以根据实际需要设置多个串联的管式膜。
实施例1
如图3所示，在散棉染色车间各个染色机(例如1#-10#染色机)的进出水口排出专用回收和投料管道，使各染缸的活性染色残液能够直接排放到特定的收集池M中，经G1、G2调酸后，进入回收系统中后，经过在萃取剂的作用下使染色残液脱色，经过管式膜组件的分离得到的盐水经G3和G4进行盐水浓度调节后转入N盐水收集池，与此同时萃取剂完成络合萃取后进入萃取循环系统进行萃取剂的反萃取，使水解染料与有机相分离，有机相进入下次的循环使用。
本发明所采用的管式膜萃取分离技术是一种基于可逆反应的极性有机物化学萃取分离方法，在对染色残液的处理过程中形成了水+盐和萃取剂两个体系的闭环循环，在管式膜萃取装置中相互作用，连续性地将染色残液中的水解染料提取出来，从而使含高盐度的残液得以循环使用，避免了盐的大量排放。既减少了对环境的污染，又降低了生产成本。同时去除95％以上的水解染料等污染物，所用的萃取剂能够再生循环利用，并实现了产业化应用；开发了再生盐水回收活性染料染色工艺技术，解决了活性染料染色的高色度、高盐度废水处理难题，实现了染色残液盐和水的资源化利用，突破了现有活性染料染色生产方式的生态与环境制约。
当然，本发明还可有其它多种实施例，在不背离本发明精神及其实质的情况下，熟悉本领域的技术人员当可根据本发明作出各种相应的改变和变形，但这些相应的改变和变形都应属于本发明所附的权利要求的保护范围。

Claims (8)

  1. 一种活性染料染色残液回收系统，包括萃取系统和反萃系统；
    所述萃取系统将残液中的活性染料萃取至有机溶剂中，经过萃取后的残液用于染色；以及所述反萃系统将所述萃取系统中萃取有活性染料的有机溶剂中的活性染料反萃至水溶液中，经过反萃后的有机溶剂回至萃取系统作为萃取剂；其中所述萃取系统和反萃系统均为管式膜萃取。
  2. 根据权利要求1所述的活性染料染色残液回收系统，其特征在于，所述萃取系统中的萃取剂是按体积比为1-2:1-2:3-5的三辛胺、正辛醇和柴油的混合物。
  3. 根据权利要求1所述的活性染料染色残液回收系统，其特征在于，所述反萃系统中的水相萃取剂是pH为10-11的碱性溶液。
  4. 一种活性染料染色残液回收方法，包括如下步骤：
    S1，萃取残液，将残液中的水解活性染料萃取至有机溶剂中，萃取后含盐的水溶液再次用于染色；
    S2，通过反萃将萃取有活性染料的有机溶剂中活性染料萃取至水相；以及
    S3，将通过反萃后的有机溶剂作为萃取剂再利用；
    其中所述萃取系统和反萃系统均为管式膜萃取。
  5. 根据权利要求4所述的回收方法，其特征在于，在所述S1步骤之前还包括预处理步骤，所述预处理步骤是用酸将染色残液的pH调整到2-3。
  6. 根据权利要求4所述的回收方法，其特征在于，所述酸为硫酸、甲酸、乙酸中的至少一种。
  7. 根据权利要求4所述的回收方法，其特征在于，所述萃取的萃取剂是按体积比为1-2:1-2:3-5的三辛胺、正辛醇和柴油的混合物。
  8. 根据权利要求4所述的回收方法，其特征在于，所述反萃的水相萃取剂是pH为10-11的碱性溶液。
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