CN110508231B - Continuous production system of azo reactive dyes using hypergravity - Google Patents

Continuous production system of azo reactive dyes using hypergravity Download PDF

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CN110508231B
CN110508231B CN201910711393.XA CN201910711393A CN110508231B CN 110508231 B CN110508231 B CN 110508231B CN 201910711393 A CN201910711393 A CN 201910711393A CN 110508231 B CN110508231 B CN 110508231B
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reactor
reaction
spiral coil
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coil reactor
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CN110508231A (en
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邹海魁
肖振根
陈建峰
初广文
孙宝昌
罗勇
张亮亮
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BEIJING ZHONGCHAO HAIQI TECHNOLOGY CO LTD
Beijing University of Chemical Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00Other mixers; Mixing plants; Combinations of mixers
    • B01F33/80Mixing plants; Combinations of mixers
    • B01F33/82Combinations of dissimilar mixers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • B01J19/0013Controlling the temperature of the process
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/10Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24Stationary reactors without moving elements inside
    • B01J19/2415Tubular reactors
    • B01J19/243Tubular reactors spirally, concentrically or zigzag wound
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B62/00Reactive dyes, i.e. dyes which form covalent bonds with the substrates or which polymerise with themselves
    • C09B62/44Reactive dyes, i.e. dyes which form covalent bonds with the substrates or which polymerise with themselves with the reactive group not directly attached to a heterocyclic ring
    • C09B62/503Reactive dyes, i.e. dyes which form covalent bonds with the substrates or which polymerise with themselves with the reactive group not directly attached to a heterocyclic ring the reactive group being an esterified or non-esterified hydroxyalkyl sulfonyl or mercaptoalkyl sulfonyl group, a quaternised or non-quaternised aminoalkyl sulfonyl group, a heterylmercapto alkyl sulfonyl group, a vinyl sulfonyl or a substituted vinyl sulfonyl group, or a thiophene-dioxide group
    • C09B62/507Azo dyes
    • C09B62/51Monoazo dyes

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Abstract

本发明提供应用超重力的偶氮活性染料的连续化生产系统,将螺旋盘管反应器与超重力技术结合,对于重氮化反应和偶合反应区分对待,重氮化反应在螺旋盘管反应器中进行,超重力反应器用于偶合反应能够很大程度上提高转化率以及产品的质量。而螺旋盘管反应器能够精确控温,避免重氮盐的分解,这样配合下,由于温度控制精确,重氮盐分解极少,不会影响后续的偶合反应的进行,因此能够保证连续生产时重氮盐的浓度维持在较高的范围,从而能够保证同一批次的偶氮活性染料性能接近或相同,适应工业的实际需求。进一步的,在螺旋盘管内设置扰动件,可以扰动所述螺旋盘管反应器中的反应溶液,加快反应溶液的流动和混合,有利于均一化反应。

Figure 201910711393

The invention provides a continuous production system for azo reactive dyes using supergravity, combines a spiral coil reactor with a supergravity technology, and treats the diazotization reaction and the coupling reaction separately. The diazotization reaction is carried out in the spiral coil reactor. For the coupling reaction, the supergravity reactor can greatly improve the conversion rate and the quality of the product. The spiral coil reactor can precisely control the temperature to avoid the decomposition of the diazonium salt. In this way, due to the precise temperature control, the decomposition of the diazonium salt is very small, which will not affect the subsequent coupling reaction, so it can ensure continuous production. The concentration of the diazonium salt is maintained in a high range, so as to ensure that the properties of the azo reactive dyes in the same batch are close to or the same, and meet the actual needs of the industry. Further, a disturbance member is arranged in the spiral coil tube, which can disturb the reaction solution in the spiral coil tube reactor, accelerate the flow and mixing of the reaction solution, and facilitate the homogenization reaction.

Figure 201910711393

Description

应用超重力的偶氮活性染料的连续化生产系统Continuous production system of azo reactive dyes using hypergravity

技术领域technical field

本发明涉及偶氮活性染料制备技术领域。更具体地,涉及一种应用超重力的偶氮活性染料的连续化生产系统。The invention relates to the technical field of preparation of azo reactive dyes. More specifically, it relates to a continuous production system of azo reactive dyes using supergravity.

背景技术Background technique

在工业上,活性偶氮染料的生产是在搅拌釜反应器中以间歇操作方式进行的。由于有机反应的复杂性,以及搅拌釜反应器体积太大,导致物料的温度和混合效果在局部区域难以达到均匀,染料的生产效率低下,而且间歇搅拌釜生产的染料各批次间差别较大,对染料的后处理以及染料的应用都带来了不便。Industrially, the production of reactive azo dyes is carried out in batch operation in stirred tank reactors. Due to the complexity of the organic reaction and the large volume of the stirred tank reactor, the temperature and mixing effect of the materials are difficult to achieve uniformity in local areas, the production efficiency of dyes is low, and the batches of dyes produced in intermittent stirred tanks are quite different. , which brings inconvenience to the post-processing of the dye and the application of the dye.

因此,亟需提供一种应用超重力的偶氮活性染料的连续化生产系统。Therefore, there is an urgent need to provide a continuous production system for azo reactive dyes using supergravity.

发明内容SUMMARY OF THE INVENTION

有鉴于此,为了解决目前缺少有效的偶氮活性染料的连续化生产系统,本发明提供一种应用超重力的偶氮活性染料的连续化生产系统。In view of this, in order to solve the current lack of an effective continuous production system for azo reactive dyes, the present invention provides a continuous production system for azo reactive dyes using supergravity.

在某些实施例中,一种应用超重力的偶氮活性染料的连续化生产系统,所述系统包括:In certain embodiments, a continuous production system of azo reactive dyes using supergravity, the system comprises:

缩合反应单元,所述缩合反应单元包括缩合反应罐,用于生成偶合组分;a condensation reaction unit comprising a condensation reaction tank for generating coupling components;

重氮化反应单元,所述重氮化反应单元包括:A diazotization reaction unit, the diazotization reaction unit includes:

预混组件,对重氮组分和重氮试剂进行预混,和A premix kit for premixing the diazo component and diazo reagent, and

螺旋盘管反应器,与所述预混组件连通,以使预混后的反应溶液在所述螺旋盘管反应器内进行重氮化反应产生重氮盐;a helical coil reactor, communicated with the premixing component, so that the premixed reaction solution is subjected to diazotization reaction in the helical coil reactor to generate diazonium salt;

所述系统进一步包括:The system further includes:

与所述重氮化反应单元和所述缩合反应单元相连通的超重力偶合反应单元,所述超重力偶合反应单元用于在超重力环境下使重氮盐与偶合组分进行偶合反应产生所述偶氮活性染料;The hypergravity coupling reaction unit communicated with the diazotization reaction unit and the condensation reaction unit, and the hypergravity coupling reaction unit is used to carry out the coupling reaction of the diazonium salt and the coupling component under the hypergravity environment to produce the said azo reactive dyes;

其中,所述螺旋盘管反应器发生重氮化反应的内腔中设置有固定结构的扰动件,所述扰动件用于扰动所述螺旋盘管反应器中的反应溶液。Wherein, a disturbance member with a fixed structure is arranged in the inner cavity of the helical coil reactor where the diazotization reaction occurs, and the disturbance member is used to disturb the reaction solution in the helical coil reactor.

在某些实施例中,所述扰动件包括固定在所述螺旋盘管反应器内腔表面上的固定部,以及与所述固定部远离所述螺旋盘管反应器内腔表面的一端结合固定的自由部,所述自由部包括两个,两个所述自由部与所述固定部构成“Y”型结构或者“T”型结构。In some embodiments, the perturbation member includes a fixing part fixed on the inner cavity surface of the helical coil reactor, and is fixed in combination with an end of the fixing part away from the inner cavity surface of the helical coil reactor The free part includes two free parts, and the two free parts and the fixed part form a "Y"-shaped structure or a "T"-shaped structure.

在某些实施例中,所述扰动件与所述螺旋盘管反应器内腔表面垂直设置,或者倾斜设置。In some embodiments, the perturbation member is arranged perpendicular to the inner cavity surface of the helical coil reactor, or is arranged obliquely.

在某些实施例中,所述扰动件包括沿进液方向缩径的第一部分,以及与所述第一部分的内径较小的一端连通的第二部分,所述第二部分沿进液方向呈扩径结构,并且所述第一部分和所述第二部分以其连接面为对称平面对称设置。In some embodiments, the disturbing member includes a first portion with a diameter reduced along the liquid feeding direction, and a second portion communicating with an end of the first portion with a smaller inner diameter, the second portion extending along the liquid feeding direction The diameter-expanding structure is provided, and the first part and the second part are symmetrically arranged with their connecting surfaces as the symmetry plane.

在某些实施例中,所述系统进一步包括:In certain embodiments, the system further includes:

超声馈入器,用于分别向所述螺旋盘管反应器以及所述超重力偶合反应单元馈入超声,其中向所述螺旋盘管反应器和所述超重力偶合反应单元馈入的超声强度相同或不同。An ultrasonic feeder is used to feed ultrasonic waves to the helical coil reactor and the supergravity coupling reaction unit respectively, wherein the intensity of the ultrasonic waves fed into the helical coil reactor and the supergravity coupling reaction unit same or different.

在某些实施例中,所述预混组件包括第一输液管和第二输液管;In certain embodiments, the premix assembly includes a first infusion tube and a second infusion tube;

所述第一输液管套设于所述第二输液管的外侧,并且所述第一输液管和所述第二输液管之间具有空隙以供重氮组分和重氮试剂的其中一个流通,所述第二输液管内的空腔供重氮组分和重氮试剂的其中另一个流通;The first infusion tube is sleeved on the outside of the second infusion tube, and there is a gap between the first infusion tube and the second infusion tube for one of the diazonium components and the diazonium reagent to circulate , the cavity in the second infusion tube is for circulation of the other of the diazo component and the diazo reagent;

所述第一输液管靠近所述螺旋盘管反应器的一端形成供重氮组分和重氮试剂混合的预混区,所述第二输液管延伸至所述预混区的入口处,并向所述预混区喷射所述重氮组分和重氮试剂的其中另一个。The first infusion pipe is close to one end of the helical coil reactor to form a premixed area for mixing the diazo component and the diazonium reagent, and the second infusion pipe extends to the inlet of the premixed area, and The other of the diazo component and the diazo reagent is sprayed into the premix zone.

在某些实施例中,所述预混区包括临近其入口处的缩径部和与所述缩径部一体连通的平直部。In certain embodiments, the premixing zone includes a reduced diameter portion adjacent to its inlet and a straight portion in integral communication with the reduced diameter portion.

在某些实施例中,所述超重力偶合反应单元包括:In certain embodiments, the hypergravity coupling reaction unit comprises:

超重力反应器,与所述螺旋盘管反应器连通;a hypergravity reactor, communicated with the helical coil reactor;

搅拌釜反应器,与所述超重力反应器串联,以及a stirred tank reactor in series with the hypergravity reactor, and

用于将重氮反应后的重氮盐泵入所述超重力旋转填充床反应器的泵和搅拌釜反应器出料口循环打回超重力反应器的泵。The pump used to pump the diazonium salt after the diazo reaction into the supergravity rotating packed bed reactor and the pump of the discharge port of the stirred tank reactor to circulate back to the supergravity reactor.

在某些实施例中,所述系统进一步包括换热单元,所述换热单元用于控制所述螺旋盘管反应器反应腔体内的温度和所述超重力偶合反应单元反应腔体内的温度。In certain embodiments, the system further includes a heat exchange unit for controlling the temperature in the reaction chamber of the helical coil reactor and the temperature in the reaction chamber of the hypergravity coupling reaction unit.

在某些实施例中,所述换热单元包括:In some embodiments, the heat exchange unit includes:

套设在所述螺旋盘管反应器的管道外部的管道夹套,所述管道夹套具有可通入液体的空腔;a pipe jacket sleeved on the outside of the pipe of the spiral coil reactor, the pipe jacket has a cavity through which liquid can be passed;

套设在所述超重力反应器形成反应腔体的外壳外侧的外壳夹套,所述外壳夹套具有可通入液体的空腔;以及an outer shell jacket sleeved on the outer side of the outer shell of the hypergravity reactor forming the reaction cavity, the outer shell jacket has a cavity through which liquid can be passed; and

用于加热或冷却通入所述管道夹套和所述外壳夹套内液体的换热装置。A heat exchange device for heating or cooling the liquid passing into the pipe jacket and the shell jacket.

本发明的有益效果如下:The beneficial effects of the present invention are as follows:

本发明提供应用超重力的偶氮活性染料的连续化生产系统,将螺旋盘管反应器与超重力技术结合,对于重氮化反应和偶合反应区分对待,重氮化反应在螺旋盘管反应器中进行,超重力反应器用于偶合反应能够很大程度上提高转化率以及产品的质量。而螺旋盘管反应器能够精确控温,避免重氮盐的分解,这样配合下,由于温度控制精确,重氮盐分解极少,不会影响后续的偶合反应的进行,因此能够保证连续生产时重氮盐的浓度维持在较高的范围,从而能够保证同一批次的偶氮活性染料性能接近或相同,适应工业的实际需求。进一步的,在螺旋盘管内设置扰动件,可以扰动所述螺旋盘管反应器中的反应溶液,加快反应溶液的流动和混合,有利于均一化反应。The invention provides a continuous production system for azo reactive dyes using supergravity, combines a spiral coil reactor with a supergravity technology, and treats the diazotization reaction and the coupling reaction separately. The diazotization reaction is carried out in the spiral coil reactor. The supergravity reactor used for the coupling reaction can greatly improve the conversion rate and the quality of the product. The spiral coil reactor can precisely control the temperature to avoid the decomposition of the diazonium salt. In this way, due to the precise temperature control, the decomposition of the diazonium salt is very small, which will not affect the subsequent coupling reaction, so it can ensure continuous production. The concentration of the diazonium salt is maintained in a high range, so as to ensure that the properties of the azo reactive dyes in the same batch are close to or the same, and meet the actual needs of the industry. Further, a disturbance member is arranged in the spiral coil tube, which can disturb the reaction solution in the spiral coil tube reactor, accelerate the flow and mixing of the reaction solution, and facilitate the homogenization reaction.

附图说明Description of drawings

下面结合附图对本发明的具体实施方式作进一步详细的说明。The specific embodiments of the present invention will be described in further detail below with reference to the accompanying drawings.

图1示出本发明实施例中的应用超重力的偶氮活性染料的连续化生产系统结构示意图。FIG. 1 shows a schematic structural diagram of a continuous production system for azo reactive dyes using hypergravity in an embodiment of the present invention.

图2示出本发明实施例中的预混组件的结构示意图。FIG. 2 shows a schematic structural diagram of a premix component in an embodiment of the present invention.

图3a示出本发明实施例中螺旋盘管内腔中的扰动件的结构示意图之一。Fig. 3a shows one of the structural schematic diagrams of the disturbance member in the inner cavity of the helical coil according to the embodiment of the present invention.

图3b示出本发明实施例中螺旋盘管内腔中的扰动件的结构示意图之二。Fig. 3b shows the second schematic diagram of the structure of the disturbance member in the inner cavity of the helical coil according to the embodiment of the present invention.

图3c示出本发明实施例中螺旋盘管内腔中的扰动件的结构示意图之三。Fig. 3c shows the third schematic diagram of the structure of the disturbance member in the inner cavity of the spiral coil according to the embodiment of the present invention.

图3d示出本发明实施例中螺旋盘管内腔中的扰动件的结构示意图之四。Fig. 3d shows the fourth schematic diagram of the structure of the disturbance member in the inner cavity of the spiral coil according to the embodiment of the present invention.

具体实施方式Detailed ways

为了更清楚地说明本发明,下面结合优选实施例和附图对本发明做进一步的说明。附图中相似的部件以相同的附图标记进行表示。本领域技术人员应当理解,下面所具体描述的内容是说明性的而非限制性的,不应以此限制本发明的保护范围。In order to illustrate the present invention more clearly, the present invention will be further described below with reference to the preferred embodiments and accompanying drawings. Similar parts in the figures are denoted by the same reference numerals. Those skilled in the art should understand that the content specifically described below is illustrative rather than restrictive, and should not limit the protection scope of the present invention.

有鉴于此,本发明首先提供一种应用超重力的偶氮活性染料的连续化生产系统,所述系统包括:缩合反应单元,所述缩合反应单元包括缩合反应罐,用于生成偶合组分;重氮化反应单元,所述重氮化反应单元包括:预混组件,对重氮组分和重氮试剂进行预混,和螺旋盘管反应器,与所述预混组件连通,使预混后的反应溶液在所述螺旋盘管反应器内进行重氮化反应产生重氮盐;所述系统进一步包括:与所述重氮化反应单元和所述缩合反应单元相连通的超重力偶合反应单元,所述超重力偶合反应单元用于在超重力环境下使重氮盐与偶合组分进行偶合反应产生所述偶氮活性染料;其中,所述螺旋盘管反应器发生重氮化反应的内腔中设置有固定结构的扰动件,所述扰动件用于扰动所述螺旋盘管反应器中的反应溶液。In view of this, the present invention first provides a continuous production system of azo reactive dyes using supergravity, the system includes: a condensation reaction unit, the condensation reaction unit includes a condensation reaction tank for generating coupling components; A diazotization reaction unit, the diazotization reaction unit includes: a premixing component, which premixes the diazonium components and the diazonium reagent, and a spiral coil reactor, which is communicated with the premixing component to make the premixing The latter reaction solution is subjected to diazotization reaction in the spiral coil reactor to generate diazonium salt; the system further comprises: a hypergravity coupling reaction communicated with the diazotization reaction unit and the condensation reaction unit unit, the hypergravity coupling reaction unit is used to make the diazonium salt and the coupling component carry out the coupling reaction in the hypergravity environment to produce the azo reactive dye; wherein, the helical coil reactor undergoes the diazotization reaction. A perturbation member with a fixed structure is arranged in the inner cavity, and the perturbation member is used to perturb the reaction solution in the helical coil reactor.

本发明提供的上述偶氮活性染料的连续化生产系统,首先采用螺旋盘管反应器应用于重氮化反应,由于螺旋盘管式反应器的反应腔为螺旋盘管状,当需要温度控制时,可以将加热介质或冷却介质通入套设在盘管外壁的夹套中,螺旋盘管的管体直径小,管体侧壁较薄,因此设置在外侧壁上的夹套可以在极短时间内将热量通过金属管壁直接传导或移出反应体系,并且管径小,管体内的反应溶液热传导均匀,从而达到精确控温的目的,能够准确控制体系温度的升降,很大程度上降低重氮盐的分解。The continuous production system for the above-mentioned azo reactive dyes provided by the present invention firstly adopts a spiral coil reactor to be applied to the diazotization reaction. Since the reaction chamber of the spiral coil reactor is in the shape of a spiral coil, when temperature control is required , the heating medium or cooling medium can be passed into the jacket set on the outer wall of the coil. The heat is directly conducted or removed from the reaction system through the metal tube wall within a short period of time, and the tube diameter is small, and the heat conduction of the reaction solution in the tube body is uniform, so as to achieve the purpose of precise temperature control, and can accurately control the rise and fall of the system temperature and greatly reduce the weight. Decomposition of nitrogen salts.

此外,本发明进一步将螺旋盘管反应器与超重力技术结合,对于重氮化反应和偶合反应区分对待,重氮化反应在螺旋盘管反应器中进行,超重力反应器用于偶合反应能够很大程度上提高转化率以及产品的质量。而螺旋盘管反应器能够精确控温,避免重氮盐的分解,二者相结合,由于温度控制精确,重氮盐分解极少,不会影响后续的偶合反应的进行,因此能够保证连续生产时重氮盐的浓度维持在较高的范围,从而能够保证同一批次的偶氮活性染料性能接近或相同,适应工业的实际需求。In addition, the present invention further combines the spiral coil reactor with the supergravity technology, and treats the diazotization reaction and the coupling reaction differently. The diazotization reaction is carried out in the spiral coil reactor, and the supergravity reactor can be used for the coupling reaction. Maximize conversion rates and product quality. The spiral coil reactor can precisely control the temperature to avoid the decomposition of the diazonium salt. The combination of the two, due to the precise temperature control, the decomposition of the diazonium salt is very little, and will not affect the subsequent coupling reaction, so it can ensure continuous production. At the same time, the concentration of diazonium salt is maintained in a high range, so that the performance of the same batch of azo reactive dyes can be guaranteed to be close to or the same, and it can meet the actual needs of the industry.

再次,通过设置扰动件,提高盘管内反应溶液的混合,加快反应速度的同时,有利于均一化反应。Thirdly, the mixing of the reaction solution in the coil is improved by setting the perturbation element, the reaction speed is accelerated, and the uniform reaction is facilitated.

在一些实施例中,超重力反应器可以选用例如旋转填充床、定转子、折流式、螺旋通道、旋转碟片式等超重力旋转装置,其中旋转填充床包括壳体、旋转腔室,旋转腔室通过电机带动旋转,旋转腔室内设置有填料,填料用于将液体切割为微纳尺度的微元(液滴或)例如丝网填料等,本发明对此不作限制。定转子与旋转填充床不同之处在于通过固定的定子柱和旋转的转子之间的切割,进而将液体切割为微纳尺度的微元(液滴或液膜)。In some embodiments, the supergravity reactor can use a supergravity rotating device such as a rotating packed bed, a fixed rotor, a baffled flow, a spiral channel, a rotating disc type, etc., wherein the rotating packed bed includes a shell, a rotating chamber, and a rotating The chamber is driven to rotate by a motor, and a filler is arranged in the rotation chamber, and the filler is used to cut the liquid into micro-elements (droplets or) of micro-nano scale, such as wire mesh filler, etc., which is not limited in the present invention. The difference between the stator-rotor and the rotating packed bed is that the liquid is cut into micro-elements (droplets or liquid films) at the micro-nano scale by cutting between the fixed stator column and the rotating rotor.

进一步的,在优选的实施例中,所述系统进一步包括:超声馈入器,用于分别向所述螺旋盘管反应器以及所述超重力偶合反应单元馈入超声,其中向所述螺旋盘管反应器和所述超重力偶合反应单元馈入的超声强度相同或不同。Further, in a preferred embodiment, the system further comprises: an ultrasonic feeder for feeding ultrasonic waves to the helical coil reactor and the hypergravity coupling reaction unit, respectively, wherein the helical coil is fed The ultrasonic intensity fed into the tube reactor and the hypergravity coupling reaction unit is the same or different.

由于扰动件使得反应液体在盘管内形成扰流环境,同时结合超声,能够与扰流环境的宏观混合配合,通过分子振动进一步实现微观混合,进而在宏观和微观的混合同时进行,进一步达到传质混合的效果,与此同时,由于盘管管径较小,对于黏度较高的反应溶液或者浆液,扰动件的设置容易导致部分堵塞的现象,配合超声能够通过分子振动,使得分子不会在固定位置停留,显著降低堵塞现象,加快反应溶液或浆液的流动。Due to the perturbation element, the reaction liquid forms a turbulent environment in the coil. At the same time, combined with ultrasound, it can cooperate with the macro-mixing of the turbulent environment, and further realize micro-mixing through molecular vibration, and then the macro- and micro-mixing is carried out at the same time to further achieve mass transfer. The effect of mixing, at the same time, due to the small diameter of the coil tube, for the reaction solution or slurry with high viscosity, the setting of the perturbation element may easily lead to partial blockage. With the help of ultrasound, the molecules can vibrate, so that the molecules will not be fixed. Stay in place, significantly reduce the clogging phenomenon, and speed up the flow of the reaction solution or slurry.

在一个具体实施例中,如图1所示,图1示出了一种连续生产系统,该连续生产系统包括:重氮组分混合罐1、重氮试剂原料罐2、泵3、泵4、预混组件5、螺旋盘管反应器7、偶合组分原料罐9、超重力反应器11、采集容器14。其中,重氮组分混合罐1通过泵3与预混组件5连通,从而将重氮组分通入预混组件5。重氮试剂原料罐2通过泵4与预混组件5连通,从而将重氮试剂通入预混组件5,进而在预混组件5中,重氮组分和重氮试剂混合。预混组件5与螺旋盘管反应器7连通,将混合在一起的重氮组分和重氮试剂通入螺旋盘管反应器7中进行反应,经过重氮反应后进入超重力反应器11进行偶合反应,偶合反应后的产物进入采集容器14中。In a specific embodiment, as shown in FIG. 1, FIG. 1 shows a continuous production system, the continuous production system includes: a diazo component mixing tank 1, a diazo reagent raw material tank 2, a pump 3, a pump 4 , Premixing component 5 , spiral coil reactor 7 , coupling component raw material tank 9 , supergravity reactor 11 , collection container 14 . Wherein, the diazo component mixing tank 1 is communicated with the premix component 5 through the pump 3 , so that the diazo component is passed into the premix component 5 . The diazo reagent raw material tank 2 is communicated with the pre-mixing component 5 through the pump 4, so that the diazo reagent is passed into the pre-mixing component 5, and in the pre-mixing component 5, the diazo component and the diazo reagent are mixed. The premixing assembly 5 is communicated with the spiral coil reactor 7, and the mixed diazo components and the diazo reagent are passed into the spiral coil reactor 7 for reaction, and then enter the hypergravity reactor 11 after the diazo reaction. In the coupling reaction, the product after the coupling reaction enters the collection container 14 .

该实施例中包括超重力反应器11,可以用于重氮化反应-偶合反应的连续生产。例如红色活性偶氮染料活性红M-3BE。Included in this example is a hypergravity reactor 11 that can be used for continuous production of diazotization-coupling reactions. For example, the red reactive azo dye reactive red M-3BE.

在一些实施例中,如图3a至图3d所示,所述扰动件包括固定在所述螺旋盘管反应器内腔表面上的固定部,以及与所述固定部远离所述螺旋盘管反应器内腔表面的一端结合固定的自由部,所述自由部包括两个,两个所述自由部与所述固定部构成“Y”型结构或者“T”型结构。In some embodiments, as shown in FIGS. 3 a to 3 d , the disturbance member includes a fixing portion fixed on the inner surface of the helical coil reactor, and reacts with the fixing portion away from the helical coil. One end of the surface of the inner cavity of the device is combined with a fixed free portion, the free portion includes two, and the two free portions and the fixed portion form a "Y"-shaped structure or a "T"-shaped structure.

进一步的,从图3a至图3d中可以看出,所述扰动件与所述螺旋盘管反应器内腔表面垂直设置,或者倾斜设置。Further, it can be seen from Fig. 3a to Fig. 3d that the disturbance member is arranged perpendicular to the inner cavity surface of the helical coil reactor, or is arranged obliquely.

具体的,结合上述图示,所述扰动件包括沿进液方向缩径的第一部分,以及与所述第一部分的内径较小的一端连通的第二部分,所述第二部分沿进液方向呈扩径结构,并且所述第一部分和所述第二部分以其连接面为对称平面对称设置。Specifically, with reference to the above figures, the disturbing member includes a first part with a reduced diameter along the liquid feeding direction, and a second part communicating with the end of the first part with a smaller inner diameter, the second part being along the liquid feeding direction It has an expanded diameter structure, and the first part and the second part are symmetrically arranged with their connecting surfaces as the symmetry plane.

在一些实施例中,上述系统进一步包括换热单元,换热单元可以加热或冷却螺旋盘管反应器的管体,例如螺旋盘管反应器的管体外壁套设有换热夹套(图中未示出)。由于管体直径小,因此换热夹套可以快速地将热能或冷能均匀地扩散至整个管体内的空腔中。In some embodiments, the above system further includes a heat exchange unit, which can heat or cool the tube body of the spiral coil reactor, for example, the outer wall of the tube of the spiral coil reactor is sleeved with a heat exchange jacket (Fig. not shown). Due to the small diameter of the tube body, the heat exchange jacket can quickly and uniformly diffuse heat or cold energy into the cavity in the entire tube body.

在一些实施例中,所述螺旋盘管反应器中的螺旋盘管采用聚氨酯制成。这样可以防止腐蚀,同时对热传导影响较小。In some embodiments, the helical coils in the helical coil reactor are made of polyurethane. This prevents corrosion while having less effect on heat transfer.

当然,作为与该实施例不同的实施方式,所述螺旋盘管反应器中的螺旋盘管的内表面衬有聚氨酯材料层。Of course, as a different embodiment from this embodiment, the inner surface of the spiral coil in the spiral coil reactor is lined with a polyurethane material layer.

同样,为了避免腐蚀的影响,上述的泵为聚四氟平流泵。Also, in order to avoid the influence of corrosion, the above-mentioned pump is a PTFE advection pump.

在一些优选的实施例中,所述换热单元包括套设在所述螺旋盘管反应器的管道外部的管道夹套,所述管道夹套具有可通入液体的空腔;和用于加热或冷却介质通入所述管道夹套内液体的换热装置,。即通过液体来加热或冷却螺旋盘管反应器管体以实现温度的精准控制。In some preferred embodiments, the heat exchange unit comprises a pipe jacket sleeved on the outside of the pipes of the helical coil reactor, the pipe jacket has a cavity through which liquid can be passed; and used for heating Or the cooling medium is passed into the heat exchange device of the liquid in the pipe jacket. That is, the liquid is used to heat or cool the body of the helical coil reactor to achieve precise temperature control.

另外,在管道夹套内的加热或冷却介质可以为水、醇、盐溶液,也可以为油,本发明对此不做限制。In addition, the heating or cooling medium in the pipe jacket can be water, alcohol, salt solution, or oil, which is not limited in the present invention.

在上述实施例中,预混组件的具体结构如图2所示,所述预混组件包括第一输液管51(外层输液管)和第二输液管52(内层输液管);所述第一输液管51套设于所述第二输液管52的外侧,并且所述第一输液管51和所述第二输液管52之间具有空隙以供重氮组分和重氮试剂的其中一个流通,所述第二输液管52内的空腔供重氮组分和重氮试剂的其中另一个流通;所述第一输液管51靠近所述螺旋盘管反应器的一端形成供重氮组分和重氮试剂混合的预混区53,所述第二输液管52延伸至所述预混区53的入口处,并向所述预混区53喷射所述重氮组分和重氮试剂的其中另一个。具体实施时,第一输液管51和第二输液管52之间的空隙流通重氮组分,第二输液管52中流通重氮试剂,当然,在其他实施例中,反之亦然,本发明对此不做限制。In the above embodiment, the specific structure of the premix component is shown in FIG. 2 , the premix component includes a first infusion tube 51 (outer layer infusion tube) and a second infusion tube 52 (inner layer infusion tube); the The first infusion tube 51 is sleeved on the outer side of the second infusion tube 52, and there is a gap between the first infusion tube 51 and the second infusion tube 52 for the diazo component and the diazo reagent. One circulation, the cavity in the second infusion pipe 52 is for the circulation of the other of the diazo component and the diazo reagent; the first infusion pipe 51 is close to one end of the helical coil reactor to form a supply for diazonium The premixing zone 53 where the components and the diazo reagent are mixed, the second infusion pipe 52 extends to the inlet of the premixing zone 53, and the diazonium components and the diazonium are sprayed to the premixing zone 53 the other of the reagents. During specific implementation, the diazo component is circulated in the gap between the first infusion tube 51 and the second infusion tube 52, and the diazo reagent is circulated in the second infusion tube 52. Of course, in other embodiments, and vice versa, the present invention There is no restriction on this.

需要说明的是,第一输液管51的进料为垂直进料,在管体外壁形成进料口,进而避免第一输液管51和第二输液管52从同一位置(图示中的左边位置)进料导致无法进料的问题。It should be noted that the feeding of the first infusion tube 51 is vertical feeding, and a feeding port is formed on the outer wall of the tube, thereby avoiding the first infusion tube 51 and the second infusion tube 52 from the same position (the left position in the figure). ) feeding causes the problem of inability to feed.

进一步的,为了能够使得通过预混组件流出的溶液具有更快的速度,所述预混区包括临近其入口处的缩径部和与所述缩径部一体连通的平直部。这样在出料时液体的出口口径变小,能够加快流出溶液的速度。Further, in order to enable the solution flowing out through the premixing component to have a faster speed, the premixing zone includes a diameter reduction part adjacent to the inlet thereof and a straight part integrally communicated with the diameter reduction part. In this way, the outlet diameter of the liquid becomes smaller when the material is discharged, and the speed of the outflow of the solution can be accelerated.

在一些优选的实施例中,换热夹套与螺旋盘管反应器的管体外壁之间没有间隙,这样避免了低传热率的空气对传热产生影响。In some preferred embodiments, there is no gap between the heat exchange jacket and the outer wall of the tube of the helical coil reactor, so as to avoid the influence of air with low heat transfer rate on heat transfer.

螺旋盘管反应器中发生重氮化反应,生成重氮盐,由于螺旋盘管反应器可以精确控制温度,因此能够避免重氮盐的分解,使得在同一批次的连续生产中重氮盐在后续的进料浓度保持稳定不变,进而使得产品质量稳定,同一批次的产品性能相差较小。The diazotization reaction occurs in the spiral coil reactor to generate diazonium salts. Since the spiral coil reactor can precisely control the temperature, the decomposition of the diazonium salts can be avoided, so that in the continuous production of the same batch, the diazonium salts are The subsequent feed concentration remains stable, so that the product quality is stable, and the product performance of the same batch varies little.

在一些实施例中,超重力反应器可以为超重力旋转床反应器或者定转子反应器,本领域技术人员明了,本发明对超重力反应器的具体类型不做限制,根据需要,可以任意设置现有技术中所有超重力反应器的其中一种。In some embodiments, the hypergravity reactor may be a hypergravity rotating bed reactor or a stator-rotor reactor. Those skilled in the art will understand that the present invention does not limit the specific type of the hypergravity reactor, and can be arbitrarily set as required. One of all hypergravity reactors in the prior art.

需要说明的是,本实施例中超重力反应器的液体分布器为图示中的两股进料,分别喷射,但在另外一些实施例中,液体分布器喷射口处还可以设置预混区,进而在喷射前,重氮盐溶液和偶合组分各自通过第一液体进口和第二液体进口进入超重力反应器先在液体分布器的预混区进行预混,然后喷射至反应内腔中,本发明对此不做进一步限制。It should be noted that in this embodiment, the liquid distributor of the supergravity reactor is the two feeds shown in the figure, which are sprayed separately, but in other embodiments, a premixing zone can also be set at the injection port of the liquid distributor, Furthermore, before spraying, the diazonium salt solution and the coupling component respectively enter the hypergravity reactor through the first liquid inlet and the second liquid inlet to be premixed in the premixing zone of the liquid distributor, and then sprayed into the reaction inner cavity, The present invention does not further limit this.

需要说明的是,偶合反应同样需要保证一定的温度,但相较于重氮化反应而言,偶合反应对温度的控制需求不高,通过实验证明,对于偶合反应采用超重力反应器相较于螺旋盘管反应器更具优势。It should be noted that the coupling reaction also needs to ensure a certain temperature, but compared with the diazotization reaction, the coupling reaction does not require high temperature control. Spiral coil reactors are more advantageous.

另外,由于偶合反应需要保证一定的温度,可以通过上述的换热单元对超重力反应器的外壳进行加热或冷却,从而实现对温度的控制。In addition, since the coupling reaction needs to ensure a certain temperature, the outer shell of the hypergravity reactor can be heated or cooled by the above-mentioned heat exchange unit, so as to realize the temperature control.

在一些具体实施例中,换热单元进一步包括套设在所述超重力反应器形成反应腔体的外壳夹套,外壳夹套具有可通入液体的空腔。进一步的,换热装置可以同时加热或冷却管道夹套和外壳夹套内的液体。更进一步的,管道夹套和外壳夹套连通,换热介质可以自管道夹套流入外壳夹套,对此不做限制。In some specific embodiments, the heat exchange unit further comprises a shell jacket sleeved on the hypergravity reactor to form a reaction cavity, and the shell jacket has a cavity through which a liquid can be passed. Further, the heat exchange device can simultaneously heat or cool the liquid in the pipe jacket and the shell jacket. Further, the pipe jacket is communicated with the shell jacket, and the heat exchange medium can flow into the shell jacket from the pipe jacket, which is not limited.

在一些具体实施例中,所述重氮组分包括2-萘胺-1,5二磺酸,所述重氮化试剂包括亚硝酸盐和盐酸,所述偶合组分包括H酸、对位酯和三聚氯氰两次缩合所得的缩合液,这样经过本发明的上述系统产生的所述偶氮活性染料为红色活性偶氮染料活性红M-3BE。In some specific embodiments, the diazonium component includes 2-naphthylamine-1,5 disulfonic acid, the diazotization reagent includes nitrite and hydrochloric acid, and the coupling component includes H acid, para-position The condensate obtained by condensing ester and cyanuric chloride twice, so the azo reactive dye produced by the above system of the present invention is a red reactive azo dye reactive red M-3BE.

当然,本发明的连续生产系统并不局限于上述两种具体实施例,应当知晓,本系统能够适用于任何进行重氮化反应和偶合反应的偶氮活性染料,本发明在此不做穷举。Of course, the continuous production system of the present invention is not limited to the above two specific embodiments. It should be known that the system can be applied to any azo reactive dyes that carry out diazotization reaction and coupling reaction, and the present invention will not be exhaustive here. .

下面结合两个具体实例对本发明提供的连续化生成系统进行详细的说明。The continuous generation system provided by the present invention will be described in detail below with reference to two specific examples.

红色活性偶氮染料活性红M-3BE连续化生成Continuous Generation of Red Reactive Azo Dye Reactive Red M-3BE

该实施例中,所述重氮组分包括2-萘胺-1,5二磺酸,所述重氮化试剂包括盐酸和亚硝酸钠,所述偶合组分包括H酸、对位酯和三聚氯氰两次缩合所得的缩合液。In this embodiment, the diazonium component includes 2-naphthylamine-1,5 disulfonic acid, the diazonium reagent includes hydrochloric acid and sodium nitrite, and the coupling component includes H acid, para-ester and The condensate obtained by two condensations of cyanuric chloride.

重氮化反应过程为:将2-萘胺-1,5二磺酸和亚硝酸盐混合液与盐酸溶液通过预混组件进行预混,如图2所示,然后通过管道分别连续输进螺旋盘管反应器中,在出口处再循环打回螺旋管进口处,得到重氮盐悬浮液,重氮化反应在-10℃到+40℃,优选0℃到12℃下进行,进料时重氮化反应盐酸的氢离子与2-萘胺-1,5二磺酸的摩尔比为2.5~4:1,优选3:1,亚硝酸钠与对位酯的摩尔比为1~2:1,优选1.01~1.1:1,进料流速在0.08~0.8m/s,优选0.25~0.7m/s。The diazotization reaction process is as follows: the mixed solution of 2-naphthylamine-1,5 disulfonic acid and nitrite and the hydrochloric acid solution are premixed through the premixing component, as shown in Figure 2, and then continuously fed into the screw through the pipeline. In the coiled tube reactor, it is recirculated at the outlet and pumped back to the inlet of the spiral tube to obtain a diazonium salt suspension. The diazotization reaction is carried out at -10°C to +40°C, preferably 0°C to 12°C. The mol ratio of the hydrogen ion of diazotization reaction hydrochloric acid and 2-naphthylamine-1,5 disulfonic acid is 2.5~4:1, preferably 3:1, and the mol ratio of sodium nitrite and para-ester is 1~2: 1, preferably 1.01-1.1:1, the feed flow rate is 0.08-0.8m/s, preferably 0.25-0.7m/s.

缩合反应过程为:通过恒流泵将三聚氯氰和H酸通入搅拌釜中在温度0-5℃,pH为2.5~3.5下进行一次缩合反应,反应结束后再通入对位酯与一次缩合液在温度30-35℃,pH为3~4条件下进行二次缩合得到二次缩合液即偶合原料液。The condensation reaction process is as follows: the cyanuric chloride and H acid are introduced into the stirred tank through a constant flow pump to carry out a condensation reaction at a temperature of 0-5 ° C and a pH of 2.5 to 3.5. After the reaction is completed, the para-ester and The primary condensation solution is subjected to secondary condensation at a temperature of 30-35° C. and a pH of 3 to 4 to obtain a secondary condensation solution, that is, a coupling raw material solution.

偶合反应过程为:将重氮盐与偶合组分分别连续输进超重力旋转床反应器中,经混合反应生成偶氮化合物,反应温度为0℃到45℃,优选8℃~15℃;,优选pH=6~8.5;超重力反应器转速为1200~3200rpm,优选1600~1900rpm。The coupling reaction process is as follows: the diazonium salt and the coupling components are respectively continuously fed into the supergravity rotating bed reactor, and the azo compound is generated through the mixing reaction, and the reaction temperature is 0°C to 45°C, preferably 8°C to 15°C; Preferably pH=6~8.5; the rotation speed of the supergravity reactor is 1200~3200rpm, preferably 1600~1900rpm.

下面以某些具体的实验参数为示例,对通过本发明的连续化生产方法生产的红色活性偶氮染料活性红M-3BE的性能进行说明。The performance of the red reactive azo dye reactive red M-3BE produced by the continuous production method of the present invention is described below by taking some specific experimental parameters as examples.

(a)2-萘胺-1,5二磺酸重氮盐的制备(螺旋盘管反应器)(a) Preparation of 2-naphthylamine-1,5 disulfonic acid diazonium salt (spiral coil reactor)

称取6.40g2-萘胺-1,5二磺酸加水90ml,再加10%Na2CO3溶液搅拌,室温溶解至pH=6~6.5,再加入1.1178gNaNO2搅拌溶解,称为2-萘胺-1,5二磺酸与亚硝酸钠混合液液量大概为105ml。Weigh 6.40g of 2-naphthylamine-1,5 disulfonic acid, add 90ml of water, add 10 % Na2CO3 solution and stir, dissolve at room temperature to pH=6~6.5, then add 1.1178g NaNO2 and stir to dissolve, which is called 2-naphthylamine The amount of -1,5 disulfonic acid and sodium nitrite mixed solution is about 105ml.

将2-萘胺-1,5二磺酸与亚硝酸钠混合液与45ml浓度为1mol/L的盐酸通过蠕动泵打入螺旋盘管反应器的预混组件。温度由恒温槽夹套控制在8℃。得到淡黄色2-萘胺-1,5二磺酸重氮盐悬浮液。The mixed solution of 2-naphthylamine-1,5 disulfonic acid and sodium nitrite and 45 ml of hydrochloric acid with a concentration of 1 mol/L were pumped into the premixed component of the spiral coil reactor through a peristaltic pump. The temperature was controlled at 8°C by a thermostat jacket. A pale yellow suspension of 2-naphthylamine-1,5 disulfonic acid diazonium salt was obtained.

(b)偶合组分的制备(搅拌釜反应器)(b) Preparation of coupling components (stirred tank reactor)

称取4.45g的对位酯粉末,加水30ml,再加入10%Na2CO3溶液搅拌,室温溶解至pH=6~6.5,再将其抽滤得到对位酯钠盐溶液;称取5.63g H酸粉末,加水30ml,再加入10%Na2CO3溶液搅拌,室温溶解至pH=6~6.5,得到H酸双钠盐溶液;称取三聚氯氰粉末2.83g,直接倒入搅拌釜反应器中,再加入冰水混合溶液72ml,在0~5℃下打浆三聚氯氰,再通过恒流泵将H酸通入搅拌釜中进行一次缩合反应,待反应结束后,通过恒流泵将对位酯溶液再通入搅拌釜中,在30~35℃下进行二次缩合,得到二次缩合液即偶合原料液。Weigh 4.45g of para-ester powder, add 30ml of water, add 10% Na 2 CO 3 solution and stir, dissolve at room temperature to pH=6~6.5, then filter it with suction to obtain para-ester sodium salt solution; weigh 5.63g H acid powder, add 30 ml of water, then add 10% Na 2 CO 3 solution and stir, dissolve at room temperature to pH=6~6.5 to obtain H acid disodium salt solution; weigh 2.83 g of cyanuric chloride powder and pour it directly into the stirring tank In the reactor, add 72ml of ice-water mixed solution, beating cyanuric chloride at 0~5℃, and then pass H acid into the stirred tank through a constant flow pump to carry out a condensation reaction, after the reaction is over, pass the constant flow Pump the para-ester solution into the stirring tank again, and carry out secondary condensation at 30-35°C to obtain secondary condensation liquid, that is, coupling raw material liquid.

(c)偶合反应(超重力反应器)(c) Coupling reaction (hypergravity reactor)

将上述得到二次缩合液与偶合反应旋转床的其中一个入口连接,将螺旋盘管反应器出口与超重力旋转床的另外一个入口连接,分两股料进入超重力旋转床中反应,再进入搅拌釜反应器后循环打回超重力反应器,温度由恒温槽夹套控制在10℃左右,旋转床转速为1700rpm,得到红色偶合产物。The secondary condensation solution obtained above is connected with one of the inlets of the coupling reaction rotating bed, the outlet of the spiral coil reactor is connected with the other inlet of the supergravity rotating bed, and two feeds are divided into the supergravity rotating bed to react, and then enter The stirred tank reactor is recycled back to the supergravity reactor, the temperature is controlled by a constant temperature tank jacket at about 10°C, and the rotating bed speed is 1700rpm to obtain a red coupling product.

将料液进行盐析,烘干,精制,再烘干后,得到活性红M-3BE染料,收率高达96%,样品纯度高达92%。The feed liquid is salted out, dried, refined, and dried again to obtain reactive red M-3BE dye with a yield as high as 96% and a sample purity as high as 92%.

显然,本实验场景中的产品能够达到高收率和高纯度的样品,并且同一批次的产品性能几乎相同,当然,虽然本发明以红色活性偶氮染料活性红M-3BE作为连续化生产的示例,但并非表示本发明仅仅能够用于上述的示例,从本发明的发明构思来看,偶氮活性染料的种类与本发明的主体构思并无直接关联。需要了解的是,本领域普通技术人员结合本发明提出的发明构思,可以应用于任何偶氮活性染料中,本发明在此不做穷举。Obviously, the products in this experimental scenario can achieve high yield and high purity samples, and the product performance of the same batch is almost the same. Of course, although the present invention uses the red reactive azo dye reactive red M-3BE as the continuous production It is an example, but it does not mean that the present invention can only be used for the above-mentioned examples. From the perspective of the inventive concept of the present invention, the types of azo reactive dyes are not directly related to the main concept of the present invention. It should be understood that the inventive concept proposed by those skilled in the art in combination with the present invention can be applied to any azo reactive dyes, and the present invention is not exhaustive here.

显然,本发明的上述实施例仅仅是为清楚地说明本发明所作的举例,而并非是对本发明的实施方式的限定,对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式的变化或变动,这里无法对所有的实施方式予以穷举,凡是属于本发明的技术方案所引伸出的显而易见的变化或变动仍处于本发明的保护范围之列。Obviously, the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Changes or changes in other different forms cannot be exhausted here, and all obvious changes or changes derived from the technical solutions of the present invention are still within the protection scope of the present invention.

Claims (10)

1. A system for the continuous production of azo reactive dyes using supergravity, said system comprising:
a condensation reaction unit comprising a condensation reaction tank for generating a coupling component;
a diazotization reaction unit, the diazotization reaction unit comprising:
a pre-mix assembly for pre-mixing the heavy nitrogen component and the diazonium reagent, an
The spiral coil reactor is communicated with the premixing component so that the premixed reaction solution can perform diazotization reaction in the spiral coil reactor to generate diazonium salt;
the system further comprises:
the hypergravity coupling reaction unit is communicated with the diazotization reaction unit and the condensation reaction unit and is used for performing coupling reaction on diazonium salt and coupling components under a hypergravity environment to generate the azo reactive dye;
wherein, a disturbance piece with a fixed structure is arranged in an inner cavity of the spiral coil reactor for diazotization reaction, and the disturbance piece is used for disturbing the reaction solution in the spiral coil reactor.
2. The system according to claim 1, wherein the disturbing member comprises a fixed part fixed on the inner cavity surface of the spiral coil reactor and two free parts fixed with one end of the fixed part far away from the inner cavity surface of the spiral coil reactor, and the two free parts and the fixed part form a Y-shaped structure or a T-shaped structure.
3. The system of claim 2, wherein the disturbance element is disposed perpendicular to the inner cavity surface of the helical coil reactor or is disposed obliquely.
4. The system according to claim 1, wherein the disturbing member comprises a first portion which is reduced in diameter in the liquid inlet direction, and a second portion which is communicated with one end of the first portion having a smaller inner diameter, the second portion has an enlarged diameter structure in the liquid inlet direction, and the first portion and the second portion are symmetrically arranged with the connecting surface as a symmetrical plane.
5. The system of claim 1, further comprising:
and the ultrasonic feeder is used for feeding ultrasonic waves into the spiral coil reactor and the hypergravity coupling reaction unit respectively, wherein the ultrasonic intensities fed into the spiral coil reactor and the hypergravity coupling reaction unit are the same or different.
6. The system of claim 1, wherein the premix assembly comprises a first fluid line and a second fluid line;
the first infusion tube is sleeved outside the second infusion tube, a gap is formed between the first infusion tube and the second infusion tube to allow one of the diazo component and the diazo reagent to flow through, and a cavity in the second infusion tube allows the other of the diazo component and the diazo reagent to flow through;
one end of the first liquid conveying pipe, which is close to the spiral coil reactor, forms a pre-mixing area for mixing the diazo component and the diazo reagent, and the second liquid conveying pipe extends to an inlet of the pre-mixing area and sprays the other one of the diazo component and the diazo reagent to the pre-mixing area.
7. The system of claim 6, wherein the premixing zone comprises a reduced diameter portion adjacent to an inlet thereof and a flat portion in integral communication with the reduced diameter portion.
8. The system of claim 1, wherein the supergravity coupling reaction unit comprises:
the supergravity reactor is communicated with the spiral coil reactor;
a stirred tank reactor in series with the hypergravity reactor, an
And the pump is used for pumping diazonium salt after diazo reaction into the hypergravity rotating packed bed reactor and the pump of the discharge port of the stirred tank reactor to circularly pump back to the hypergravity reactor.
9. The system of claim 1, further comprising a heat exchange unit for controlling the temperature within the helical coil reactor reaction chamber and the temperature within the supergravity coupled reaction unit reaction chamber.
10. The system of claim 9, wherein the heat exchange unit comprises:
the pipeline jacket is sleeved outside the pipeline of the spiral coil reactor and is provided with a cavity into which liquid can be introduced;
the shell jacket is sleeved on the outer side of a shell of the reaction cavity formed by the supergravity reactor and is provided with a cavity into which liquid can be introduced; and
and the heat exchange device is used for heating or cooling liquid introduced into the pipeline jacket and the shell jacket.
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