KR20100111557A - Salting-out crystallization apparatus - Google Patents

Abstract

PURPOSE: A salting-out crystallization apparatus is provided to improve energy efficiency by varying conditions for salting-out crystallization processes. CONSTITUTION: A transferring and supplying unit(110) supplies salt. A reacting unit includes a reaction tank(121) and a mixing motor(122). The reacting unit mixes a mixed liquid containing the salt in the reaction tank. A separating and collecting unit(130) includes an internal rotator and a separating motor(133). The internal rotator includes a filtering net. The separating motor rotates the internal rotator in one direction. The separating and collecting unit separates crystallized reactive dye.

Description

Salting out crystallization device {Salting-out Crystallization Apparatus}

The present invention relates to a salt crystallization apparatus for separating the solid phase dye from the dye synthesis liquid, more specifically, it is possible to vary the process conditions for the salt crystallization in various ways, through which the energy cost and production cost required to produce the dye The present invention relates to a salt crystallization apparatus which can obtain a maximum production yield while reducing the cost.

In particular, the present invention is a device designed for the salt crystallization process for the precipitation of the reactive dye in the dye synthesis liquid salt salt that can proceed a plurality of processes such as dye synthesis process, salt crystallization process, dye separation / recovery process in a single device It is a crystallizer. The reactor portion is a general reactor type, in addition to the salt crystallization process can proceed with the organic synthesis reaction process, and the connection device is configured to proceed with the reaction of several stages using a single reactor. Through the salt injector at the top of the reactor, salts can be added according to the appropriate amount / time to optimize the salt input method with minimal error. From the reactor to the separation recovery device, gravity can be used to deliver the solution without specific power. In the case of the separation recovery device, the dye is separated from the dye solution by rotating the inner cylinder using the principle of centrifugation. Vacuum filter which is generally used for separating and recovering dyes obtained through salt crystallization consumes a lot of time and energy. The separation and recovering apparatus of the present invention consumes much less time and energy than the existing process and is higher. Yield can be obtained. The entire series of processes can be easily controlled in real time through the computer screen drawn from the control panel outside the device through the electronic control device inside the device, and equipped with equipment to check the power consumption of the entire device. In the recovery process optimization study, the energy recovery effect can be directly calculated by designing and optimizing the process so that the dye recovery rate and energy consumption can be considered as a high yield and low energy process.

As the chemical industry develops, there is an increasing demand for improving the properties and physical properties of the final product, and it is becoming more important from an economic point of view. The crystallization process is carried out in a homogeneous solution or a mixed solution in which solid, liquid, or gas are dissolved. It is to selectively separate useful substances.

The R & D cost of the fine chemicals using this crystallization process exceeds the R & D cost of bulk chemicals, and the crystallization process of producing the final product in the form of crystals includes biotechnology, resource engineering, environmental engineering, pollution control, energy storage, It is applied in various fields such as manufacturing new materials.

On the other hand, the above crystallization process is also required in the process of manufacturing the dye. Water and an organic solvent are mainly used as a solvent used to prepare the dye, and the water and the organic solvent dissolve the reactants so that a liquid phase reaction may occur.

However, the organic solvent has a high solubility in the intermediate product as a product and prevents the dye from depositing into the solid powder. Moreover, since the intermediate product contains a large amount of water, the mixing relationship between water and the organic solvent is also an important variable in dye synthesis. In particular, in the mixed solution of water and organic solvent, the solubility of the intermediate product is remarkably low, and solid particles may be precipitated. As such, the amount of the solid powder obtained varies according to the composition of water and the organic solvent, and energy loss occurs due to the phenomenon, and there is a problem in that it is difficult to reduce the quality of the product and recycle the resources. Therefore, there was a need to solve this problem by improving the crystallization process.

In general, the crystallization method is known as the single crystal manufacturing method (Singl Crystarllization), which is known to manufacture semiconductor wafers or artificial diamond, and the industrial crystallization method that produces many crystals is known.

In addition, depending on the method of forming the driving force to precipitate the solute into a solid phase it may be classified into Reaction Crystallization, Cooling Crystallization, Salting-out Crystallization and the like.

There are various types of dyes, and each dye has a different salt crystallization method, so that the existing salt crystallization method cannot be established systematically, and the yield of salt crystallization is remarkably improved even with a slight modification of the conditions affecting the salt crystallization. There was a declining issue. Thus, no attempt has been made to improve the salt crystallization method until now.

Therefore, the present invention has been made to solve the above problems, the object of which is to vary the process conditions for crystallizing salts, the maximum production yield while reducing the energy and production costs required to produce dyes It is to provide a salt crystallization apparatus that can be obtained.

Through the present invention, the three main points were mainly focused on, the first is the unification of the various process equipment, the second is the new process application of the separation / recovery device, the third is the energy saving of the entire process.

Implementing a process that has been carried out by moving devices of all single processes into a single device in one device can reduce the loss of various resources consumed while moving the device. Overall, the entire process can be controlled easily and quickly. It is also designed to be applicable to additional processes such as organic synthesis processes other than salt crystallization processes.

In the case of separation / recovery device, a small cylinder inside a large cylinder rotates using the principle of centrifugal separator, and dye is separated / recovered by using a membrane on the outer surface of the small cylinder, which is much larger than conventional vacuum filtration. The same result can be obtained by consuming less energy and time.

By combining the whole process into a single device, you can easily and quickly control it, and you can see the energy consumption through a panel that can check the total power consumption. Can give

As a specific means for achieving the above object, the present invention is provided with a salt storage chamber filled with a predetermined amount of salt, and equipped with a feeder for transferring the salt discharged from the discharge port provided in the lower end of the salt storage chamber to one side A transfer supply unit for discharging and supplying the transfer; A stirring tank including a mixed solution of a predetermined amount of salt and a predetermined amount of the dye synthesis liquid is discharged from the outlet end of the transfer supply unit for mixing, for stirring to rotate the stirring blades disposed inside the reaction tank in one direction A reaction unit equipped with a motor to stir a mixed solution of a supernatant and a salt in the reaction tank to determine a reactive dye; And an inner rotary body having a filtering network to which a predetermined amount of a mixed solution including a reactive dye crystallized in the inner space of the outer fixing body connected through the reaction tank and the discharge pipe is injected, and separating the rotating inner rotating body in one direction. A separation and recovery unit equipped with a motor for separating and recovering the crystallized reactive dye from the mixed solution; It provides a salt crystallization apparatus comprising a.

Preferably, the feeder unit includes a feeder tube having one end connected to the outlet of the salt storage chamber and the other end connected to the reaction tank, and a transfer motor for rotating and rotating the screw shaft disposed in the feeder tube in one direction.

Preferably, the reaction tank is extended from the inner reaction tube to form a space between the inner reaction tube having an inner space in which the mixed liquid is stored a certain amount, and the outer surface of the inner reaction tube to form a space, the inner reaction An outer reaction tube surrounding the outer surface of the tube and a cover member assembled through a sealing member to seal the open upper portion of the inner reaction tube.

More preferably, the inner reaction tube is the inner hollow tube through the inner flow through the upflow flow of the mixed solution from the bottom to the upper side during the rotation of the stirring blade disposed in the center, the inner hollow tube through the gap between the maintaining member It is disposed and includes an outer hollow park clearance to induce the downflow flow of the mixed liquid from the top to the bottom.

More preferably, the inner hollow tube has an inclined plate protruding inwardly in a plurality of openings formed through the outer surface.

Preferably, the outer fixing body is mounted on the upper surface of the mixed liquid processing chamber having an internal space of a predetermined size, the separation motor is fixedly installed by the support bracket in the inner space of the mixed liquid processing chamber, and the internal fixed body And a drain tube having a valve member to discharge the mixed liquid separated from the mixture into the mixed liquid processing chamber.

Preferably, the conveying supply and the reaction unit measures and displays the temperature of the mixed solution, displays the measured stirring speed of the stirring blades, displays the reaction time in the reaction tank, measured by the measured concentration of the mixed liquid It is provided in the main body part which has a display part.

Preferably, the salt is KCl or NaCl, and the dye synthesis solution contains 20 to 25% by weight of a reactive dye by adding ammonium hydroxide to the dye intermediate combined the chromophore and trichlorotriazine.

Preferably, 10-15% by weight of the salt is added to the dye synthesis liquid in the reaction tank and mixed, and the mixing of the salt and the dye synthesis liquid is made at a reaction temperature of 20 ~ 25 ℃.

As described above, according to the salt crystallization apparatus according to the present invention, it is possible to vary the process conditions for crystallizing the reactive dye, and to improve energy efficiency by reducing the energy cost required to produce the dye. In addition, it can reduce the power consumption required to produce dyes, reduce production costs, reduce the emission of carbon dioxide and environmentally harmful substances, and significantly improve the yield of producing high-quality dyes.

Hereinafter, preferred embodiments of the present invention will be described in more detail with reference to the accompanying drawings.

1 is an overall configuration diagram showing a salt crystallization apparatus according to a preferred embodiment of the present invention, Figure 2 is a block diagram showing a reaction portion employed in the salt crystallization apparatus according to a preferred embodiment of the present invention, Figure 3 is Figure 2 is a block diagram showing a separation recovery portion employed in the salt crystallization apparatus according to a preferred embodiment of the present invention.

Salt crystallization apparatus 100 according to a preferred embodiment of the present invention, as shown in Figures 1 to 3, the transfer supply unit 110, the reaction unit 120 and the separation recovery unit 130.

The transfer supply unit 110 includes a salt storage chamber 111 and a feeder unit 115 to inject salt into the reaction tank of the reaction unit, the salt storage unit 111 of a predetermined amount stored in a powder state The salt is filled and stored, and consists of a chamber member having an outlet 112 for discharging the salt at the lower end.

The feeder unit 115 is provided at the lower portion of the salt storage chamber 111 so that the salt discharged from the discharge port provided at the lower end of the salt storage chamber 111 can be transferred to the reaction unit side.

The feeder unit 115 has one end connected to the outlet of the salt storage chamber 111, the other end is connected to the reaction tank and the screw shaft 117 disposed in the feeder tube 116 And a conveying motor 118 for forcibly transferring the salt supplied into the feeder pipe 116 to the reaction tank by rotating the screw shaft 117 in one direction.

Here, the transfer motor 118 is connected to the end of the screw shaft 117 through the belt member 118a to drive and rotate the screw shaft 117, but it is not limited thereto. In addition, the screw shaft 117 and the drive shaft of the feed motor may be directly connected or connected via a gear member to transmit rotational power.

Accordingly, the salt stored in the salt storage chamber 111 is a reaction tank 121 in which a predetermined amount of the dye synthesis liquid is stored through the feeder pipe 116 in proportion to the amount of rotation when the transfer motor 118 rotates. It can be mixed with the dye synthesis liquid is added into the pre-stored in the reactor.

The reaction unit 120 is a reaction tank 121 and the stirring motor 122 to crystallize the reactive dye by forcibly stirring the mixed solution of the pre-stored dye synthesis solution and the salt introduced through the feeder at a predetermined temperature Include.

The reaction tank 121 stores a mixture of a predetermined amount of salt and a predetermined amount of the dye synthesis liquid discharged from the outlet end of the feeder unit 115, and stores a reaction mixture having a predetermined size to precipitate a reactive dye. Has

The reaction tank 121 is formed so as to form a space with a predetermined interval between the internal reaction tube (121a) having a predetermined size of the internal space in which the mixed liquid is stored a certain amount, and the outer surface of the internal reaction tube (121a). An external reaction tube 121b extending from the internal reaction tube 121a and surrounding the outer surface of the internal reaction tube 121 and a sealing member 123a to seal the opened upper portion of the internal reaction tube 121a are mediated. The cover member 123 is assembled with.

Here, the inner and outer reaction tubes (121a, 121b) is preferably made of a transparent glass material so that the reaction state of the mixed liquid can be observed with the naked eye.

The locking jaw formed at the upper end of the inner reaction tube 121a is raised over the upper end of the support 124 provided in the main body 140, and the sealing member 123a is disposed on the upper end surface of the inner reaction tube 121a. The close cover member 123 is assembled to the support 124 by a plurality of fastening members.

The inner reaction tube (121a) and the inner hollow park pipe 126a to guide the upward flow of the mixed solution from the bottom to the upper side during the rotation of the stirring blades 125 disposed in the center, and the inner hollow park pipe (126a) and It is disposed on the outside via the gap holding member 126c and includes an outer hollow park pipe 126b for inducing a downward flow of the mixed liquid from the top to the bottom.

Here, the outer hollow park pipe (126b) is connected to the support rod 127, the upper end of which is fixed to the cover member 123 is supported by the inner hollow park pipe (126a) in the inner space of the inner reaction tube (121a) With can be arranged.

Accordingly, when the stirring blade 125 is rotated, the mixed liquid in the inner reaction tube forms an upward flow flowing from the lower portion of the inner hollow park clearance to the upper portion, and from the upper portion between the inner hollow park clearance and the outer hollow park clearance. After forming a downward flow flowing to the bottom to form a circulating flow flowing into the lower portion of the inner hollow park clearance.

At this time, the inner hollow pipe 126a is provided with a slope plate 126d protruding obliquely inward in the plurality of openings 126e formed through the outer surface, thereby flowing from the bottom to the top in the inner cylindrical pipe 126a. Part of the upstream flow can be guided through the opening 126e between the inner and outer hollow parks 126a and 126b.

The stirring motor 122 is a motor member for rotationally driving the stirring blades 125 disposed in the inner reaction tube of the reaction tank 121 in one direction, and the stirring blades 125 penetrate the cover member 123. It is preferably assembled to the end of the drive shaft (122a), between the cover member 123 and the drive shaft (122a) is preferably assembled via a bearing member.

In addition, the inner reaction tube (121a) is provided with a liquid supplement tube 128, which is supplemented with a dye synthesis liquid mixed with the salt, the dye synthesis liquid is added ammonium hydroxide (NH ₄ OH) to the dye intermediate. It is an aqueous solution containing a certain amount of the reactive dye.

The separating and recovering unit 130 separates and recovers the crystallized reactive dye from the mixed solution stirred inside the reactor, the outer fixing body 131a and the inner rotating body 131b, the filtering network 132 and the separating motor 133 The outer fixing body (131a) is connected to the inner reaction tube 121a and the discharge tube 134 of the reaction tank 121 is a substantially cylindrical shape that is supplied with a mixed solution containing the crystallized reactive dye It is a receiving member.

Here, a valve member 134a is provided in the middle of the length of the discharge pipe 134 so as to control the discharge amount of the mixed liquid discharged from the reaction tank 121.

The inner rotating body 131b is a substantially cylindrical structure that is rotatably disposed in the inner space of the outer fixing body 131a by inserting and placing the filtering net 132 inside the body.

The internal rotating body 131b has a connecting pipe 135 connected to the discharge pipe 134 at the upper end of the body, and the connecting pipe 135 is a bearing member 135a provided in the external fixing body 131a. It is rotatably assembled via a medium, the lower end of the body of the inner rotating body (131b) is driven by the separation motor 133 is connected to the rotating shaft 136 supported by the bearing member (136a).

The filter net 132 is disposed in the inner space of the inner rotor 131b and is further rotated at a high speed while remaining only the crystallization reactive dye contained in the mixed solution supplied into the inner rotor through the discharge pipe 134. Is a substantially hollow cylindrical filter member having a mesh member of a predetermined size on the outer surface of the body for external discharge.

The separation motor 133 has been shown and described as rotating the drive shaft by connecting the rotary shaft 136 and the belt member 133a connected to the lower end of the body of the internal rotating body 131b, but is not limited thereto. The rotation shaft 136 and the driving shaft of the separation motor 133 may be directly connected or may be connected via a gear member to transmit rotational power.

Accordingly, the inner rotating body 131b having the filter net 132 disposed therein may be capable of separating the crystallization reactive dye contained in the mixed solution while rotating at a high speed in one direction inside the outer casing when the separation motor is driven. .

On the other hand, the outer fixing body 131a is mounted on the upper surface of the mixed liquid processing chamber 137 having an internal space of a predetermined size, and separated by a support bracket 133b in the inner space of the mixed liquid processing chamber 137. The motor 133 is fixedly installed, and has a drain pipe 139 having a valve member 139a for discharging and transporting the mixed liquid separated from the internal fixing body into the mixed liquid processing chamber 137.

In addition, the transfer supply unit 110 and the reaction unit 120 measures and displays the temperature of the mixed solution, measures and displays the stirring speed of the stirring blade 125, and displays the reaction time in the reaction tank 121. It is provided in the main body 140 having a display unit 141 for displaying and measuring the lung concentration of the mixed liquid.

The main body 140 may include a power computer 142, a power switch 143, and an emergency switch 144. The lower end may include a wheel member 145 to facilitate free movement of the main body. have.

Before preparing the reactive dye using the salt crystallization apparatus according to a preferred embodiment of the present invention to prepare a dye synthesis liquid supplied into the inner reaction tube of the reactor.

That is, by combining the chromophore (Formula 1) below with the unique color of the reactive dye to be prepared with trichlorotriazine having three chlorine groups (Cl group), the first intermediate group of trichlorotriazine is substituted with a dye intermediate. Manufacture.

[Formula 1]

Subsequently, when ammonium hydroxide (NH ₄ OH) is added to the dye intermediate prepared in Chemical Formula 1, a dye synthesis including 20 to 25 wt% of Reactive Black 8, which is a reactive dye in which a second chlorine group (Cl group) of trichlorotriazine is substituted, is added. The liquid is prepared, and the prepared dye synthesis liquid is filled with a predetermined amount of the internal space of the internal reaction tube 121a of the reaction tank 121 through the liquid supplement pipe 128.

Here, the temperature of the dye synthesis liquid to be filled in the inner reaction tube reaches approximately 45 ℃, after that the temperature of the dye synthesis liquid gradually lowered without a separate heating and cooling to maintain the temperature from the outside 20 ~ 25 By inducing to have a temperature range of ℃ it is not necessary to supply a separate energy source for maintaining the temperature can reduce the energy cost, and the cost of producing the dye.

In this state, when the transfer motor 118 provided in the feeder unit is operated, the salt stored in the salt storage chamber 111 and discharged through the discharge port 112 is transferred to the transfer motor 118. In the rotational drive in proportion to the amount of rotation is introduced into the internal reaction tube (121a) of the reaction tank 121 through the feeder tube 116 and mixed with the pre-stored dye synthesis liquid inside the internal reaction tube (121a) mixed liquid To prepare.

In this case, the mixed solution is preferably mixed by adding 10 to 15% by weight of the salt to the dye synthesis liquid, this mixing is preferably made at a reaction temperature of 20 to 25 ℃, salt mixed with the dye synthesis liquid Silver selectively uses either potassium chloride (KCl) or sodium chloride (NaCl).

Subsequently, when the stirring blade 125 disposed in the inner reaction tube 121a of the reaction tank 121 is stirred at 100 to 200 rpm for 2 hours at a temperature of approximately 25 ° C., the inner reaction tube Of the mixed liquid forms an upward flow flowing from the bottom of the inner hollow park clearance to the top, and forms a downward flow flowing from the top to the bottom between the inner hollow park clearance and the outer hollow park clearance, and then to the lower portion of the inner hollow park clearance. Crystallization of the reactive dye contained in the mixed solution proceeds while forming an inflowing flow.

Then, the mixed solution including the reactive dye crystallized through the discharge pipe 134 connected to the internal reaction tube 121a is supplied to the internal space of the internal rotating body 131b of the separation recovery unit 130.

In this state, when the inner rotary body 131b disposed in the inner space of the outer fixing body 131a by high speed rotation driving by the rotation driving force of the separating motor 133 is supplied to the inner rotating body, Crystallized reactive dye in the mixed solution is retained by the filter net 132 disposed inside the inner rotor 131b, while the remaining mixed solution is discharged into the external fixture to separate and recover the mixed solution and the reactive dye. will be.

Reactive Black 8, which is a reactive dye such as Chemical Formula 2, is colored when one non-reacted chlorine group (Cl group) of trichlorotriazine is combined with a fiber product when coloring the fiber product.

[Formula 2]

Example 1 (variables of reactive dye concentration)

For the dye concentrations of Reactive Black 8, a reactive dye, (a) 15 wt%, (b) 20 wt%, and (c) 25 wt%, the crystallization yield was determined according to the salt concentration (salt conc.) And the reaction temperature (temp.). The contour diagrams are shown in Figs. 4 (a) (b) (c). At this time, the stirring speed of the stirring blade was 100 rpm, and the reaction time in the reactor was fixed at 1 hour.

As shown in Figs. 4 (a) to 4 (c), as the concentration of Reactive Black 8 increases, the green part showing the crystallization yield of 96% or more increases. That is, the higher the concentration of Reactive Black 8, the higher the crystallization yield, and the higher the crystallization yield when the reaction temperature (temp.) Was low and the salt concentration (salt conc.) Was high.

Example 2 (variable salt concentrations)

For the case of the salt concentration of (a) 5wt%, (b) 10wt%, (c) 15wt%, the contour diagram of the crystallization yield according to the concentration of Reactive Black 8 and the reaction temperature (salt conc.) Is shown in FIG. (b) and (c). At this time, the stirring speed of the stirring blade was 100 rpm, and the reaction time in the reactor was fixed at 1 hour.

As shown in Fig. 5 (a) to Fig. 5 (c), as the salt concentration increases, the green portion showing a crystallization yield of 90% or more increases. That is, the higher the salt concentration, the higher the crystallization yield, the lower the reaction temperature (salt conc.) And the higher the concentration of Reactive Black 8 (dye conc.), The higher the crystallization yield.

Example 3 (variable of reaction temperature)

Contour plot for crystallization yield according to the concentration of Reactive Black 8 (dye conc.) And salt concentration (salt conc.) For the reaction temperature of (a) 20 ° C, (b) 30 ° C, and (c) 40 ° C. Is shown to Fig.6 (a) (b) (c). At this time, the stirring speed of the stirring blade was 100 rpm, and the reaction time in the reactor was fixed at 1 hour.

As shown in Fig. 6 (a) to (c), as the reaction temperature is lowered, there are more green parts showing 96% or more of crystallization yield. That is, the crystallization yield was high when the salt concentration (salt conc.) And Reactive Black 8 concentration (dye conc.) Is high.

In Examples 1 to 3, the optimum conditions in the salt crystallization apparatus are 20 to 25 wt% of the reactive dye, Reactive Black 8, 13 to 15 wt% of the salt, and a temperature range of 20 to 25 ° C. I could see that.

While the invention has been shown and described with respect to particular embodiments, it will be understood that various changes and modifications can be made in the art without departing from the spirit or scope of the invention as set forth in the claims below. It will be appreciated that those skilled in the art can easily know.

1 is an overall configuration diagram showing a salt crystallization apparatus according to a preferred embodiment of the present invention.

Figure 2 is a block diagram showing a reaction unit employed in the salt crystallization apparatus according to a preferred embodiment of the present invention.

Figure 3 is a block diagram showing a separate recovery portion employed in the salt crystallization apparatus according to a preferred embodiment of the present invention.

4 (a) to 4 (c) show the salt concentration and the reaction temperature when the dye concentration (dye conc.) Is (a) 15wt%, (b) 20wt%, and (c) 25wt%. Graph showing contour plot for crystallization yield according to (temp.).

5 (a) to 3 (c) show the concentration of RB 8 dye (c) and the reaction temperature (temp.) When the salt concentration is (a) 5 wt%, (b) 10 wt%, and (c) 15 wt%. Is a graph showing the contour plot for the crystallization yield according to

6 (a) to 4 (c) show the RB 8 dye concentration and salt concentration for the reaction temperature of (a) 20 ° C, (b) 30 ° C, and (c) 40 ° C. Graph showing contour plot for crystallization yield according to.

Explanation of symbols on the main parts of the drawings

110: transfer supply 111: salt storage chamber

112: outlet 115: feeder portion

116: feeder tube 117: the screw shaft

118: transfer motor 120: reaction unit

121: reactor 121a: internal reaction tube

121b: external reaction tube 122: stirring motor

123: cover member 124: support

125: stirring blade 128: liquid filling pipe

130: separate recovery unit 131a: external fixture

132: internal rotating body 132: filter network

133: separation motor 134: discharge pipe

137: mixed liquid processing chamber 140: main body

Claims (9)

A transfer supply unit having a salt storage chamber filled with a predetermined amount of salt, and having a feeder unit for transferring the salt discharged from the discharge port provided at the lower end of the salt storage chamber, to transfer and discharge the salt to one side; A stirring tank including a mixed solution of a predetermined amount of salt and a predetermined amount of the dye synthesis liquid is discharged from the outlet end of the transfer supply unit for mixing, for stirring to rotate the stirring blades disposed inside the reaction tank in one direction A reaction unit equipped with a motor to stir a mixed solution of a supernatant and a salt in the reaction tank to determine a reactive dye; And An inner rotary body having a filter net to which a predetermined amount of a mixed liquid containing a reactive dye crystallized into an inner space of an outer fixing body connected through the reaction tank and the discharge pipe is provided, and for rotating the inner rotating body in one direction A separation and recovery unit equipped with a motor to separate and recover the crystallized reactive dye from the mixed solution; Salt crystallization apparatus comprising a.  The feeder unit of claim 1, wherein the feeder unit includes a feeder tube having one end connected to an outlet of the salt storage chamber and the other end connected to the reaction tank, and a transfer motor rotating the screw shaft disposed in the feeder tube in one direction. Salt crystallization apparatus, characterized in that.  The method of claim 1, wherein the reaction tank is extended from the inner reaction tube to form a space between the inner reaction tube having an inner space in which the mixed liquid is stored a predetermined amount and the outer surface of the inner reaction tube at a predetermined interval Salt crystallization apparatus comprising an outer reaction tube surrounding the outer surface of the inner reaction tube, and a cover member assembled through a sealing member to seal the open upper portion of the inner reaction tube. According to claim 3, The inner reaction pipe is the inner hollow pipe through the inner flow through the flow of the mixed liquid from the bottom to the upper side during the rotation of the stirring blade disposed in the center, and through the inner hollow park clearance and the space maintaining member through the medium; Salt crystallization device, characterized in that it comprises an outer hollow pipe through which is disposed on the outside to direct the flow of the mixed flow from the top to the bottom.  5. The salt crystallization apparatus as claimed in claim 4, wherein the inner hollow passage has an inclined plate which protrudes inwardly in a plurality of openings formed through the outer surface thereof. According to claim 1, wherein the outer fixture is mounted on the upper surface of the mixed liquid processing chamber having a predetermined internal space, the separation motor is fixed to the inner space of the mixed liquid processing chamber by a support bracket), And a drain pipe having a valve member for discharging and transporting the mixed liquid separated from the internal fixed body into the mixed liquid processing chamber. The method of claim 1, wherein the feed supply and the reaction unit measures and displays the temperature of the mixed solution, measures and displays the stirring speed of the stirring blade, displays the reaction time in the reaction tank, and the waste concentration of the mixed solution Salt-crystallization apparatus provided in the main-body part which has a display part to measure and display.  The salt crystallization apparatus of claim 1, wherein the salt is KCl or NaCl, and the dye synthesis solution contains 20 to 25 wt% of a reactive dye by adding ammonium hydroxide to a dye intermediate in which a chromophore and trichlorotriazine are combined. . According to claim 1, wherein the salt is added to the dye mixture in the reaction mixture by mixing 10 to 15% by weight of the salt, the salt and the dye mixture is mixed salt characterized in that the reaction is made at a reaction temperature of 20 ~ 25 ℃ Crystallization device.

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