CN108727856A - The synthetic method of the water-soluble dye of a kind of cyano-containing - Google Patents
The synthetic method of the water-soluble dye of a kind of cyano-containing Download PDFInfo
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- CN108727856A CN108727856A CN201810878515.XA CN201810878515A CN108727856A CN 108727856 A CN108727856 A CN 108727856A CN 201810878515 A CN201810878515 A CN 201810878515A CN 108727856 A CN108727856 A CN 108727856A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B29/00—Monoazo dyes prepared by diazotising and coupling
- C09B29/06—Monoazo dyes prepared by diazotising and coupling from coupling components containing amino as the only directing group
- C09B29/08—Amino benzenes
- C09B29/0801—Amino benzenes containing acid groups, e.g. COOH, SO3H, PO3H2, OSO3H, OPO3H2; SO2NHSO2R or salts thereof, R being hydrocarbonyls
- C09B29/0803—Amino benzenes containing acid groups, e.g. COOH, SO3H, PO3H2, OSO3H, OPO3H2; SO2NHSO2R or salts thereof, R being hydrocarbonyls containing SO3H, OSO3H
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
- B01F27/90—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/181—Preventing generation of dust or dirt; Sieves; Filters
- B01F35/188—Preventing generation of dust or dirt; Sieves; Filters using sieves in mixers for purposes other than mixing, e.g. eliminating dust during venting
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B29/00—Monoazo dyes prepared by diazotising and coupling
- C09B29/0003—Monoazo dyes prepared by diazotising and coupling from diazotized anilines
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Accessories For Mixers (AREA)
Abstract
The invention discloses the synthetic methods of the water-soluble dye of a kind of cyano-containing, including fixed bottom plate, the upper end of the support base is fixedly installed a seal casinghousing, the seal casinghousing is internally provided with a reaction compartment, the rotary shaft for being internally provided with a vertical direction of the reaction compartment, it is evenly distributed with multiple stirring rods on the axis body that the rotary shaft is located in reaction compartment, the aft bulkhead upper end of the reaction compartment is provided with an automatically controlled feeding gate, it is installed with a liquid reserve tank on rear side of the fixed bottom plate upper surface, it is installed with a filter on front side of the fixed bottom plate upper surface.In present invention work, water in first connected space enters the second connected space by recirculation hole, convenient for the temperature inside control reaction compartment, the temperature of device is set to control sensitiveer, quick, diazotising, multiple reaction process of coupling reaction are completed by a device, the usage quantity for the equipment effectively saved saves resource for the preparation of dyestuff.
Description
Technical field
The present invention relates to dye field, the synthetic method of the water-soluble dye of specially a kind of cyano-containing.
Background technology
Direct dyes or reactive dye are wide in variety, and chromatography is complete, bright in colour, cheap, are easy to colorant match, dyeing or
Printing method is easy, widely used, is particularly important one of the dye class of dye industry.But it is maximum the disadvantage is that this kind of dyestuff
Dyefastness it is most of all not ideal enough, degree of fixation is low, and against weather is poor, is easy to decompose under the action of external environment,
Lead to pollutant colour fading etc., influences the dyeability of these dyestuffs, for the defect that dyefastness is poor, people have made many
Reform, for example, by using chemicals, post-processes the cloth for having caught color, improves the washable and light fastness of painting cloth；
Also have and the post-processing fastness of dyed fabric is improved using novel interlinkage color fixing agent, and have can for the water-soluble dye of cyano-containing
By ground fastness, but it is limited to production cost height, and can not put goods on the market, at present both at home and abroad about the water-soluble dye of cyano-containing
Synthetic method be also rarely reported.
Invention content
The purpose of the present invention is to provide the synthetic methods of the water-soluble dye of a kind of cyano-containing, to solve above-mentioned background skill
The problem of being proposed in art.
To achieve the above object, the present invention provides the following technical solutions：The synthesis side of the water-soluble dye of a kind of cyano-containing
Method, including fixed bottom plate, the middle position of the fixed bottom plate upper surface are provided with a support base, the upper end of the support base
It is fixedly installed a seal casinghousing, the seal casinghousing is internally provided with a reaction compartment, and the inside of the reaction compartment is set
It is equipped with the rotary shaft of a vertical direction, the reaction compartment upper and lower ends pars intramuralis is respectively set at position corresponding with rotary shaft
There are the first connected space and the second connected space, the first intercommunicating pore is provided at the lower end wall of first connected space, it is described
First intercommunicating pore is connected to reaction compartment and the first connected space, and the upper end of the rotary shaft passes through the first intercommunicating pore and extends into
First connected space, the second intercommunicating pore is provided at the upper end wall of second connected space, and the second intercommunicating pore connection is anti-
Space and the second connected space, the lower end of the rotary shaft is answered to pass through the second intercommunicating pore and extend into the second connected space, institute
It states equal fixing sleeve on the axis body of rotary shaft upper and lower ends and one sealing rubber plug is housed, the rotary shaft is located in the second intercommunicating pore
Fixing sleeve is equipped with the support plate of an annular on axis body, is provided at the inner wall position corresponding with support plate of second intercommunicating pore
One annular groove, the support plate are located in annular groove, and fixing sleeve is equipped on the axis body that the rotary shaft is located in the first intercommunicating pore
It is empty to be provided with the transmission that one extends to the right at the inner wall position corresponding with transmission gear of first intercommunicating pore for one transmission gear
Between, a driving space is internally provided on the right side of the transmission space upper end wall, the driving space interior is fixedly installed one
The lower end be connected by power of driving motor, the driving motor has a drive shaft, the lower end of the drive shaft to pass through driving space
It lower end wall and is fixedly connected in the lower end wall rotary type of transmission space, the drive shaft is located at fixed on the axis body in driving space
It is set with a rotate gear, the rotate gear is connected by meshing transmission with transmission gear, and the rotary shaft is located in reaction compartment
Axis body on be evenly distributed with multiple stirring rods, the circulation of integral structure is distributed with stirring rod internal circumference for the rotary shaft
Hole, the recirculation hole are connected to the first connected space and the second connected space, and the lower end of the seal casinghousing left end wall, which is fixed, to be connected
It is connected to a temperature-controlled box, the temperature-controlled box is internally provided with a temperature control space, is provided at the left end wall of second connected space
First water pipe, the first water pipe connection temperature control space and the second connected space, the interior lower end fixation in the temperature control space are set
It is equipped with a water pump, the water pump upper end is connected with the second water pipe, and the upper end of second water pipe extends to the right and is connected to the first company
Logical space, the middle position of the reaction compartment left end wall is embedded to be installed with a temperature inductor, and the reaction is empty
Between aft bulkhead upper end be provided with an automatically controlled feeding gate, the upper end of the seal casinghousing right side is connected with third water pipe, described
The left end of third water pipe extends into reaction compartment and is provided with and communicated with a water injection pipe to the left, and the water injection pipe is spirally coiled in instead
It answers in the upper end wall in space, and is evenly distributed with multiple high-pressure nozzles on the tube body of the water injection pipe, the third water pipe is located at
One control valve is housed on the tube body on the outside of seal casinghousing, the 4th water pipe is provided on the upside of the seal casinghousing right side, it is described
4th water pipe is connected to reaction compartment, and flow control valve, the reaction compartment right end are housed on the tube body of the 4th water pipe
The middle position of wall is embedded to be installed with a PH measuring appliances, and the lower end of the seal casinghousing front end face is provided with the 5th water
Pipe, the 5th water pipe are connected to reaction compartment, and a water discharging valve is housed on the tube body of the 5th water pipe, on the fixed bottom plate
It is installed with a liquid reserve tank on rear side of end face, is fixedly connected with the lower face of seal casinghousing on front side of the upper end of the liquid reserve tank,
The liquid reserve tank is internally provided with a liquid storage space, and the feed liquor of integral structure is provided on front side of the upper end wall of the liquid storage space
Hole, inlet opening connection liquid storage space month reaction compartment, the inlet opening are internally provided with the first solenoid valve, the liquid reserve tank
The lower end of rear end face is provided with and communicated with a hydraulic pump, and the hydraulic pump is connected with the 6th water pipe, the 6th water pipe it is upper
End extends forward the middle position for being connected to seal casinghousing rear end face, the 6th water pipe connection reaction compartment and hydraulic pump,
6th water pipe is internally provided with second solenoid valve, and a filter is installed on front side of the fixed bottom plate upper surface,
It is fixedly connected with the lower face of seal casinghousing on rear side of the upper end of the filter, is provided on front side of the reaction compartment lower end wall
One drainage hole, the drainage hole connection reaction compartment and filter, the drainage hole are internally provided with third solenoid valve.
It the described method comprises the following steps：
Automatically controlled feeding gate is opened, reaction compartment is added in suitable concentrated sulfuric acid and suitable sodium nitrite is added, heating is allowed to molten
Solution adds the nitroaniline of suitable cyano-containing after cooling, driving motor works at this time, and rotate gear is driven by drive shaft
Rotation drives stirring rod rotation by rotary shaft, completes the stirring of solution, realize reaction in the engagement of transmission gear
Diazotising in the process, after the completion of diazotising, the first solenoid valve is opened, and diazonium salt solution flows into liquid storage space by inlet opening,
It carries out spare, clear water is sprayed by reaction compartment by high-pressure nozzle, at this point, the first solenoid valve is closed, water discharging valve is opened, to
The chemicals washed away in reaction compartment are residual miscellaneous, ensure the progress of subsequent reactions, it is residual it is miscellaneous rinse well after, water discharging valve is closed, after
Continue and be filled with clear water in reaction compartment, open automatically controlled feeding gate, suitable aminobenzenesulfonic acid is added, then, it is molten that sodium carbonate is added
Liquid is allowed to dissolve, and after the completion of dissolving, the diazonium salt solution in liquid storage space is injected reaction compartment by hydraulic pump, is stirred
It mixes, completes coupling reaction, after the completion of reaction, be obtained by filtration the water-soluble dye of cyano-containing by filter, in reaction process, lead to
Temperature information inside excess temperature sensor measurement reaction compartment, and temperature information is fed back into water pump, to control plugman
Make, ensure the leakproofness of rotary shaft and the first connected space and the second connected space by sealing rubber plug, keeps the first connection empty
Interior water enters the second connected space by recirculation hole, is convenient for the exchange of heat, convenient for controlling the temperature inside reaction compartment,
So that the temperature of device is controlled sensitiveer, quick, realizes the temperature control inside reaction compartment, meet the temperature in reaction process
It is required that PH measuring appliances measure the PH information of liquid in reaction compartment, and information is fed back into flow control valve, to control carbonic acid
The injection rate of sodium solution adjusts the pH value of solution in reaction compartment, meets the PH requirements in reaction process, and the present invention passes through one
Device completes diazotising, the multiple reaction process of coupling reaction of cyano-containing water-soluble dye, and the equipment effectively saved makes
With quantity, resource is saved for the preparation of dyestuff.
Preferably, equal fixing sleeve is equipped with a sealing rubber plug, the sealing on the axis body of the rotary shaft upper and lower ends
The outer diameter of rubber stopper is fitted closely with the first connected space and the second connected space, and the recirculation hole is through rotary shaft and relatively
The stirring rod and the first connected space of connection answered and the second connected space.
Preferably, the electrically connected water pump of temperature inductor, the electrically connected flow control valve of PH measuring appliances, institute
It states the 4th water pipe right end and is connected with a sodium carbonate injection device.
Description of the drawings
Fig. 1 is the main structure diagram of the synthetic method entirety complete section of the water-soluble dye of a kind of cyano-containing of the present invention；
Fig. 2 is the left view structural representation of the synthetic method entirety complete section of the water-soluble dye of a kind of cyano-containing of the present invention；
Fig. 3 be the water-soluble dye of a kind of cyano-containing of the present invention synthetic method in water injection pipe arrangement schematic diagram.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
- 3 are please referred to Fig.1, a kind of embodiment provided by the invention：The synthetic method of the water-soluble dye of a kind of cyano-containing,
Including fixed bottom plate 1, the middle position of 1 upper surface of fixed bottom plate is provided with a support base 2, the support base 2 it is upper
End is fixedly installed a seal casinghousing 3, and the seal casinghousing 3 is internally provided with a reaction compartment 4, the reaction compartment 4
It is internally provided with the rotary shaft 5 of a vertical direction, 4 upper and lower ends pars intramuralis of reaction compartment position corresponding with rotary shaft 5
Place is respectively arranged with the first connected space 8 and the second connected space 9, and is provided at the lower end wall of first connected space 8
One intercommunicating pore 6, first intercommunicating pore 6 are connected to reaction compartment 4 and the first connected space 8, and the upper end of the rotary shaft 5 is across the
One intercommunicating pore 6 and the first connected space 8 is extended into, the second intercommunicating pore is provided at the upper end wall of second connected space 9
7, second intercommunicating pore 7 is connected to reaction compartment 4 and the second connected space 9, and the lower end of the rotary shaft 5 passes through the second intercommunicating pore
7 and the second connected space 9 is extended into, equal fixing sleeve is equipped with a sealing rubber plug on the axis body of 5 upper and lower ends of the rotary shaft
10, the rotary shaft 5 is located at support plate 12 of the fixing sleeve equipped with an annular on the axis body in the second intercommunicating pore 7, and described second connects
An annular groove 11 is provided at the inner wall of through-hole 7 position corresponding with support plate 12, the support plate 12 is located in annular groove 11,
The rotary shaft 5 is located at fixing sleeve on the axis body in the first intercommunicating pore 6 and one transmission gear 14 is housed, first intercommunicating pore 6
A transmission space 13 extended to the right, 13 upper end wall of the transmission space are provided at inner wall position corresponding with transmission gear 14
Right side be internally provided with a driving space 15, be fixedly installed a driving motor 16, the drive inside the driving space 15
The lower end be connected by power of dynamic motor 16 has a drive shaft 17, the lower end of the drive shaft 17 pass through the lower end wall in driving space 15 and
It is fixedly connected in the lower end wall rotary type of transmission space 13, the drive shaft 17 is located at fixing sleeve on the axis body in driving space 15
Equipped with a rotate gear 18, the rotate gear 18 is connected by meshing transmission with transmission gear 14, and it is empty that the rotary shaft 5 is located at reaction
Between be evenly distributed with multiple stirring rods 19 on axis body in 4, integral type is distributed with 19 internal circumference of stirring rod in the rotary shaft 5
The recirculation hole 20 of structure, the recirculation hole 20 are connected to the first connected space 8 and the second connected space 9, and the seal casinghousing 3 is left
The lower end of end wall is fixedly connected with a temperature-controlled box 21, and the temperature-controlled box 21 is internally provided with a temperature control space 22, and described second connects
The first water pipe 23 is provided at the left end wall in logical space 9, first water pipe 23 is connected to temperature control space 22 and the second connected space
9, the interior lower end in the temperature control space 22 is fixedly installed a water pump 24, and 24 upper end of the water pump is connected with the second water pipe 25,
The upper end of second water pipe 25 extends to the right and is connected to the first connected space 8, the centre position of 4 left end wall of the reaction compartment
Locate it is embedded be installed with a temperature inductor 45, the aft bulkhead upper end of the reaction compartment 4 is provided with an automatically controlled feeding gate
26, the upper end of 3 right side of the seal casinghousing is connected with third water pipe 27, and the left end of the third water pipe 27 extends into the left
Reaction compartment 4 and it being provided with and communicated with a water injection pipe 28, the water injection pipe 28 is spirally coiled in the upper end wall of reaction compartment 4, and
Multiple high-pressure nozzles 29 are evenly distributed on the tube body of the water injection pipe 28, the third water pipe 27 is located at 3 outside of seal casinghousing
Tube body on a control valve 30 is housed, be provided with the 4th water pipe 42, the 4th water pipe on the upside of 3 right side of the seal casinghousing
42 connection reaction compartments 4, and flow control valve 43,4 right end of the reaction compartment are housed on the tube body of the 4th water pipe 42
The middle position of wall is embedded to be installed with a PH measuring appliances 46, and the lower end of 3 front end face of the seal casinghousing is provided with
Five water pipes 31, the 5th water pipe 31 are connected to reaction compartment 4, a water discharging valve 32 are housed on the tube body of the 5th water pipe 31,
A liquid reserve tank 33, the upper end front side of the liquid reserve tank 33 and capsul are installed on rear side of 1 upper surface of fixed bottom plate
The lower face of body 3 is fixedly connected, and the liquid reserve tank 33 is internally provided with a liquid storage space 34,34 upper end wall of liquid storage space
Front side is provided with the inlet opening 35 of integral structure, and the inlet opening 35 is connected to the 34 months reaction compartments 4 in liquid storage space, the feed liquor
Hole 35 is internally provided with the first solenoid valve 36, and the lower end of 33 rear end face of the liquid reserve tank is provided with and communicated with a hydraulic pump 37, described
Hydraulic pump 37 is connected with the 6th water pipe 38, and the upper end of the 6th water pipe 38, which extends forward, is connected to 3 rear end of seal casinghousing
The middle position in face, the 6th water pipe 38 connection reaction compartment 4 and hydraulic pump 37, the 6th water pipe 38 are internally provided with
Second solenoid valve 44 is installed with a filter 39, the upper end of the filter 39 on front side of 1 upper surface of fixed bottom plate
Rear side is fixedly connected with the lower face of seal casinghousing 3, and a drainage hole 40, institute are provided on front side of 4 lower end wall of the reaction compartment
It states drainage hole 40 and is connected to reaction compartment 4 and filter 39, the drainage hole 40 is internally provided with third solenoid valve 41.
It the described method comprises the following steps：
Automatically controlled feeding gate 26 is opened, reaction compartment 4 is added in suitable concentrated sulfuric acid and suitable sodium nitrite is added, heating is allowed to
Dissolving adds the nitroaniline of suitable cyano-containing after cooling, driving motor 16 works at this time, by drive shaft 17 with turn
Moving gear 18 rotates, and in the engagement of transmission gear 14, drives stirring rod 19 to rotate by rotary shaft 5, completes solution
It stirs, the diazotising in realization reaction process, after the completion of diazotising, the first solenoid valve 36 is opened, and diazonium salt solution passes through feed liquor
Hole 35 flows into liquid storage space 34, and progress is spare, clear water is sprayed into reaction compartment by high-pressure nozzle 29, at this point, the first solenoid valve
36 close, and water discharging valve 32 is opened, residual miscellaneous to wash away the chemicals in reaction compartment 4, ensures the progress of subsequent reactions, residual miscellaneous
After rinsing well, water discharging valve 32 is closed, and continuation is filled with clear water in reaction compartment 4, opens automatically controlled feeding gate 26, is added appropriate
Aminobenzenesulfonic acid then sodium carbonate liquor is added and is allowed to dissolve, after the completion of dissolving, by hydraulic pump 37 by liquid storage space 34
Interior diazonium salt solution injects reaction compartment 4, is stirred, and completes coupling reaction, after the completion of reaction, is filtered by filter 39
It obtains the water-soluble dye of cyano-containing, in reaction process, passes through temperature inductor 45 and measure temperature letter inside reaction compartment 4
Breath, and temperature information is fed back into water pump 24, to control 24 water pumps 24 work, rotary shaft 5 is ensured by sealing rubber plug 10
With the leakproofness of the first connected space 8 and the second connected space 9, so that the water in the first connected space 8 is passed through recirculation hole 19 and enter
Second connected space 9 is convenient for the exchange of heat, convenient for the temperature inside control reaction compartment 4, the temperature of device is made to control more
It is sensitive, quick, it realizes the temperature control inside reaction compartment 4, meets the temperature requirement in reaction process, PH measuring appliances 46 measure
The PH information of liquid in reaction compartment 4, and information is fed back into flow control valve 43, to control the injection of sodium carbonate liquor
Amount adjusts the pH value of solution in reaction compartment 4, meets the PH requirements in reaction process, and the present invention is contained by a device completion
The diazotising of cyano water-soluble dye, multiple reaction process of coupling reaction, the usage quantity for the equipment effectively saved, for dye
The preparation of material saves resource.
Valuably, equal fixing sleeve is equipped with a sealing rubber plug 10, the sealing on the axis body of 5 upper and lower ends of the rotary shaft
The outer diameter of rubber stopper 10 is fitted closely with the first connected space 8 and the second connected space 9, and the recirculation hole 20 runs through rotary shaft
5 and corresponding stirring rod 19 and connection the first connected space 8 and the second connected space 9.Its effect is to pass through sealing rubber plug
10 ensure the leakproofness of rotary shaft 5 and the first connected space 8 and the second connected space 9, and the water in the first connected space 8 is made to pass through
Recirculation hole 19 enters the second connected space 9, is convenient for the exchange of heat, convenient for the temperature inside control reaction compartment 4, makes device
Temperature control is sensitiveer, quick.
Valuably, 45 electrically connected water pump 24 of the temperature inductor, 46 electrically connected flow control of the PH measuring appliances
Valve 43,42 right end of the 4th water pipe are connected with a sodium carbonate injection device.Its effect is measured instead by temperature inductor 45
The temperature information inside space 4 is answered, and temperature information is fed back into water pump 24, to control 24 water pumps 24 work, realizes reaction
Temperature control inside space 4, meets the temperature requirement in reaction process, and PH measuring appliances 46 measure liquid in reaction compartment 4
PH information, and information is fed back into flow control valve 43, to control the injection rate of sodium carbonate liquor, adjust in reaction compartment 4
The pH value of solution meets the PH requirements in reaction process.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Profit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent requirements of the claims
Variation is included within the present invention.Any reference signs in the claims should not be construed as limiting the involved claims.
Claims (3)
1. the synthetic method of the water-soluble dye of a kind of cyano-containing, including fixed bottom plate, it is characterised in that：On the fixed bottom plate
The middle position of end face is provided with a support base, and the upper end of the support base is fixedly installed a seal casinghousing, the sealing
Shell is internally provided with a reaction compartment, and the rotary shaft for being internally provided with a vertical direction of the reaction compartment is described anti-
It should spatially descend inside end walls and be respectively arranged with the first connected space and the second connected space at position corresponding with rotary shaft,
The first intercommunicating pore is provided at the lower end wall of first connected space, the first intercommunicating pore connection reaction compartment and first connect
The upper end in logical space, the rotary shaft passes through the first intercommunicating pore and extends into the first connected space, second connected space
Upper end wall at be provided with the second intercommunicating pore, the second intercommunicating pore connection reaction compartment and the second connected space, the rotation
The lower end of axis passes through the second intercommunicating pore and extends into the second connected space, fixed on the axis body of the rotary shaft upper and lower ends
It is set with a sealing rubber plug, the rotary shaft is located at support of the fixing sleeve equipped with an annular on the axis body in the second intercommunicating pore
Plate, an annular groove is provided at the inner wall position corresponding with support plate of second intercommunicating pore, and the support plate is located at annular
In slot, the rotary shaft is located at fixing sleeve on the axis body in the first intercommunicating pore and one transmission gear is housed, first intercommunicating pore
A transmission space extended to the right, the right side of the transmission space upper end wall are provided at inner wall position corresponding with transmission gear
It is internally provided with a driving space, the driving space interior is fixedly installed a driving motor, the lower end of the driving motor
Be connected by power has a drive shaft, the lower end of the drive shaft to pass through the lower end wall in driving space and turn in the lower end wall of transmission space
Dynamic formula is fixedly connected, and fixing sleeve is equipped with a rotate gear, the turning gear on the axis body that the drive shaft is located in driving space
Wheel is connected by meshing transmission with transmission gear, and multiple stirrings are evenly distributed on the axis body that the rotary shaft is located in reaction compartment
The recirculation hole of integral structure is distributed with stirring rod internal circumference for bar, the rotary shaft, and the recirculation hole is connected to the first company
Logical space and the second connected space, the lower end of the seal casinghousing left end wall are fixedly connected with a temperature-controlled box, in the temperature-controlled box
Portion is provided with a temperature control space, and the first water pipe, the first water pipe connection are provided at the left end wall of second connected space
The interior lower end of temperature control space and the second connected space, the temperature control space is fixedly installed a water pump, and the water pump upper end connects
It is connected to the second water pipe, the upper end of second water pipe extends to the right and be connected to the first connected space, the reaction compartment left end wall
Middle position it is embedded be installed with a temperature inductor, it is automatically controlled that the aft bulkhead upper end of the reaction compartment is provided with one
The upper end of feeding gate, the seal casinghousing right side is connected with third water pipe, and the left end of the third water pipe extends into the left
Reaction compartment and it is provided with and communicated with a water injection pipe, the water injection pipe is spirally coiled in the upper end wall of reaction compartment, and the note
Multiple high-pressure nozzles are evenly distributed on the tube body of water pipe, the third water pipe, which is located on the tube body on the outside of seal casinghousing, is equipped with one
Control valve is provided with the 4th water pipe on the upside of the seal casinghousing right side, and the 4th water pipe is connected to reaction compartment, and described
Flow control valve, the embedded fixed installation of middle position of the reaction compartment right end wall are housed on the tube body of the 4th water pipe
There are a PH measuring appliances, the lower end of the seal casinghousing front end face to be provided with the 5th water pipe, the 5th water pipe is connected to reaction compartment,
One water discharging valve is housed on the tube body of the 5th water pipe, a liquid storage is installed on rear side of the fixed bottom plate upper surface
The upper end front side of case, the liquid reserve tank is fixedly connected with the lower face of seal casinghousing, and the liquid reserve tank is internally provided with a liquid storage
Space is provided with the inlet opening of integral structure, inlet opening connection liquid storage space on front side of the upper end wall of the liquid storage space
Month reaction compartment, the inlet opening are internally provided with the first solenoid valve, and the lower end of the liquid reserve tank rear end face is provided with and communicated with one
Hydraulic pump, the hydraulic pump are connected with the 6th water pipe, and the upper end of the 6th water pipe, which extends forward, is connected to seal casinghousing
The middle position of rear end face, the 6th water pipe connection reaction compartment and hydraulic pump, the 6th water pipe are internally provided with the
Two solenoid valves, are installed with a filter on front side of the fixed bottom plate upper surface, on rear side of the upper end of the filter with it is close
The lower face of capsule body is fixedly connected, and a drainage hole, the drainage hole connection are provided on front side of the reaction compartment lower end wall
Reaction compartment and filter, the drainage hole are internally provided with third solenoid valve;
It the described method comprises the following steps：
Automatically controlled feeding gate is opened, reaction compartment is added in suitable concentrated sulfuric acid and suitable sodium nitrite is added, heating is allowed to molten
Solution adds the nitroaniline of suitable cyano-containing after cooling, driving motor works at this time, and rotate gear is driven by drive shaft
Rotation drives stirring rod rotation by rotary shaft, completes the stirring of solution, realize reaction in the engagement of transmission gear
Diazotising in the process, after the completion of diazotising, the first solenoid valve is opened, and diazonium salt solution flows into liquid storage space by inlet opening,
It carries out spare, clear water is sprayed by reaction compartment by high-pressure nozzle, at this point, the first solenoid valve is closed, water discharging valve is opened, to
The chemicals washed away in reaction compartment are residual miscellaneous, ensure the progress of subsequent reactions, it is residual it is miscellaneous rinse well after, water discharging valve is closed, after
Continue and be filled with clear water in reaction compartment, open automatically controlled feeding gate, suitable aminobenzenesulfonic acid is added, then, it is molten that sodium carbonate is added
Liquid is allowed to dissolve, and after the completion of dissolving, the diazonium salt solution in liquid storage space is injected reaction compartment by hydraulic pump, is stirred
It mixes, completes coupling reaction, after the completion of reaction, be obtained by filtration the water-soluble dye of cyano-containing by filter, in reaction process, lead to
Temperature information inside excess temperature sensor measurement reaction compartment, and temperature information is fed back into water pump, to control plugman
Make, ensure the leakproofness of rotary shaft and the first connected space and the second connected space by sealing rubber plug, keeps the first connection empty
Interior water enters the second connected space by recirculation hole, is convenient for the exchange of heat, convenient for controlling the temperature inside reaction compartment,
So that the temperature of device is controlled sensitiveer, quick, realizes the temperature control inside reaction compartment, meet the temperature in reaction process
It is required that PH measuring appliances measure the PH information of liquid in reaction compartment, and information is fed back into flow control valve, to control carbonic acid
The injection rate of sodium solution adjusts the pH value of solution in reaction compartment, meets the PH requirements in reaction process, and the present invention passes through one
Device completes diazotising, the multiple reaction process of coupling reaction of cyano-containing water-soluble dye, and the equipment effectively saved makes
With quantity, resource is saved for the preparation of dyestuff.
2. the synthetic method of the water-soluble dye of one kind cyano-containing according to claim 1, it is characterised in that：The rotation
Equal fixing sleeve is equipped with a sealing rubber plug, the outer diameter of the sealing rubber plug and the first connected space on the axis body of axis upper and lower ends
And second connected space fit closely, the recirculation hole through rotary shaft and corresponding stirring rod and the first connection of connection it is empty
Between with the second connected space.
3. the synthetic method of the water-soluble dye of one kind cyano-containing according to claim 1, it is characterised in that：The temperature
The electrically connected water pump of inductor, the electrically connected flow control valve of PH measuring appliances, the 4th water pipe right end are connected with a carbon
Sour sodium injection device.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810878515.XA CN108727856A (en) | 2018-08-03 | 2018-08-03 | The synthetic method of the water-soluble dye of a kind of cyano-containing |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109569365A (en) * | 2018-11-23 | 2019-04-05 | 黎庆佳 | A kind of food liquid detection pretreatment unit with agitating function |
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2018
- 2018-08-03 CN CN201810878515.XA patent/CN108727856A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109569365A (en) * | 2018-11-23 | 2019-04-05 | 黎庆佳 | A kind of food liquid detection pretreatment unit with agitating function |
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