Preparation method of 6-chloro-2, 4-dinitroaniline
阅读说明：本技术 一种6-氯-2,4-二硝基苯胺制备方法 (Preparation method of 6-chloro-2, 4-dinitroaniline ) 是由 阮煜翔 王凯 于 2019-10-29 设计创作，主要内容包括：本发明公开了一种6-氯-2,4-二硝基苯胺制备方法,a、将2,4-二硝基苯胺分散于盐酸和催化剂中进行打浆,其中盐酸的质量分数为1％～6％；b、往步骤a中的打浆物料中通入氯气进行氯化反应；c、往步骤b中的反应液中加入氯酸钠溶液继续进行氯化反应,其中氯酸钠溶液的质量分数为20％～40％；d、将步骤c中得到的反应液过滤,通过清洗装置将滤饼洗至pH值6.0～7.0,母液返回到步骤a中作为盐酸和催化剂循环套用,直至母液中氯化钠浓度达到饱和时,将母液排入废水处理系统；e、将步骤d中得到的滤饼投入至气流干燥机中干燥,得到2,4-二硝基-6-氯苯胺。本发明具有整体耗水量小、清洗效果好的优点。(The invention discloses a preparation method of 6-chloro-2, 4-dinitroaniline, comprising the following steps of a, dispersing 2, 4-dinitroaniline in hydrochloric acid and a catalyst for pulping, wherein the mass fraction of the hydrochloric acid is 1-6%; b. b, introducing chlorine into the pulping material in the step a to perform chlorination reaction; c. adding a sodium chlorate solution into the reaction liquid in the step b to continue chlorination reaction, wherein the mass fraction of the sodium chlorate solution is 20-40%; d. c, filtering the reaction liquid obtained in the step c, washing a filter cake to a pH value of 6.0-7.0 through a washing device, returning the mother liquid to the step a to be used as hydrochloric acid and a catalyst for cyclic application, and discharging the mother liquid into a wastewater treatment system until the concentration of sodium chloride in the mother liquid is saturated; e. and d, putting the filter cake obtained in the step d into an airflow dryer for drying to obtain the 2, 4-dinitro-6-chloroaniline. The invention has the advantages of small integral water consumption and good cleaning effect.)
1. A preparation method of 6-chloro-2, 4-dinitroaniline is characterized by comprising the following steps: the method comprises the following steps:
a. dispersing 2, 4-dinitroaniline in hydrochloric acid and a catalyst for pulping, wherein the mass fraction of the hydrochloric acid is 1-6%;
b. b, introducing chlorine into the pulping material in the step a to perform chlorination reaction;
c. adding a sodium chlorate solution into the reaction liquid in the step b to continue chlorination reaction, wherein the mass fraction of the sodium chlorate solution is 20-40%;
d. c, filtering the reaction liquid obtained in the step c, washing a filter cake to a pH value of 6.0-7.0 through a washing device, returning the mother liquid to the step a to be used as hydrochloric acid and a catalyst for cyclic application, and discharging the mother liquid into a wastewater treatment system until the concentration of sodium chloride in the mother liquid is saturated;
e. d, putting the filter cake obtained in the step d into an airflow dryer for drying to obtain 2, 4-dinitro-6-chloroaniline;
wherein, the cleaning device in the step d comprises a frame (1), a feeding box (2), a material collecting box (3) and a cleaning mechanism, the feeding box (2) is arranged at the upper part of the frame (1), the cleaning mechanism is arranged at the middle part of the frame (1), a blanking plate (4) is obliquely arranged below the feeding box (2), the blanking plate (4) is used for guiding filter cakes in the feeding box (2) to the cleaning mechanism, the material collecting box (3) is arranged below the cleaning mechanism, the cleaning mechanism comprises two belt wheels (5) which are horizontally and symmetrically arranged, a conveying belt (6) wound between the two belt wheels (5) and a cleaning driving piece (7) used for driving the belt wheels (5) to rotate, a plurality of cleaning grooves (8) are uniformly arranged on the conveying belt (6), filter cloth (9) is arranged in the cleaning grooves (8), and a spray cleaning mechanism is arranged above the conveying belt (6), the spraying mechanism is used for spraying water into the cleaning tank (8) to clean filter cakes, and an anti-splash part is further arranged between the spraying mechanism and the conveyor belt (6).
2. The process for preparing 6-chloro-2, 4-dinitroaniline according to claim 1, wherein: in the step a, the mass ratio of the 2, 4-dinitroaniline to the hydrochloric acid to the catalyst is 1: (3-4.9): (0.004-0.01).
3. The process for preparing 6-chloro-2, 4-dinitroaniline according to claim 1, wherein: in the step b, the chlorination temperature is controlled to be 25-40 ℃, and the chlorination time is 2-8 hours.
4. The process for preparing 6-chloro-2, 4-dinitroaniline according to claim 1, wherein: the spray rinsing mechanism comprises a spray rinsing box (10), a spray rinsing cavity (11) is arranged in the spray rinsing box (10), a plurality of spray rinsing grooves (12) communicated with the spray rinsing cavity (11) are formed in the lower end of the spray rinsing box (10), a spray rinsing driving piece (13) used for conveying cleaning water into the spray rinsing cavity (11) is arranged on the spray rinsing box (10), and a pressurizing part is arranged at each spray rinsing groove (12).
5. The process for preparing 6-chloro-2, 4-dinitroaniline according to claim 1, wherein: the splash-proof part comprises two fixing strips (14) which are symmetrically arranged on two sides of the inner wall of the rack (1) and splash-proof cloth (15) which is fixed between the two fixing strips (14), the upper end face of the splash-proof cloth (15) is attached to the lower end face of the spray washing box (10), and the lower end face of the splash-proof cloth (15) is attached to the upper end face of the conveyor belt (6).
6. The process according to claim 4 for the preparation of 6-chloro-2, 4-dinitroaniline, wherein: spray rinsing groove (12) are formed by two adjacent spray rinsing strip (16) intervals, pressure parts is including offering sliding chamber (17) on spray rinsing strip (16), sliding chamber (17) are linked together with spray rinsing groove (12), be equipped with pressurization slider (18) in sliding chamber (17), through a plurality of piece (19) elastic connection that reset between pressurization slider (18) and sliding chamber (17) inner wall, pressurization groove (20) have been seted up on pressurization slider (18) upper end right side, pressurization slider (18) top is equipped with connecting strip (21), sliding seal cooperation between terminal surface and pressurization groove (20) inner wall under connecting strip (21), interval formation is used for communicateing spray rinsing chamber (11) and connection passageway (22) of pressurization groove (20) between connecting strip (21) and spray rinsing strip (16).
7. The process according to claim 5, wherein the reaction mixture comprises the following components: conveyer belt (6) top is located spray rinsing mechanism right side and still is equipped with dewatering mechanism, dewatering mechanism is including removing water tank (23), it has except that water chamber (24) in water tank (23) to remove, remove water tank (23) lower extreme and offer a plurality of and remove that water chamber (24) are linked together remove basin (25), it is used for to removing water driving piece (26) of conveying gas in water chamber (24) to be equipped with on water tank (23), it fits in splashproof cloth (15) up end to remove water tank (23) lower terminal surface.
8. The process for preparing 6-chloro-2, 4-dinitroaniline according to claim 1, wherein: be equipped with water receiving tank (27) between two band pulleys (5), water receiving tank (27) are located conveyer belt (6), water receiving tank (28) have been seted up to water receiving tank (27) one side near the wiper mechanism, be equipped with many drain pipes (29) that are linked together with water receiving tank (28) on water receiving tank (27) lateral wall, the drain pipe (29) other end stretches out outside frame (1).
9. The process for preparing 6-chloro-2, 4-dinitroaniline according to claim 1, wherein: frame (1) interior slope is equipped with striker plate (30), blanking passageway (31) have between blanking plate (4) and striker plate (30), be equipped with in blanking passageway (31) and change rod (32), be equipped with on frame (1) and be used for the drive to change rod (32) pivoted blanking driving piece (33), it evenly is equipped with a plurality of feeding baffle (34) along its circumference direction on rod (32) to change, feeding chamber (35) have between two adjacent feeding baffle (34), when changeing rod (32) static, blanking passageway (31) are closed.
10. The process for preparing 6-chloro-2, 4-dinitroaniline according to claim 1, wherein: conveyer belt (6) are located and have connecting portion (36) between two adjacent washing tanks (8), connecting portion (26) outside all is equipped with toper convex part (37), still be equipped with in frame (1) a plurality of with connecting portion (36) intermittent type nature conflict complex sand grip (38), work as when connecting portion (36) contradict with sand grip (38), vibrations about conveyer belt (6).
Technical Field
The invention relates to the technical field of chemical industry, in particular to a preparation method of 6-chloro-2, 4-dinitroaniline.
Background
6-chloro-2, 4-dinitroaniline, also known as 2-chloro-4, 6-dinitroaniline, CAS number 3531-19-9, is an important dye intermediate, as a diazo component, mainly used for the synthesis of disperse blue 270, 264, 259, 125 and 130, etc., from which the disperse dyes produced are widely used in the printing and dyeing industry for synthetic fibers.
The concentration of hydrochloric acid used in the existing industrial production is higher, the cost is high, the number of circulated batches of mother liquor is small, the acid content of the mother liquor wastewater is high, in addition, the acid content in a filter cake is also high, the water consumption is high during washing, and the wastewater discharge is increased; the existing filter cake cleaning mode is immersion cleaning, if a large amount of filter cakes are cleaned simultaneously, the cleaning efficiency is low, the filter cakes are easy to mutually pollute, and the water consumption is high; if divide into the filter cake many copies and wash alone, then need intermittent type nature start and stop equipment in order to put the material, influence equipment life, waste time and energy, if need improve cleaning efficiency then prepare many cleaning equipment under this mode, manufacturing cost increases, and the manual operation of not being convenient for.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provide a method for preparing 6-chloro-2, 4-dinitroaniline.
The purpose of the invention can be realized by the following technical scheme: a preparation method of 6-chloro-2, 4-dinitroaniline comprises the following steps:
a. dispersing 2, 4-dinitroaniline in hydrochloric acid and a catalyst for pulping, wherein the mass fraction of the hydrochloric acid is 1-6%;
b. b, introducing chlorine into the pulping material in the step a to perform chlorination reaction;
c. adding a sodium chlorate solution into the reaction liquid in the step b to continue chlorination reaction, wherein the mass fraction of the sodium chlorate solution is 20-40%;
d. c, filtering the reaction liquid obtained in the step c, washing a filter cake to a pH value of 6.0-7.0 through a washing device, returning the mother liquid to the step a to be used as hydrochloric acid and a catalyst for cyclic application, and discharging the mother liquid into a wastewater treatment system until the concentration of sodium chloride in the mother liquid is saturated;
e. d, putting the filter cake obtained in the step d into an airflow dryer for drying to obtain 2, 4-dinitro-6-chloroaniline;
wherein, in step d belt cleaning device include frame, feeding case, collection workbin and wiper mechanism, frame upper portion is located to the feeding case, the wiper mechanism locates the frame middle part, feeding case below slope is equipped with the blanking board, the blanking board is used for drainage to the wiper mechanism with the filter cake of feeding incasement, the wiper mechanism below is located to the collection workbin, the wiper mechanism includes two band pulleys that the horizontal symmetry set up, around locating the conveyer belt between two band pulleys and being used for driving pulley pivoted washing driving piece, a plurality of washing tanks have evenly been seted up on the conveyer belt, be equipped with the filter cloth in the washing tank, the conveyer belt top is equipped with spray rinsing mechanism, spray rinsing mechanism is used for to spraying water in the washing tank in order to wash the filter cake, still be equipped with splashproof part between spray rinsing mechanism and the conveyer belt.
The working principle of the cleaning device is as follows: the cleaning driving part is started, the cleaning driving part drives the belt pulley to rotate, the belt pulley drives the conveying belt to rotate, a filter cake in the feeding box passes through a blanking plate to slide into a cleaning tank on the conveying belt and moves together along with the conveying belt, meanwhile, the cleaning mechanism sprays water into the cleaning tank to clean the filter cake, and when the cleaning tank rotates to the bottom along with the conveying belt, the filter cake in the cleaning tank drops to the material collecting box due to the action of gravity to be collected.
The invention adopts low-concentration hydrochloric acid, has small acid consumption and low cost, and the filter cake after the reaction liquid is filtered has low acid content, little water or alkali consumption during washing and reduced wastewater discharge; the sodium chloride content in the filtered mother liquor is low, the frequency of returning hydrochloric acid and the catalyst in the mother liquor for continuous cyclic application is greatly increased, resources are fully utilized, the acid content in the mother liquor wastewater which can not be recycled for application is low, and the energy-saving and emission-reducing benefits are remarkable; according to the invention, the cleaning device is provided with the cleaning tank, so that the position of the filter cake is relatively fixed when the filter cake is cleaned, the filter cake is not easy to flush out of the cleaning tank when the filter cake is flushed, and the filter cake is prevented from splashing everywhere when the filter cake is flushed; through the arrangement of the filter cloth, the waste water after the filter cake is washed can be discharged through the filter cloth, the waste water is prevented from polluting the
In the step a, the mass ratio of the 2, 4-dinitroaniline to the hydrochloric acid to the catalyst is 1: (3-4.9): (0.004-0.01).
In the step b, the chlorination temperature is controlled to be 25-40 ℃, and the chlorination time is 2-8 hours.
The spray rinsing mechanism comprises a spray rinsing box, a spray rinsing cavity is formed in the spray rinsing box, a plurality of spray rinsing grooves communicated with the spray rinsing cavity are formed in the lower end of the spray rinsing box, a spray rinsing driving piece used for conveying cleaning water to the spray rinsing cavity is arranged on the spray rinsing box, and a pressurizing part is arranged at each spray rinsing groove.
The splashproof part is located two fixed strips of frame inner wall both sides and is fixed in the splashproof cloth between two fixed strips including the symmetry, the terminal surface is laminated under the spray rinsing case to splashproof cloth up end, the terminal surface is laminated in the conveyer belt up end under the splashproof cloth.
The spray rinsing groove is formed by two adjacent spray rinsing strip intervals, the pressure part is including seting up the slip chamber on the spray rinsing strip, the slip chamber is linked together with the spray rinsing groove, the slip intracavity is equipped with the pressurization slider, through a plurality of elastic connection that reset between pressurization slider and the slip intracavity wall, the pressurization groove has been seted up on pressurization slider upper end right side, pressurization slider top is equipped with the connecting strip, sliding seal cooperation between terminal surface and the pressurization inslot wall under the connecting strip, the interval forms the interface channel who is used for communicateing spray rinsing chamber and pressurization groove between connecting strip and the spray rinsing strip.
The conveyer belt top is located spray rinsing mechanism right side and still is equipped with dewatering mechanism, dewatering mechanism is including removing the water tank, the dewatering chamber has in the dewatering tank, a plurality of dewatering grooves that are linked together with the dewatering chamber are seted up to the dewatering tank lower extreme, be equipped with the dewatering driving piece that is used for to the conveying gas in the dewatering chamber on the dewatering tank, terminal surface laminating in splashproof cloth up end under the dewatering tank.
A water receiving tank is arranged between the two belt wheels and is positioned in the conveying belt, a water receiving groove is formed in one side, close to the cleaning mechanism, of the water receiving tank, a plurality of drain pipes communicated with the water receiving groove are arranged on the side wall of the water receiving tank, and the other end of each drain pipe extends out of the rack.
The utility model discloses a blanking device, including frame, blanking board, feeding chamber, feeding baffle, feeding rod, blanking channel, feeding rod, blanking board, blanking channel, feeding rod, feeding chamber, feeding rod, blanking channel, blanking rod, feeding rod, blanking channel, feeding rod, blanking channel, blanking.
The conveyer belt is located and has connecting portion between two adjacent washing tanks, the connecting portion outside all is equipped with the toper convex part, still be equipped with a plurality ofly in the frame and the conflict complex sand grip of connecting portion intermittent type nature, work as when connecting portion contradict with the sand grip, the conveyer belt shakes from top to bottom.
Compared with the prior art, the invention has the advantages of small overall water consumption and good cleaning effect.
Drawings
FIG. 1 is a flow chart of the steps of the present invention.
FIG. 2 is a first schematic structural diagram of the cleaning apparatus of the present invention.
FIG. 3 is a second schematic structural view of the cleaning apparatus of the present invention.
Fig. 4 is a sectional view of the cleaning apparatus of the present invention.
Fig. 5 is a partial schematic view at a in fig. 4.
Fig. 6 is a partial schematic view at B in fig. 4.
Fig. 7 is a partial schematic view at C in fig. 4.
FIG. 8 is a schematic view of the structure of the material collecting box of the present invention.
FIG. 9 is a sectional view of the head box of the present invention.
Fig. 10 is a partial schematic view at D in fig. 9.
In the figure, 1, a frame; 2. a feeding box; 3. a material collecting box; 4. a blanking plate; 5. a pulley; 6. a conveyor belt; 7. cleaning the driving part; 8. a cleaning tank; 9. filtering cloth; 10. a spray washing tank; 11. a spray rinsing chamber; 12. a spray washing tank; 13. spray rinsing the drive member; 14. a fixing strip; 15. anti-splash cloth; 16. spraying and washing the strips; 17. a sliding cavity; 18. a pressurizing slider; 19. a reset member; 20. a pressurizing tank; 21. a connecting strip; 22. a connecting channel; 23. removing the water tank; 24. a water removal cavity; 25. a water removal tank; 26. a dewatering drive; 27. a water receiving tank; 28. a water receiving tank; 29. a drain pipe; 30. a striker plate; 31. a blanking channel; 32. rotating the stick; 33. a blanking driving member; 34. a feed baffle; 35. a feed cavity; 36. a connecting portion; 37. a tapered convex portion; 38. a convex strip; 39. pressurizing and punching the block; 40. reinforcing the strips; 41. a blanking sloping plate; 42. a water falling plate; 43. a water falling gap; 44. a spring; 45. a water falling hole; 46. a connecting rod; 47. a material receiving plate; 48. a waste water channel; 49. a box door; 50. a handle; 51. a second wastewater channel; 52. blocking strips; 53. an elastic member; 54. a resisting plate; 55. a movable cavity; 56. a top chamber; 57. a top block; 58. an air bag portion; 59. an air bag channel; 60. a limiting strip; 61. a limiting groove.
Detailed Description
The following are specific embodiments of the present invention and are further described with reference to the drawings, but the present invention is not limited to these embodiments.