CN109323590A - A kind of p-aminobenzene sulfonic acid solidifies the preparation method of indexable furnace and p-aminobenzene sulfonic acid - Google Patents
A kind of p-aminobenzene sulfonic acid solidifies the preparation method of indexable furnace and p-aminobenzene sulfonic acid Download PDFInfo
- Publication number
- CN109323590A CN109323590A CN201811272067.5A CN201811272067A CN109323590A CN 109323590 A CN109323590 A CN 109323590A CN 201811272067 A CN201811272067 A CN 201811272067A CN 109323590 A CN109323590 A CN 109323590A
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- Prior art keywords
- oil
- furnace
- pipe
- indexable
- high temperature
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- HVBSAKJJOYLTQU-UHFFFAOYSA-N 4-aminobenzenesulfonic acid Chemical compound NC1=CC=C(S(O)(=O)=O)C=C1 HVBSAKJJOYLTQU-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229950000244 sulfanilic acid Drugs 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 68
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000010438 heat treatment Methods 0.000 claims abstract description 33
- 238000003860 storage Methods 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000002485 combustion reaction Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 24
- 238000007711 solidification Methods 0.000 claims description 21
- 230000008023 solidification Effects 0.000 claims description 21
- 239000010410 layer Substances 0.000 claims description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- 239000012043 crude product Substances 0.000 claims description 11
- 238000002425 crystallisation Methods 0.000 claims description 11
- 239000000047 product Substances 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 9
- 238000004090 dissolution Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 230000008025 crystallization Effects 0.000 claims description 7
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 7
- BEHLMOQXOSLGHN-UHFFFAOYSA-N benzenamine sulfate Chemical class OS(=O)(=O)NC1=CC=CC=C1 BEHLMOQXOSLGHN-UHFFFAOYSA-N 0.000 claims description 6
- 230000018044 dehydration Effects 0.000 claims description 6
- 238000006297 dehydration reaction Methods 0.000 claims description 6
- 239000011229 interlayer Substances 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 238000004873 anchoring Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 239000000498 cooling water Substances 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 239000000428 dust Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- 238000011049 filling Methods 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 claims description 2
- 238000001727 in vivo Methods 0.000 claims description 2
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000011344 liquid material Substances 0.000 claims description 2
- 239000011490 mineral wool Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000004806 packaging method and process Methods 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 238000011027 product recovery Methods 0.000 claims description 2
- 230000008707 rearrangement Effects 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 claims description 2
- 238000010025 steaming Methods 0.000 claims description 2
- 230000005945 translocation Effects 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims 1
- 238000005096 rolling process Methods 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 5
- 238000013461 design Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 description 7
- 238000010586 diagram Methods 0.000 description 4
- 238000004534 enameling Methods 0.000 description 4
- 239000012452 mother liquor Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000006277 sulfonation reaction Methods 0.000 description 3
- 239000011449 brick Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000233855 Orchidaceae Species 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- UKJLNMAFNRKWGR-UHFFFAOYSA-N cyclohexatrienamine Chemical group NC1=CC=C=C[CH]1 UKJLNMAFNRKWGR-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011981 development test Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000007115 recruitment Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B17/00—Furnaces of a kind not covered by any preceding group
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D19/00—Arrangements of controlling devices
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D19/00—Arrangements of controlling devices
- F27D2019/0003—Monitoring the temperature or a characteristic of the charge and using it as a controlling value
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses the preparation methods that a kind of p-aminobenzene sulfonic acid solidifies indexable furnace and p-aminobenzene sulfonic acid, it is to be equipped with oil storage tank in the left side for solidifying indexable furnace, the upper end of oil storage tank is equipped with repairing tank, the right side of oil storage tank is equipped with heat-conducting oil furnace, the upper right side of heat-conducting oil furnace is equipped with low-temperature oil oil inlet pipe, the bottom righthand side of heat-conducting oil furnace is equipped with high temperature oil flowline, the bottom end of heat-conducting oil furnace is equipped with combustion chamber, solidify in the furnace body of indexable furnace and is from top to bottom successively arranged 10 row's loose rolls, the lower end of loose roll is equipped with high temperature oil heating tube, high temperature oil heating tube is set as the S type bend pipe of continuous bend, bend pipe is successively mounted on the lower end of loose roll by bolt, the upper end of loose roll is equipped with baking charging tray, the upper left side for solidifying indexable furnace rear end is equipped with aniline measuring tank and concentrated sulfuric acid measuring tank, the configuration of the present invention is simple, design is reasonable, it is low to process cost, system It is advanced to make technique, it is high-efficient.
Description
Technical field
The present invention relates to a kind of p-aminobenzene sulfonic acid production baking device, be specifically it is a kind of with heat-conducting oil furnace for heat
The special stainless steel in source solidifies the fabricating technology of indexable furnace and p-aminobenzene sulfonic acid.
Background technique
Solidification indexing apparatus is all using refractory material laying into heated brick bed type in the production of country's p-aminobenzene sulfonic acid at present
Sulfonation enameling furnace, the disadvantage is that take up a large area, using low, temperature does not increase the thermal efficiency.Before the heated brick bed type enameling furnace flue of a kang
It holds close to burner, causes head temperature high, tail end temperature is low, in order to balance stoving temperature substantially, needs three in a wheel baking
Secondary blowing out cooling, is baked in room by being manually entered, and drying charging tray is switched in front and back by hand, and manual operation large labor intensity bakes
Time is long, and is high-temperature operation, and furnace temperature is difficult to control.During normal operation, furnace temperature will generally carry out between 180-230 DEG C
Indexing dehydration, temperature range span is larger, and a wheel solidification indexing needs 5-6 hours.Not only yield is lower, unstable quality, and
Energy consumption is higher.
Summary of the invention
To overcome drawbacks described above, by research repeatedly and repeatedly inquiry investigation, although heat-conducting oil furnace is widely applied at present
In many industries of industrial circle, but without sulfonation enameling furnace that p-aminobenzene sulfonic acid uses.The reason is that although heat-conducting oil furnace is
The universal product, but all trades and professions must separately manufacture and design the dedicated of adaptation according to the product characteristics, performance, feature of oneself in use
After equipment is connected with heat-conducting oil furnace, it could use.Therefore, the applicant determines that voluntarily having developed a set of utilization conduction oil is heat source
Stainless steel solidifying indexing furnace.
The present inventor passes through a large amount of development test design, improve and perfect, is developed finally using p-aminobenzene sulfonic acid
Special stainless steel solidify indexable furnace, substitute former Adobe kang type sulfonation enameling furnace.On this basis, and through repetition test and summary,
Energy-saving and environment-friendly new production technology is formd, so as to complete the present invention.
It is an object of the invention to provide a kind of p-aminobenzene sulfonic acid stainless steels to solidify indexable furnace, to solve traditional adobe kang furnace
High consumption low energy and pollute the defect of environment, in favor of the update of plant produced equipment.
Another object of the present invention is just to provide the preparation method of p-aminobenzene sulfonic acid energy conservation and environmental protection new process, to promote
The technological progress of the industry.
Technical solution of the present invention includes solidifying indexable furnace, heat-conducting oil furnace, repairing tank, oil storage filling and reaction kettle, and structure is special
Point is to be equipped with oil storage tank in the left side for solidifying indexable furnace, and the bottom end of oil storage tank is equipped with chassis, and oil storage tank is mounted on pedestal by chassis
On, the outside of oil storage tank is equipped with upper bracket, and the upper end of upper bracket is equipped with repairing tank, and the right side of oil storage tank is equipped with heat-conducting oil furnace, storage
The left end of oil tank is equipped with oil inlet pipe, and oil inlet pipe is equipped with oil inlet valve, and the lower end of oil inlet pipe is equipped with oil-feed pump, the left end of oil-feed pump
Equipped with oil pump connecting tube, oil-feed pump is connected on oil inlet valve by oil pump connecting tube, and the upper end connection of oil inlet pipe is mounted on repairing
The left upper end of tank, the bottom righthand side of repairing tank are equipped with repairing pipe, and repairing pipe is equipped with upper valve, and the lower end connection of repairing pipe is mounted on
The upper end of heat-conducting oil furnace, the upper right side of repairing tank are equipped with upper exhaust pipe, and the downside of upper exhaust pipe is equipped with lower exhaust pipe, heat-conducting oil furnace
Upper right side be equipped with low-temperature oil oil inlet pipe, upper exhaust pipe right end connection is mounted on low-temperature oil oil inlet pipe, the right side of lower exhaust pipe
End connection is mounted on the exhaust-gas treatment pipeline of unit upper end, and the bottom righthand side of heat-conducting oil furnace is equipped with high temperature oil and goes out oil connecting pipe, high
The bottom righthand side that warm oil goes out oil connecting pipe is equipped with high temperature oil pump, and the upper end of high temperature oil pump is equipped with the fuel-displaced valve of high temperature oil, and high temperature oil goes out
The upper end of oil valve door be equipped with high temperature oil oil pipeline, the oil inlet and outlet of high temperature oil pump be connected to high temperature oil go out oil connecting pipe and
On high temperature oil oil pipeline, the left upper end for solidifying indexable furnace is equipped with low-temperature oil oil return pipe, and the lower end of low-temperature oil oil return pipe is equipped with height
Warm oil oil outlet branch pipe, low-temperature oil oil inlet pipe are mounted on low-temperature oil oil return pipe by upper flange connection, and high temperature oil oil pipeline is under
For flanged joint in high temperature oil oil outlet branch pipe, the bottom end of heat-conducting oil furnace is equipped with combustion chamber, and the left end of heat-conducting oil furnace is surveyed equipped with oil temperature
Warm instrument.The indexable furnace of the solidification is integrally set as cuboid, and shell is made interlayer body by 316L stainless steel plate, is equipped with rock in interlayer
Cotton insulating layer, the lower end for solidifying indexable furnace are equipped with pedestal, and the bottom end for solidifying indexable furnace is fixed on pedestal by anchoring bolt.
Solidify and be from top to bottom successively arranged 1-10 row's loose roll in the furnace body of indexable furnace, the indexable furnace body positioned at loose roll both ends is equipped with
Bearing, every row 5, loose roll is sequentially arranged on furnace body by bearing, and the lower end of loose roll is equipped with high temperature oil heating tube, high temperature oil
Heating tube is set as the S type bend pipe of continuous bend, and bend pipe is successively mounted on the lower end of loose roll by bolt, public away from loose roll 2-2.5
Divide and form one layer of heated baking system, the left end of high temperature oil heating tube is equipped with heating connecting tube, heats the left end connection of connecting tube
In high temperature oil oil outlet branch pipe, it is located at every layer of heating connecting tube and is equipped with high temperature oil control valve, the end of high temperature oil heating tube
Equipped with oil return connecting tube, the left end of oil return connecting tube is connected on low-temperature oil oil return pipe, is equipped with positioned at every layer of oil return connecting tube
The upper end of low temperature oil control valve, every row's loose roll is respectively equipped with baking charging tray.The baking charging tray is the bucket shape disk of cuboid, bucket
Shape disk is lain on the loose roll of every row, and disengaging can be slided arbitrarily on loose roll, and the outer end for toasting charging tray is equipped with knob.Solidification
The upper left side of indexable furnace rear end is equipped with aniline measuring tank and concentrated sulfuric acid measuring tank, and the lower end of measuring tank is equipped with reaction kettle, reaction kettle
Upper middle part be equipped with electric mixer, the bottom end of aniline measuring tank is equipped with aniline tank connecting tube, and the bottom end of concentrated sulfuric acid measuring tank is set
There is concentrated sulfuric acid tank connecting tube, aniline measuring tank and concentrated sulfuric acid measuring tank are connected to the upper end of reaction kettle, aniline by connecting tube respectively
Tank connecting tube is equipped with aniline control valve, and concentrated sulfuric acid tank connecting tube is equipped with concentrated sulfuric acid control valve, and the bottom end of reaction kettle is set
There is charge pipe, the middle part of charge pipe is equipped with control total valve, and the upper end for toasting charging tray is respectively equipped with feed pipe, and feed pipe connects respectively
It connects on charge pipe, the junction of feed pipe and charge pipe is respectively equipped with control valve, and the upper top for solidifying indexable furnace, which is equipped with, steams
Send out gas outlet pipe, the front end that every row toasts charging tray is respectively equipped with dodge gate, and the downside of dodge gate is equipped with pull ring, before furnace body in
Portion is equipped with furnace temperature temperature instrumentation.
The configuration of the present invention is simple, rationally, processing cost is low, and manufacture craft is advanced, high-efficient for design.
It is described in further detail with reference to the accompanying drawing.
Detailed description of the invention
Fig. 1 is to solidify indexable stokehold to regard structural schematic diagram；
Fig. 2 is drying charging tray schematic diagram；
Fig. 3 is to solidify indexable furnace overlooking structure diagram；
Fig. 4 is to solidify indexable furnace interior structural schematic diagram；
Fig. 5 is to solidify indexable furnace right side structural representation；
Fig. 6 is to solidify indexable furnace technology flow chart.
Specific embodiment
The left side for solidifying indexable furnace 24 shown in Fig. 1-5 is equipped with oil storage tank 1, and the bottom end of oil storage tank is equipped with chassis, oil storage
Tank is mounted on the base by chassis, and the outside of oil storage tank is equipped with upper bracket 4, and the upper end of upper bracket is equipped with repairing tank 6, oil storage tank
Right side is equipped with heat-conducting oil furnace 12, and the left end of oil storage tank is equipped with oil inlet pipe 5, and oil inlet pipe is equipped with oil inlet valve 3, the lower end of oil inlet pipe
Equipped with oil-feed pump 2, the left end of oil-feed pump is equipped with oil pump connecting tube, and oil-feed pump is connected on oil inlet valve by oil pump connecting tube, into
The upper end connection of oil pipe is mounted on the left upper end of repairing tank, and the bottom righthand side of repairing tank is equipped with repairing pipe 9, and repairing pipe is equipped with upper valve
Door 10, the lower end connection of repairing pipe are mounted on the upper end of heat-conducting oil furnace, and the upper right side of repairing tank is equipped with upper exhaust pipe 7, upper exhaust
The downside of pipe is equipped with lower exhaust pipe 8, and the upper right side of heat-conducting oil furnace is equipped with low-temperature oil oil inlet pipe 11, and the right end of upper exhaust pipe connects peace
On low-temperature oil oil inlet pipe, the right end connection of lower exhaust pipe 8 is mounted on the exhaust-gas treatment pipeline of unit upper end, heat-conducting oil furnace
Bottom righthand side be equipped with high temperature oil and go out oil connecting pipe 37, the bottom righthand side that high temperature oil goes out oil connecting pipe is equipped with high temperature oil pump 15, high temperature oil
The upper end of pump is equipped with the fuel-displaced valve 16 of high temperature oil, and the upper end of the fuel-displaced valve of high temperature oil is equipped with high temperature oil oil pipeline 17, high temperature oil
The oil inlet and outlet of pump is connected to high temperature oil and goes out on oil connecting pipe and high temperature oil oil pipeline, and the left upper end for solidifying indexable furnace is set
There is low-temperature oil oil return pipe 20, the lower end of low-temperature oil oil return pipe is equipped with high temperature oil oil outlet branch pipe 21, and low-temperature oil oil inlet pipe 11 is by upper method
19 connection of orchid is mounted on low-temperature oil oil return pipe, and high temperature oil oil pipeline 17 is connected to high temperature oil oil outlet branch pipe 21 by lower flange 18
On, the bottom end of heat-conducting oil furnace is equipped with combustion chamber 14, and the left end of heat-conducting oil furnace is equipped with oil temperature temperature instrumentation 13.The indexable furnace of the solidification
24 entirety are set as cuboid, and interlayer body is made by 316L stainless steel plate in shell, and rock wool heat-preservation layer 36, solidification indexing are equipped in interlayer
The lower end of furnace is equipped with pedestal 35, and the bottom end for solidifying indexable furnace is fixed on pedestal by anchoring bolt.Solidify the furnace of indexable furnace
It is from top to bottom successively arranged 1-10 row's loose roll 32 in vivo, the indexable furnace body positioned at loose roll both ends is equipped with bearing 25, every row 5
A, loose roll is sequentially arranged on furnace body by bearing, and the lower end of loose roll is equipped with high temperature oil heating tube 33, and high temperature oil heating tube is set
For the S type bend pipe of continuous bend, bend pipe is successively mounted on the lower end of loose roll by bolt 31, away from 2-2.5 centimeters of loose roll, is formed
One layer of heated baking system, the left end of high temperature oil heating tube are equipped with heating connecting tube, and the left end for heating connecting tube is connected to high temperature
In oily oil outlet branch pipe 21, it is located at every layer of heating connecting tube and is equipped with high temperature oil control valve 22, the end of high temperature oil heating tube is set
There is oil return connecting tube, the left end of oil return connecting tube is connected on low-temperature oil oil return pipe 20, is equipped with positioned at every layer of oil return connecting tube
Low temperature oil control valve 23, the upper end of every row's loose roll are respectively equipped with baking charging tray 29.The baking charging tray is the bucket shape of cuboid
Disk, bucket shape disk are lain on the loose roll of every row, and disengaging can be slided arbitrarily on loose roll, and the outer end for toasting charging tray is equipped with knob
30.The upper left side for solidifying indexable furnace rear end is equipped with aniline measuring tank 38 and concentrated sulfuric acid measuring tank 39, and the lower end of measuring tank is equipped with anti-
Kettle 42 is answered, the upper middle part of reaction kettle is equipped with electric mixer 43, and the bottom end of aniline measuring tank is equipped with aniline tank connecting tube, the concentrated sulfuric acid
The bottom end of measuring tank is equipped with concentrated sulfuric acid tank connecting tube, and aniline measuring tank is connected to by connecting tube respectively with concentrated sulfuric acid measuring tank to react
The upper end of kettle, aniline tank connecting tube are equipped with aniline control valve 40, and concentrated sulfuric acid tank connecting tube is equipped with concentrated sulfuric acid control valve
41, the bottom end of reaction kettle is equipped with charge pipe 44, and the middle part of charge pipe is equipped with control total valve 45, and the upper end for toasting charging tray is set respectively
There is feed pipe 46, feed pipe is connected on charge pipe, and the junction of feed pipe and charge pipe is respectively equipped with hierarchical control valve
Door 47, the upper top for solidifying indexable furnace are equipped with boil-off gas discharge pipe 26, and the front end of every layer of baking charging tray is respectively equipped with dodge gate
27, the downside of dodge gate is equipped with pull ring 28, and the front middle part of furnace body is equipped with furnace temperature temperature instrumentation 34.
It is following (referring to Fig. 1) that stainless steel solidifies indexable furnace operation operating process:
Oil inlet valve 3 is opened, starting oil pump 2 fills in 6 to repairing and inputs conduction oil, is then turned on valve 10, flows into conduction oil
In heat-conducting oil furnace 12, after reaching setting oil level, the combustion chamber of heat-conducting oil furnace bottom end is lighted, is heated to heat-conducting oil furnace, oil temperature is improved.
While the above operation, it is first 93% sulfuric acid by concentration, is added in concentrated sulfuric acid measuring tank 39 (referring to fig. 4), weighs
21.75 tons, concentrated sulfuric acid control valve 41 is opened, is put into reaction kettle 42, then aniline measuring tank 38 is added in the aniline of concentration 99%
Interior, weigh 19.2 tons, it is 1:1 that the weight ratio of aniline and the concentrated sulfuric acid is 1:1.133(originally), slightly unlatching aniline control valve 40,
It allows aniline to be slowly added dropwise in reaction kettle 42, after dripping, closes aniline control valve 40, concentrated sulfuric acid control valve 41, starting
Electric mixer 43, is mixed and stirs evenly, and using physical reactions heat, after temperature rises to 170-180 DEG C, continues to stir
It 20 minutes, allows the concentrated sulfuric acid and aniline sufficiently to react and generates anilinesulfonic acid salt.
Aniline and concentrated sulfuric acid weight ratio are changed to 1:1.133 by original 1:1, bring the effect to be to reaction process: having reacted
Entirely, output ratio is improved.
It is total to open control below reaction kettle 42 when oil temperature is up to 200 degree for the temperature instrumentation 13 for observing 12 left end of heat-conducting oil furnace
Valve 45 and sandwich valve 47 are from top to bottom sequentially placed into liquid aniline sulfonate in the indexable charging tray 29 of solidification along charge pipe 44
Until (totally ten up and down, illustrate 5) pile.The fuel-displaced valve 16 of high temperature oil is opened, high temperature oil pump 15 is opened, hot oil along thermally conductive
Oily high temperature oil oil pipeline 17 inputs high temperature oil oil outlet branch pipe 21, is pumped into the high temperature oil heating pipe 33 solidified in indexable furnace,
High temperature oil is heat cycles one week in the continuous S type bend pipe in furnace, while heating, carries out solidification indexing.It is then turned on low temperature
Low-temperature oil after using is back in heat-conducting oil furnace 12 and heats again by oil control valve 23.
In continuous operation due to high temperature evaporation etc., reduce oil mass.At this point, opening valve 10 on repairing pipe, lead to
The repairing into heat-conducting oil furnace 12 of overfill oil tank 6 guarantees that conduction oil recycles heating, the gas generated when heating in operation in systems
Entered in repairing tank by upper exhaust pipe 7, the gas in repairing tank after the separation of upper layer is discharged by lower exhaust pipe 8, through exhaust-gas treatment
Pipeline introduces emission-control equipment.Observation solidifies the temperature instrumentation 34 of indexable furnace body front middle part, when temperature rises to 260 DEG C ± 3
Shi Jinhang truce thermal relief is stablized, and keeps the temperature 1 hour, with thoroughly indexing and solidification, generates p-aminobenzene sulfonic acid crude product.
The translocation reaction is molecular rearrangement --- refer to that a kind of quality of object and form are determined by molecule, molecule
Arrangement architecture change, so as to cause the variation of mass of object and form.
Solidification indexing terminates, and first closes high temperature oil control valve 22, turns off low-temperature oil control valve 23, conduction oil is made to exist
Second layer circular heating.The dodge gate 27 at indexable stokehold end is opened, drying charging tray knob 30 is pulled, pulls out charging tray through loose roll 32
Overturn discharging.Then it reinstalls charging tray and rejoins anilinesulfonic acid liquid material, resolidification indexing is recycled with this.Solidifying indexable process
In, the gas outlet pipe road 26 that the gas evaporated passes through indexable furnace top is discharged, and tail vapour processing system is introduced, at water injection
Reason, (ten layers) solidification index times of wheel shorten to complete for 4 hours.
Crude product crushes: by p-aminobenzene sulfonic acid bulk crude product, the graininess that crusher is ground into 1-10 mesh is rolled with double roller,
The tail gas for crushing release is trapped with dust collector simultaneously；
Crude product dissolution: smashed p-aminobenzene sulfonic acid crude product is closed with screw conveyor and is sent into dissolution kettle, water is added to mix
At solution, the weight ratio of water and p-aminobenzene sulfonic acid is 10:5.6, then activated carbon is added by the weight 0.8 ‰ -3 ‰ of solution,
It is heated by steam, maintains the temperature at 80-100 DEG C and keep stirring, p-aminobenzene sulfonic acid sufficiently dissolves, and is taken off by activated carbon adsorption
Color；
Filter: the p-aminobenzene sulfonic acid solution of dissolution decoloration be put into vacuumfilter and filter, make active carbon in solution and
Other impurity filter out, and obtain purer p-aminobenzene sulfonic acid solution；
Crystallization, centrifugation: filtered filtrate is entered into crystallization kettle, crystallization kettle is cooling with recirculated cooling water, and cooling temperature is at 30 DEG C
Hereinafter, crystallisation by cooling under constant stirring, the mixture after crystallisation by cooling is put into centrifuge dehydration, and dewatered product is essence
P-aminobenzene sulfonic acid processed；
Steam drying: p-aminobenzene sulfonic acid product is obtained by filtration in centrifugal dehydration, and the interior moisture containing 2.0% steam enters back into steaming
Vapour dries hopper, is dried, and controls drying time 10-13 minutes, is dried to moisture < 0.5%, makes product recovery rate up to 99%,
Product purity is up to 99.5%；
It weighs, packaging, storage.
Regenerated carbon is made through high-temperature activation in the active carbon containing a small amount of waste residue after suction filtration.
The mother liquor that centrifugal dehydration goes out contains 7% or so p-aminobenzene sulfonic acid, and backspace solution kettle is for dissolving crude product, mother liquor
After being used repeatedly, remaining impurity concentration increase will directly influence product quality, need that mother liquor is concentrated, then
Crystallization, filtering, then filter cake is reverse back to dissolution kettle, remaining mother liquor, concentration generates the residual object of kettle, and the residual object of kettle is mainly p-aminophenyl
Condensed water is concentrated in the same molecule allosome works of sulfonic acid and a small amount of sulfate, and recycling to dissolution kettle is recycled.
Conduction oil solidifies indexable furnace and the advance of new process is:
1, compared with former furnace, reduce recruitment and labor intensity, improve operating environment, it is therefore prevented that run, drip, leak are realized clear
Clean production reaches environmentally friendly purpose；
2, compared with when coal-burning boiler is heat source, the thermal energy of liquid phase conveying is at 300 DEG C, compared with water vapour vapour pressure less than 70 times, because
This, can run at lower pressures, obtain higher temperature；
3, stable heating and the control of accurate temperature can be carried out, to stabilize and increase product quality；
4, compared with former furnace, a wheel solidification indexing is saved time 1.5-2 hours, and whole energy saving 35%；
5, with complete operation control and safety monitoring assembly, to realize successional safety in production；
6, due to the improvement and equipment update of two kinds of raw material adding manners, it is therefore prevented that run, drip, leak and the indexable temperature of solidification
Raising and relatively accurate control, so that the output ratio of raw material and finished product is increased to 1:1.90- by original 1:1.65-1.70
1.95, output ratio is integrally improved 25%.
Claims (7)
1. a kind of p-aminobenzene sulfonic acid solidifies indexable furnace, including solidifies indexable furnace, heat-conducting oil furnace, repairing tank, oil storage filling and reaction
Kettle, it is characterised in that: the left side for solidifying indexable furnace (24) is equipped with oil storage tank (1), and the bottom end of oil storage tank is equipped with chassis, oil storage
Tank is mounted on the base by chassis, and the outside of oil storage tank is equipped with upper bracket (4), and the upper end of upper bracket is equipped with repairing tank (6), oil storage
The right side of tank is equipped with heat-conducting oil furnace (12), and the left end of oil storage tank is equipped with oil inlet pipe (5), and oil inlet pipe is equipped with oil inlet valve (3), into
The lower end of oil pipe is equipped with oil-feed pump (2), and the left end of oil-feed pump is equipped with oil pump connecting tube, oil-feed pump by oil pump connecting tube be connected into
On oil valve door, the upper end connection of oil inlet pipe is mounted on the left upper end of repairing tank, and the bottom righthand side of repairing tank is equipped with repairing pipe (9), mends
Oil pipe is equipped with upper valve (10), and the lower end connection of repairing pipe is mounted on the upper end of heat-conducting oil furnace, and the upper right side of repairing tank is equipped with
The downside of upper exhaust pipe (7), upper exhaust pipe is equipped with lower exhaust pipe (8), and the upper right side of heat-conducting oil furnace is equipped with low-temperature oil oil inlet pipe
(11), the right end connection of upper exhaust pipe is mounted on low-temperature oil oil inlet pipe, and the right end connection of lower exhaust pipe (8) is mounted on unit
On the exhaust-gas treatment pipeline at end, the bottom righthand side of heat-conducting oil furnace is equipped with high temperature oil and goes out oil connecting pipe (37), and high temperature oil goes out oil connecting pipe
Bottom righthand side be equipped with high temperature oil pump (15), the upper end of high temperature oil pump is equipped with the fuel-displaced valve of high temperature oil (16), the fuel-displaced valve of high temperature oil
Upper end be equipped with high temperature oil oil pipeline (17), the oil inlet and outlet of high temperature oil pump is connected to high temperature oil and goes out oil connecting pipe and height
On warm oil oil pipeline.
2. p-aminobenzene sulfonic acid according to claim 1 solidifies indexable furnace, it is characterised in that: the left side for solidifying indexable furnace
Upper end is equipped with low-temperature oil oil return pipe (20), and the lower end of low-temperature oil oil return pipe is equipped with high temperature oil oil outlet branch pipe (21), low-temperature oil oil inlet
Pipe (11) is mounted on low-temperature oil oil return pipe by upper flange (19) connection, and high temperature oil oil pipeline (17) is connected by lower flange (18)
On high temperature oil oil outlet branch pipe (21), the bottom end of heat-conducting oil furnace is equipped with combustion chamber (14), and the left end of heat-conducting oil furnace is surveyed equipped with oil temperature
Warm instrument (13), the indexable furnace (24) of the solidification are integrally set as cuboid, and interlayer body, interlayer is made by 316L stainless steel plate in shell
Interior to be equipped with rock wool heat-preservation layer (36), the lower end for solidifying indexable furnace is equipped with pedestal (35), solidifies the bottom end of indexable furnace by anchoring bolt
It is fixed on pedestal.
3. p-aminobenzene sulfonic acid according to claim 1 solidifies indexable furnace, it is characterised in that: the furnace for solidifying indexable furnace
It is from top to bottom successively arranged 1-10 row loose roll (32) in vivo, the indexable furnace body positioned at loose roll both ends is equipped with bearing (25),
Every row 5, loose roll is sequentially arranged on furnace body by bearing, and the lower end of loose roll is equipped with high temperature oil heating tube (33), high temperature oil
Heating tube is set as the S type bend pipe of continuous bend, and bend pipe is successively mounted on the lower end of loose roll by bolt (31), away from loose roll 2-
2.5 centimeters, form one layer of heated baking system.
4. p-aminobenzene sulfonic acid according to claim 3 solidifies indexable furnace, it is characterised in that: the high temperature oil heating tube
Left end is equipped with heating connecting tube, and the left end for heating connecting tube is connected on high temperature oil oil outlet branch pipe (21), is located at every layer of heating and connects
Adapter tube is equipped with high temperature oil control valve (22), and the end of high temperature oil heating tube is equipped with oil return connecting tube, a left side for oil return connecting tube
End is connected on low-temperature oil oil return pipe (20), is located at every layer of oil return connecting tube and is equipped with low temperature oil control valve (23), every row is servo-actuated
The upper end of roller is respectively equipped with baking charging tray (29).
5. p-aminobenzene sulfonic acid according to claim 4 solidifies indexable furnace, it is characterised in that: the baking charging tray is rectangular
The bucket shape disk of body, bucket shape disk are lain on the loose roll of every row, and the outer end for toasting charging tray is equipped with knob (30).
6. p-aminobenzene sulfonic acid according to claim 1 solidifies indexable furnace, it is characterised in that: the solidification indexable furnace rear end
Upper left side be equipped with aniline measuring tank (38) and concentrated sulfuric acid measuring tank (39), the lower end of measuring tank is equipped with reaction kettle (42), reaction
The upper middle part of kettle is equipped with electric mixer (43), and the bottom end of aniline measuring tank is equipped with aniline tank connecting tube, concentrated sulfuric acid measuring tank
Bottom end is equipped with concentrated sulfuric acid tank connecting tube, and aniline measuring tank is connected to the upper of reaction kettle by connecting tube respectively with concentrated sulfuric acid measuring tank
End, aniline tank connecting tube are equipped with aniline control valve (40), and concentrated sulfuric acid tank connecting tube is equipped with concentrated sulfuric acid control valve (41),
The bottom end of reaction kettle is equipped with charge pipe (44), and the middle part of charge pipe is equipped with control total valve (45), toasts the upper end difference of charging tray
Equipped with feed pipe (46), feed pipe is connected on charge pipe, and the junction of feed pipe and charge pipe is respectively equipped with layering control
Valve (47) processed, the upper top for solidifying indexable furnace are equipped with boil-off gas discharge pipe (26), and the front end of every layer of baking charging tray is set respectively
Have dodge gate (27), the downside of dodge gate is equipped with pull ring (28), and the front middle part of furnace body is equipped with furnace temperature temperature instrumentation (34).
7. a kind of preparation manipulation method of p-aminobenzene sulfonic acid, it is characterised in that: preparation manipulation method is as follows:
It opens oil inlet valve (3), starting oil pump (2) fills to repairing and inputs conduction oil in (6), is then turned on valve (10), makes to lead
Hot oil flows into heat-conducting oil furnace (12), after reaching setting oil level, lights the combustion chamber of heat-conducting oil furnace bottom end, improves oil temperature；
While the above operation, it is first 93% sulfuric acid by concentration, is added in concentrated sulfuric acid measuring tank (39), weighs 21.75 tons, beat
Concentrated sulfuric acid control valve (41) are opened, are put into reaction kettle (42), then 99% aniline is added in aniline measuring tank (38), are weighed
19.2 tons, it is 1:1 that the weight ratio of aniline and the concentrated sulfuric acid is 1:1.133(originally), slightly unlatching aniline control valve (40) allows aniline
It is slowly added dropwise in reaction kettle (42), after dripping, closes aniline control valve (40), concentrated sulfuric acid control valve (41), starting
Electric mixer (43), is mixed and stirs evenly, and using physical reactions heat, after temperature rises to 170-180 DEG C, continues to stir
It mixes 20 minutes, allows the concentrated sulfuric acid and stupid amine sufficiently to react and generate anilinesulfonic acid salt；
Aniline and concentrated sulfuric acid weight ratio are changed to 1:1.133 by original 1:1, and bring the effect to be to reaction process: fully reacting mentions
High output ratio；
The temperature instrumentation (13) for observing heat-conducting oil furnace (12) left end opens reaction kettle (42) lower section when oil temperature is up to 200 degree or so
Total valve (45) and sandwich valve (47) are controlled, liquid aniline sulfonate is sequentially placed into solidification along charge pipe (44) from top to bottom
It until being piled in indexable charging tray (29), opens the fuel-displaced valve of high temperature oil (16), opens high temperature oil pump (15), hot oil along conduction oil
High temperature oil oil pipeline (17) inputs high temperature oil oil outlet branch pipe (21), is pumped into the high temperature oil heating pipe (33) solidified in indexable furnace
In, make high temperature oil heat cycles one week in the continuous S type bend pipe in furnace, while heating, carries out solidification indexing, be then turned on
Low-temperature oil after using is back in heat-conducting oil furnace (12) and heats again by low temperature oil control valve (23)；
In continuous operation due to high temperature evaporation etc., oil mass is reduced, at this point, opening valve (10) on repairing pipe, passed through
Repairing tank (6) guarantees that conduction oil recycles heating, the gas generated when heating in operation in systems to heat-conducting oil furnace (12) interior repairing
Body is entered in repairing tank by upper exhaust pipe (7), and the gas in repairing tank after the separation of upper layer is discharged by lower exhaust pipe (8), through useless
Gas disposal pipeline introduces emission-control equipment, and observation solidifies the temperature instrumentation (34) of indexable furnace body front middle part, when temperature rises to
Truce thermal relief is carried out when 260 DEG C ± 3 to stablize, keeps the temperature 1 hour, with thoroughly indexing and solidification, generates p-aminobenzene sulfonic acid crude product；
The translocation reaction is molecular rearrangement --- refer to that a kind of quality of object and form are determined by molecule, the row of molecule
Array structure changes, so as to cause the variation of mass of object and form；
Solidification indexing terminates, and first closes high temperature oil control valve (22), turns off low-temperature oil control valve (23), conduction oil is made to exist
Second layer circular heating opens the dodge gate (27) at indexable stokehold end, pulls drying charging tray knob (30), draws through loose roll (32)
Discharge port plate overturns discharging, then reinstalls charging tray and rejoins anilinesulfonic acid liquid material, and resolidification indexing is recycled with this, is turned in solidification
During position, the gas evaporated passes through gas outlet pipe road (26) discharge on indexable furnace top, introduces tail vapour processing system, warp
Water injection processing, (ten layers) solidification index times of wheel shorten to complete for 4 hours；
Crude product crushes: by p-aminobenzene sulfonic acid bulk crude product, rolling the graininess that crusher is ground into 1-10 mesh with double roller, simultaneously
The tail gas for crushing release is trapped with dust collector；
Crude product dissolution: smashed p-aminobenzene sulfonic acid crude product is closed with screw conveyor and is sent into dissolution kettle, water is added to mix
At solution, the weight ratio of water and p-aminobenzene sulfonic acid is 10:5.6, then activated carbon is added by the weight 0.8 ‰ -3 ‰ of solution,
It is heated by steam, maintains the temperature at 80-100 DEG C and keep stirring, p-aminobenzene sulfonic acid sufficiently dissolves, and is taken off by activated carbon adsorption
Color；
Filter: the p-aminobenzene sulfonic acid solution of dissolution decoloration be put into vacuumfilter and filter, make active carbon in solution and
Other impurity filter out, and obtain purer p-aminobenzene sulfonic acid solution；
Crystallization, centrifugation: filtered filtrate is entered into crystallization kettle, crystallization kettle is cooling with recirculated cooling water, and cooling temperature is at 30 DEG C
Hereinafter, crystallisation by cooling under constant stirring, the mixture after crystallisation by cooling is put into centrifuge dehydration, and dewatered product is essence
P-aminobenzene sulfonic acid processed；
Steam drying: p-aminobenzene sulfonic acid product is obtained by filtration in centrifugal dehydration, and the interior moisture containing 2.0% steam enters back into steaming
Vapour dries hopper, is dried, and controls drying time 10-13 minutes, is dried to moisture < 0.5%, makes product recovery rate up to 99%,
Product purity is up to 99.5%；
It weighs, packaging, storage.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113121392A (en) * | 2019-12-30 | 2021-07-16 | 上海合丽亚化工科技有限公司 | Aminobenzene sulfonic acid compound crystal particles and preparation method thereof |
| CN116715607A (en) * | 2023-06-08 | 2023-09-08 | 浙江宏达化学制品有限公司 | Method for synthesizing sulfanilic acid |
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| JPS5690053A (en) * | 1979-12-24 | 1981-07-21 | Sumitomo Chem Co Ltd | Preparation of 1,4-diaminoanthraquinone-2-sulfonic acid |
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| CN113121392A (en) * | 2019-12-30 | 2021-07-16 | 上海合丽亚化工科技有限公司 | Aminobenzene sulfonic acid compound crystal particles and preparation method thereof |
| CN113121392B (en) * | 2019-12-30 | 2022-06-10 | 上海合丽亚化工科技有限公司 | Aminobenzene sulfonic acid compound crystal particles and preparation method thereof |
| CN116715607A (en) * | 2023-06-08 | 2023-09-08 | 浙江宏达化学制品有限公司 | Method for synthesizing sulfanilic acid |
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