CN112794808A - Tu's acid kettle type continuous disulfonation process and device - Google Patents
Tu's acid kettle type continuous disulfonation process and device Download PDFInfo
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- CN112794808A CN112794808A CN202110149899.3A CN202110149899A CN112794808A CN 112794808 A CN112794808 A CN 112794808A CN 202110149899 A CN202110149899 A CN 202110149899A CN 112794808 A CN112794808 A CN 112794808A
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- tobias acid
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- disulfonation
- acid
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- 238000000034 method Methods 0.000 title claims abstract description 19
- 230000008569 process Effects 0.000 title claims abstract description 16
- 239000002253 acid Substances 0.000 title description 11
- GWIAAIUASRVOIA-UHFFFAOYSA-N 2-aminonaphthalene-1-sulfonic acid Chemical compound C1=CC=CC2=C(S(O)(=O)=O)C(N)=CC=C21 GWIAAIUASRVOIA-UHFFFAOYSA-N 0.000 claims abstract description 81
- 238000006277 sulfonation reaction Methods 0.000 claims abstract description 41
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 11
- 230000007062 hydrolysis Effects 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims description 26
- HIFJUMGIHIZEPX-UHFFFAOYSA-N sulfuric acid;sulfur trioxide Chemical compound O=S(=O)=O.OS(O)(=O)=O HIFJUMGIHIZEPX-UHFFFAOYSA-N 0.000 claims description 13
- 238000005192 partition Methods 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 23
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000000376 reactant Substances 0.000 abstract description 2
- 238000011056 performance test Methods 0.000 abstract 1
- 239000000543 intermediate Substances 0.000 description 9
- KYARBIJYVGJZLB-UHFFFAOYSA-N 7-amino-4-hydroxy-2-naphthalenesulfonic acid Chemical compound OC1=CC(S(O)(=O)=O)=CC2=CC(N)=CC=C21 KYARBIJYVGJZLB-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- JBIJLHTVPXGSAM-UHFFFAOYSA-N 2-naphthylamine Chemical compound C1=CC=CC2=CC(N)=CC=C21 JBIJLHTVPXGSAM-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000020477 pH reduction Effects 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- FECNOIODIVNEKI-UHFFFAOYSA-N 2-[(2-aminobenzoyl)amino]benzoic acid Chemical class NC1=CC=CC=C1C(=O)NC1=CC=CC=C1C(O)=O FECNOIODIVNEKI-UHFFFAOYSA-N 0.000 description 1
- KZCSUEYBKAPKNH-UHFFFAOYSA-N 6-aminonaphthalene-1,3-disulfonic acid Chemical compound OS(=O)(=O)C1=CC(S(O)(=O)=O)=CC2=CC(N)=CC=C21 KZCSUEYBKAPKNH-UHFFFAOYSA-N 0.000 description 1
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- 240000007643 Phytolacca americana Species 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical class [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 239000000987 azo dye Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/04—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups
- C07C303/06—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups by reaction with sulfuric acid or sulfur trioxide
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a tobias acid kettle type continuous disulfonation device, which comprises a tobias acid feeding barrel, a tobias acid premixing kettle, a tobias acid primary sulfonation kettle, a tobias acid secondary sulfonation kettle, an intermediate tank and a hydrolysis tank from top to bottom, wherein a first overflow port is formed in the tobias acid primary sulfonation kettle, and a second overflow port is formed in the tobias acid secondary sulfonation kettle; the second aspect of the invention provides a matched production process; according to the device provided by the invention, the first overflow port is formed in the tobias acid primary sulfonation kettle and the second overflow port is formed in the tobias acid secondary sulfonation kettle respectively, so that the materials can be automatically and continuously transferred, and the intermediate reaction process of the materials is displayed, so that an operator can obtain a reactant in a certain intermediate process at any time to perform performance test, control the reaction condition of the materials in real time and make corresponding adjustment in time according to needs.
Description
Technical Field
The invention belongs to the technical field of chemical synthesis, and particularly relates to a Turkey acid kettle type continuous disulfonation process and a device.
Background
J-acids (2-amino-5-naphthol-7-sulfonic acid) are important dye intermediates for the manufacture of azo dyes and can be used for the manufacture of di-, scarlet-, and phenyl J-acids, among others. The beta-naphthylamine is used for preparing the J acid, because the beta-naphthylamine has strong carcinogenicity, the production method is eliminated, and the 2-naphthylamine-1-sulfonic acid (tobias acid) is used as a raw material for preparing the J acid. Tu's acid is sulfonated and hydrolyzed to obtain 2-naphthoic acid-5, 7-disulfonic monosodium salt (amino J acid), and then the neutralization, alkali fusion and acidification are carried out, and then fuming sulfuric acid is used for sulfonation, and hydrolysis, suction filtration, washing, alkali dissolution and acidification washing are carried out to obtain a J acid finished product.
At present, the batch fuming sulfuric acid sulfonation process is commonly used for producing the fuming sulfuric acid sulfonation product, the process has the advantages of large amount of used sulfuric acid, long reaction time and uncontrollable intermediate reaction, and the batch disulfonation process is carried out and completed in one kettle, so that the reaction is strongly exothermic, the reaction is easily uneven, and a large number of byproducts are generated.
Disclosure of Invention
Aiming at the defects, the invention provides a Tu's acid kettle type continuous disulfonation process and a device thereof.
The first aspect provides a tobias acid kettle type continuous disulfonation device, which comprises a tobias acid feeding cylinder, a tobias acid premixing kettle, a tobias acid primary sulfonation kettle, a tobias acid secondary sulfonation kettle, an intermediate tank and a hydrolysis tank from top to bottom, wherein a first overflow port is formed in the tobias acid primary sulfonation kettle, and a second overflow port is formed in the tobias acid secondary sulfonation kettle.
In a second aspect, the tobias acid kettle type continuous disulfonation process for producing by adopting the device comprises the following steps:
s1, adding tobias acid and fuming sulfuric acid into a tobias acid premixing kettle, mixing and stirring;
s2, transferring the mixture obtained in the step S1 to a tobias acid-sulfonation kettle for reaction;
s3, transferring the mixture obtained in the step S2 to a tobias acid disulfonation kettle for reaction;
s4, transferring the mixture obtained in the step S3 to an intermediate tank for storage;
s5, transferring the mixture stored in the step S4 to a hydrolysis tank for reaction.
The Tu's acid kettle type continuous disulfonation process and the device provided by the invention have the beneficial effects that:
through seting up first overflow mouth respectively on the first sulfonation cauldron of tobias acid and seting up the second overflow mouth on the second sulfonation cauldron of tobias acid for the material realizes automatic continuous transfer, and the middle reaction process of material shows, can acquire the reactant of a certain middle process at any time and carry out the capability test, control the reaction condition of material in real time and in time make corresponding adjustment as required, and the technology of stage formula continuity can fully dispel the heat at the in-process of reaction, make the material reaction more abundant and even, the accessory substance is few, be favorable to promoting the quality of product.
Drawings
FIG. 1 is a schematic diagram of the apparatus for the Tou's acid kettle-type continuous disulfonation according to the example;
FIG. 2 is a schematic structural diagram of a tobias acid-sulfonation kettle according to an embodiment;
FIG. 3 is a schematic structural diagram of the tobias acid disulfonation kettle according to the embodiment.
In the figure: 1-tobias acid feeding barrel, 2-two tobias acid premixing kettles arranged side by side, 3-tobias acid primary sulfonation kettle, 31-first overflow port, 32-first barrel, 321-first hook, 33-first stirrer, 34-first jacket, 35-first baffle, 36-first baffle, 37-first piston, 371-first traction rope, 4-a plurality of tobias acid secondary sulfonation kettles, 41-second overflow port, 42-second barrel, 421-second hook, 43-second stirrer, 44-second jacket, 45-second baffle, 46-second baffle, 47-second piston, 471-second traction rope, 5-intermediate tank and 6-hydrolysis tank.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the present invention, it should be noted that, if the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings or the orientations or positional relationships that the products of the present invention are usually placed in when used, the terms are only used for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the devices or elements indicated must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
In the description of the present invention, it should be further noted that unless otherwise explicitly stated or limited, the terms "disposed," "mounted," "connected," and "connected" should be interpreted broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
The embodiment provides a tobias acid kettle type continuous disulfonation device, which comprises two tobias acid feeding barrels 1 arranged side by side, two tobias acid premixing kettles 2 arranged side by side, a tobias acid primary sulfonation kettle 3, a plurality of tobias acid secondary sulfonation kettles 4, an intermediate tank 5 and a hydrolysis tank 6 from top to bottom, wherein a first overflow port 31 is formed in the tobias acid primary sulfonation kettle 3, and a second overflow port 41 is formed in the tobias acid secondary sulfonation kettle 4.
Wherein, the tobias acid-sulfonation kettle 3 comprises a first cylinder 32, a first stirrer 33 is arranged in the first cylinder 32, a first overflow port 31 is arranged at the top of the side wall of the first cylinder 32, a first jacket 34 is sleeved on the outer side wall of the first cylinder 32, the top of the first cylinder 32 is open, a first baffle 35 is arranged in the first cylinder 32, the first baffle 35 is not in contact with the bottom of the first cylinder 32, a first partition 36 is arranged between one side of the first baffle 35 close to the first overflow port 31 and the inner side wall of the first cylinder 32, the first stirrer 33 is arranged at one side of the first baffle 35 provided with the first partition 36, a first through hole is arranged on the first partition 36, a first piston 37 is arranged in the first through hole, the first piston 37 is matched with the first through hole, the first piston 37 is in a circular truncated cone shape, the upper part is small and the lower part is large, that is the first piston 37 can only be separated from the first through hole downwards, one side of the first piston 37, which is far away from the bottom of the first cylinder 32, is provided with a first pulling rope 371, one end of the first pulling rope 371 is fixedly connected with the first piston 37, the other end of the first pulling rope 371 is tied to the top of the side wall of the first cylinder 32 (the top of the side wall of the first cylinder 32 is provided with a first hook 321, the first pulling rope 371 is tied to the first hook 321, so that the first pulling rope 371 is ensured to be stretched straight and cannot be wound by the first stirrer 33), when the first through hole needs to be opened, the first piston 37 is poked downwards by a long rod, the first through hole is opened, when the first through hole needs to be closed, the first pulling rope 371 is pulled upwards, and the first through hole can be plugged by the first piston 37.
The first overflow port 31 is arranged to enable the material to automatically overflow to the lower tobias acid disulfonating kettle 4 after the reaction in the tobias acid monosulfonating kettle 3 is completed, and the first jacket 34 is used for controlling the temperature in the tobias acid monosulfonating kettle 3. When the materials are required to stay in the first cylinder 32 for reaction, the first through hole is closed, and the first stirrer 33 is started; when the material is required to overflow to the tobias acid disulfonating kettle below, the first stirrer 33 is closed, the first through hole is opened, and new material is injected from the side of the first baffle 35 where the first partition plate 36 is not arranged, the new material extrudes the reacted material upwards from the lower part of the first partition plate 36 through the first through hole, and the reacted material can overflow from the first overflow port 31.
Wherein, the Turkey acid secondary sulfonation kettle 4 comprises a second cylinder 42, a second stirrer 43 is arranged in the second cylinder 42, a second overflow port 41 is arranged at the top of the side wall of the second cylinder 42, a second jacket 44 is sleeved on the outer side wall of the second cylinder 42, a plurality of Turkey acid secondary sulfonation kettles 4 are arranged in a step-type manner from top to bottom in sequence, the top of the second cylinder 42 is open, in addition, a second baffle plate 45 is arranged in the second cylinder 42, the second baffle plate 45 is not contacted with the bottom of the second cylinder 42, a second baffle plate 46 is arranged between one side of the second baffle plate 45 close to the second overflow port 41 and the inner side wall of the second cylinder 42, the second stirrer 43 is arranged at one side of the second baffle plate 45 provided with the second baffle plate 46, a second through hole is arranged on the second baffle plate 46, a second piston 47 is arranged in the second through hole, the second piston 47 is matched with the second through hole, and is in a round table shape, big end down, second piston 47 can only separate with the second through-hole downwards promptly, one side of keeping away from the second barrel 42 bottom at second piston 47 is equipped with second haulage rope 471, the one end and the second piston 47 fixed connection of second haulage rope 471, the other end is tied in the lateral wall top of second barrel 42 (install a second couple 421 at the lateral wall top of second barrel 42, second haulage rope 471 is on second couple 421, thereby guarantee that second haulage rope 471 is flat and straight, can not twined by second agitator 43), when the second through-hole is opened to needs, poke second piston 47 downwards with the stock, the second through-hole is opened promptly, when the second through-hole is closed to needs, upwards pull second haulage rope 471, second piston 47 can block up the second through-hole promptly.
The second overflow port 41 enables the material to automatically overflow, and the stepwise arrangement mode enables the tobias acid disulfonating kettle 4 below to effectively receive the material overflowing above, so that the staged continuous reaction is realized. In addition, the second jacket 44 functions to control the temperature in the tobias acid disulfonation tank 4. When the materials are required to stay in the second cylinder 42 for reaction, the second through hole is closed, and the second stirrer 43 is started; when the material is required to overflow to another tobias acid disulfonating kettle below, the second through hole is opened, new material is injected from one side of the second baffle plate 45 where the second baffle plate 46 is not arranged, the new material extrudes the reacted material upwards from the lower part of the second baffle plate 46 through the second through hole, and the reacted material can overflow from the second overflow port 41.
The embodiment also provides a production process matched with the device, which comprises the following steps:
s1, adding tobias acid and fuming sulfuric acid into a tobias acid premixing kettle, mixing and stirring;
specifically, fuming sulfuric acid in a tank area is conveyed to a fuming sulfuric acid intermediate tank, fuming sulfuric acid is conveyed to a fuming sulfuric acid metering tank by a fuming sulfuric acid pump, fuming sulfuric acid is added into a tobias acid premixing kettle by the fuming sulfuric acid metering tank, stirring is started simultaneously, tobias acid is slowly added into the tobias acid premixing kettle through a tobias acid feeding barrel by a feeding screw feeder, the temperature is controlled within 20-30 ℃ in the feeding process, and the feeding whole process needs 4 hours, so that the material in the tobias acid premixing kettle is in a homogeneous state.
S2, transferring the mixture obtained in the step S1 to a tobias acid-sulfonation kettle for reaction;
specifically, a starting switch ball valve at the bottom of the tobias acid premixing kettle is opened, and the mixture is placed into the lower tobias acid-sulfonation kettle by using the liquid level difference. In the tobias acid-sulfonation kettle, cooling water is circulated and introduced into the first jacket, so that the temperature in the tobias acid-sulfonation kettle is maintained between 30 ℃ and 40 ℃, and the reaction lasts for 2 hours.
S3, transferring the mixture obtained in the step S2 to a tobias acid disulfonation kettle for reaction;
specifically, the mixture overflows from a first overflow port of the tobias acid primary sulfonation kettle, flows into the tobias acid secondary sulfonation kettle (at this time, sampling test is performed on the mixture in the tobias acid primary sulfonation kettle, and the specific test method can refer to GB/T21896-2008), in the tobias acid secondary sulfonation kettle, heat conduction oil is circularly introduced into a second jacket, so that the internal temperature is maintained between 120 ℃ and 130 ℃, and the reaction is performed for 2 hours, and the mixture is subjected to the sampling test, which is not described again, if the content of the sulfonated tobias acid in the mixture does not reach a qualified index, the mixture continues to flow into another tobias acid primary sulfonation kettle below through the second overflow port, and the mixture also reacts in the environment of 120 ℃ to 130 ℃ for 2 hours in the tobias acid secondary sulfonation kettle below, and then continues to overflow, so that a staged continuous reaction is achieved.
S4, transferring the mixture obtained in the step S3 to an intermediate tank for storage;
specifically, when the content of the sulfonated tobias acid in the sampled mixture reaches the qualified index, the mixture flows into the intermediate tank through the second overflow port to be stored.
S5, transferring the mixture stored in the step S4 to a hydrolysis tank for reaction.
Specifically, the mixture in the intermediate tank is transferred to a hydrolysis tank, sodium sulfate and water are respectively added, and hydrolysis reaction is carried out to obtain a final product.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The device for tobias acid kettle type continuous disulfonation is characterized by comprising a tobias acid feeding barrel, a tobias acid premixing kettle, a tobias acid primary sulfonation kettle, a tobias acid secondary sulfonation kettle, an intermediate tank and a hydrolysis tank from top to bottom, wherein a first overflow port is formed in the tobias acid primary sulfonation kettle, and a second overflow port is formed in the tobias acid secondary sulfonation kettle.
2. The apparatus according to claim 1, wherein the number of the tobias acid disulfonation kettles is several, and the several tobias acid disulfonation kettles are arranged in sequence from top to bottom.
3. The apparatus according to claim 2, wherein a plurality of said tobias acid disulfonation kettles are arranged in a stepwise manner.
4. The apparatus according to claim 1, wherein the tobias acid kettle type continuous disulfonation apparatus comprises a first cylinder, a first stirrer is arranged in the first cylinder, the first overflow port is arranged at the top of the side wall of the first cylinder, and a first jacket is arranged on the outer wall of the first cylinder.
5. The apparatus according to claim 4, wherein a first baffle is disposed in the first cylinder, the first baffle is not in contact with the bottom of the first cylinder, a first partition is disposed between a side of the first baffle close to the first overflow port and the inner side wall of the first cylinder, the first partition is provided with a first through hole, a first piston is disposed in the first through hole, and the first stirrer is disposed on a side of the first baffle where the first partition is disposed.
6. The apparatus for tobias acid kettle-type continuous disulfonation as defined in claim 1, wherein the tobias acid kettle comprises a second cylinder, a second stirrer is arranged in the second cylinder, the second overflow port is arranged on the top of the side wall of the second cylinder, and a second jacket is arranged on the outer wall of the second cylinder.
7. The apparatus according to claim 6, wherein a second baffle is disposed in the second cylinder, the second baffle is not in contact with the bottom of the second cylinder, a second partition is disposed between a side of the second baffle close to the second overflow port and the inner side wall of the second cylinder, the second partition is provided with a second through hole, a second piston is disposed in the second through hole, and the second stirrer is disposed on a side of the second baffle where the second partition is disposed.
8. A tobias acid tank type continuous disulfonation process, which adopts the device for tobias acid tank type continuous disulfonation as claimed in any one of claims 1 to 7, and comprises the following steps:
s1, adding tobias acid and fuming sulfuric acid into a tobias acid premixing kettle, mixing and stirring;
s2, transferring the mixture obtained in the step S1 to a tobias acid-sulfonation kettle for reaction;
s3, transferring the mixture obtained in the step S2 to a tobias acid disulfonation kettle for reaction;
s4, transferring the mixture obtained in the step S3 to an intermediate tank for storage;
s5, transferring the mixture stored in the step S4 to a hydrolysis tank for reaction.
9. The tobias acid tank type continuous disulfonation process of claim 8, wherein in step S3, the transfer method of the mixture is specifically: the mixture flows into the tobias acid disulfonating kettle from a first overflow port of the tobias acid disulfonating kettle.
10. The tobias acid tank type continuous disulfonation process of claim 8, wherein in step S4, the transfer method of the mixture is specifically: the mixture flows into the intermediate tank from a second overflow port of the tobias acid disulfonating kettle.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110149899.3A CN112794808A (en) | 2021-02-03 | 2021-02-03 | Tu's acid kettle type continuous disulfonation process and device |
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| CN202110149899.3A CN112794808A (en) | 2021-02-03 | 2021-02-03 | Tu's acid kettle type continuous disulfonation process and device |
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|---|---|---|---|---|
| US4199529A (en) * | 1977-10-03 | 1980-04-22 | Ciba-Geigy Ag | Process for the production of amino-I-acid |
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| CN107501138A (en) * | 2017-08-02 | 2017-12-22 | 天津市宏伟化工有限责任公司 | A kind of preparation method of Sulpho Tobias Acid |
| CN109704998A (en) * | 2019-01-09 | 2019-05-03 | 江苏吉华化工有限公司 | A kind of method that the continuous sulfonation of the naphthalene of high yield prepares 1,3,6- naphthalene trisulfonic acids |
| CN109876758A (en) * | 2019-04-02 | 2019-06-14 | 天津市科德化工有限公司 | Sulpho Tobias Acid sulfonating reaction kettle |
-
2021
- 2021-02-03 CN CN202110149899.3A patent/CN112794808A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4199529A (en) * | 1977-10-03 | 1980-04-22 | Ciba-Geigy Ag | Process for the production of amino-I-acid |
| CN1280123A (en) * | 1999-07-13 | 2001-01-17 | 天津市环境保护科学研究院 | Method for preparing J acid (7-amino-4-hydroxy-2-naphthalonesulfonic acid) |
| CN203295399U (en) * | 2013-06-17 | 2013-11-20 | 山西翔宇化工有限公司 | Device system for purifying tobias acid from tobias acid liquid waste |
| CN107501138A (en) * | 2017-08-02 | 2017-12-22 | 天津市宏伟化工有限责任公司 | A kind of preparation method of Sulpho Tobias Acid |
| CN109704998A (en) * | 2019-01-09 | 2019-05-03 | 江苏吉华化工有限公司 | A kind of method that the continuous sulfonation of the naphthalene of high yield prepares 1,3,6- naphthalene trisulfonic acids |
| CN109876758A (en) * | 2019-04-02 | 2019-06-14 | 天津市科德化工有限公司 | Sulpho Tobias Acid sulfonating reaction kettle |
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