CN214361092U

CN214361092U - Be used for tuo shi sour cauldron formula device of disulfonating in succession

Info

Publication number: CN214361092U
Application number: CN202120312041.XU
Authority: CN
Inventors: 王兴中
Original assignee: Individual
Current assignee: Individual
Priority date: 2021-02-03
Filing date: 2021-02-03
Publication date: 2021-10-08
Anticipated expiration: 2031-02-03

Abstract

The utility model provides a device for Tu's acid kettle type continuous secondary sulfonation, which comprises a Tu's acid feeding cylinder, a Tu's acid premixing kettle, a Tu's acid primary sulfonation kettle, a Tu's acid secondary sulfonation kettle, an intermediate tank and a hydrolysis tank from top to bottom, wherein a first overflow port is arranged on the Tu's acid primary sulfonation kettle, and a second overflow port is arranged on the Tu's acid secondary sulfonation kettle; the utility model provides a device is through offering first overflow mouth and offering the second overflow mouth on the sour sulfonation cauldron of tuo shi respectively on the sour two sulfonation kettles of tuo shi for the material realizes automatic continuous transfer, and the middle reaction process of material shows, makes operating personnel can acquire the reactant of certain middle process at any time and carry out the capability test, and the reaction condition of real-time control material in time makes corresponding adjustment as required.

Description

Be used for tuo shi sour cauldron formula device of disulfonating in succession

Technical Field

The utility model belongs to the technical field of the chemical synthesis device, concretely relates to be used for the continuous disulfonation device of tobias acid cauldron formula.

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, batch fuming sulfuric acid sulfonation equipment is commonly used for producing the fuming sulfuric acid sulfonation product, the equipment and the attached process have the disadvantages of large amount of 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.

SUMMERY OF THE UTILITY MODEL

The utility model provides a to above-mentioned weak point, provide a be used for two sulfonated devices in succession of tuo's sour cauldron formula, from top to bottom including tuo's sour throw feed cylinder, tuo's sour pre-mixing cauldron, tuo's sour sulfonation cauldron, tuo's sour two sulfonation kettles, intermediate tank and hydrolysis tank seted up first overflow mouth on the tuo's sour sulfonation cauldron set up the second overflow mouth on the tuo's sour two sulfonation kettles.

The utility model also provides a supporting technology of above-mentioned device, including following step:

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 utility model provides a beneficial effect that is used for the continuous disulfonation device of tobias acid kettle formula does:

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 embodiments of the present invention will be clearly and completely described below with reference to the accompanying 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, as 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 accompanying drawings, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative efforts belong to 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" and the like indicate the position or positional relationship based on the position or positional relationship shown in the drawings, or the position or positional relationship which is usually placed when the product of the present invention is used, the description is only for convenience of description and simplification, but the indication or suggestion that the device or element to be referred must have a specific position, be constructed and operated in a specific position, and thus, cannot be understood as a limitation of 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 meaning of the above terms in the present invention can be understood in specific cases to those skilled in the art.

As shown in fig. 1-3, the present embodiment provides a tobias acid kettle type continuous disulfonation apparatus, which comprises, from top to bottom, two tobias acid charging 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, wherein a first overflow port 31 is formed on the tobias acid primary sulfonation kettle 3, and a second overflow port 41 is formed on 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:

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.

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.

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.

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.

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

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.