CN211725783U - Preparation facilities of sulfanilic acid - Google Patents
Preparation facilities of sulfanilic acid Download PDFInfo
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- CN211725783U CN211725783U CN201921888247.6U CN201921888247U CN211725783U CN 211725783 U CN211725783 U CN 211725783U CN 201921888247 U CN201921888247 U CN 201921888247U CN 211725783 U CN211725783 U CN 211725783U
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Abstract
The utility model provides a device for preparing sulfanilic acid; the preparation device of sulfanilic acid comprises a mixer, a double-screw extruder, a powder cooler and a power device; the bottom of the mixer is provided with an opening which is a discharge hole; the upper part of one end of the double-screw extruder is provided with an opening which is an inlet of the double-screw extruder; the discharge port of the mixer is communicated with the inlet of the double-screw extruder; the lower part of the other end of the double-screw extruder is provided with an opening which is an outlet; the outlet is communicated with the feed inlet of the powder cooler. The preparation device of sulfanilic acid is a set of equipment with continuous process, safety, environmental protection and high yield, and the sulfanilic acid production equipment improves the production level of sulfanilic acid.
Description
Technical Field
The utility model belongs to the chemical industry equipment field, in particular to preparation facilities of sulfanilic acid.
Background
With the promotion of the construction of national technical facilities and the process of urbanization, the consumption of concrete and cement is at the top of the world, and the annual demand of the high-efficiency water reducing agent reaches more than 100 million tons. The sulfamate water reducer has the advantages of simple production process, good dispersibility on cement particles, high water reducing rate, high strength of prepared concrete, good durability, small slump loss with time and the like, thereby becoming a high-efficiency water reducer with relatively good development prospect in China at present and being one of the hot spots of the development and research of concrete chemical admixtures at present.
The bottleneck for restricting the market expansion of the sulfamate water reducer is that the production process of the key raw material sulfanilic acid is laggard, so that the production cost is high, the quality is low, a large amount of waste water and waste residues are generated in the production process, the post-treatment difficulty is increased, and the complicated environment-friendly problem is derived. The sulfanilic acid is an important organic chemical raw material, is used for synthesizing sulfamate water reducing agents, is also an intermediate of azo, acidic and active dyes, is mainly used for synthesizing bright yellow G, acidic orange II, acidic medium dark yellow and other varieties, can also be used for preventing the wheat rust, has a systemic treatment effect on the wheat rust, is called as sodium dikohlrabi, and is very widely applied.
At present, the production of sulfanilic acid mainly comprises two processes of a baking sulfonation method and a direct synthesis method. The baking sulfonation method is that aniline and concentrated sulfuric acid with equal molecular ratio are prepared into solid sulfate, then the solid sulfate is placed on a baking pan and baked in a baking furnace at 180-200 ℃, and the solid sulfate is dehydrated and transposed to form the product, or the sulfate is put into a drum-type ball mill to be baked, dehydrated and transposed to generate a target product; however, this method has poor operation conditions, non-uniform temperature, incomplete reaction, easy generation of coke, serious aniline residue, and easy operator poisoning. The direct synthesis method is that aniline and slightly excessive concentrated sulfuric acid are put into a stirring kettle, and are subjected to transposition dehydration at 180 ℃ after salification, and water is evaporated out under negative pressure; because the sulfate and the sulfanilic acid are solid, the caking is frequent in the reaction kettle, the heat transfer is not smooth, a plurality of byproducts are produced, the reaction is not complete, and the process is immature.
SUMMERY OF THE UTILITY MODEL
In order to overcome the defects of the traditional production process of aminobenzenesulfonic acid, the utility model provides a continuous, safe and environment-friendly process and equipment with high yield, which improves the production level of aminobenzenesulfonic acid.
The preparation device of sulfanilic acid of the utility model comprises a mixer, a double-screw extruder, a powder cooler and a power device; the bottom of the mixer is provided with an opening which is a discharge hole; the upper part of one end of the double-screw extruder is provided with an opening which is a feed inlet of the double-screw extruder; the discharge hole of the mixer is communicated with the feed inlet of the double-screw extruder; the lower part of the other end of the double-screw extruder is provided with an opening which is a discharge hole; the discharge hole is communicated with the feed inlet of the powder cooler;
the mixer is a conventional mixer in the chemical field, the inner material of the mixer is lining, a feeding pipeline of aniline and concentrated sulfuric acid is arranged at the top end of the mixer, and a heat preservation device is arranged at a discharge port at the bottom of the mixer;
the double-screw extruder consists of a barrel and more than 2 steam vents; the steam vent is arranged at the top of the barrel and communicated with the barrel, and a waste gas treatment device is arranged at the top of the steam vent; the barrel of the double-screw extruder has a resistance wire heating function.
The powder cooler 7 is internally provided with a circulating water coil pipe which is provided with a circulating water feeding hole and a discharging hole, and the bottom of the powder cooler is provided with a discharging hole.
The double-screw extruder is made of high-temperature-resistant and corrosion-resistant bicrystal steel.
The power device consists of two high-power explosion-proof motors and two transmission devices, wherein one high-power explosion-proof motor is connected with a screw of the double-screw extruder through one transmission device; a high-power explosion-proof motor is connected with the powder cooler through a transmission device.
The mixer has two metered feed inlets.
The mixer is provided with a temperature change meter which is arranged at the connecting part of the mixer and the extruder barrel.
The double-screw extruder is characterized in that a feed inlet and a discharge outlet are respectively arranged at two ends, wherein the feed inlet is one end far away from the motor.
A feed port and the barrel of the double-screw extruder are provided with a temperature change meter;
the feed inlet and the discharge outlet of the powder cooler are respectively arranged at two ends, and the discharge outlet is far away from one end of the motor;
the powder cooler is provided with a temperature change meter for measuring the temperature of powder in the cylinder and the temperature of the circulating water inlet and outlet;
the double-screw extruder and the powder cooler are arranged up and down, so that automatic blanking is facilitated.
Has the advantages that: the utility model provides a preparation facilities of sulfanilic acid to double screw extruder is core reaction unit, other powder coolers and feed mixer are the conventional equipment of chemical industry, the feasibility is enlargied to the engineering has, open up the nature and realize sulfanilic acid serialization production, overcome defects such as traditional baking method or rotary drum method production efficiency low, product poor quality, expanded sulfanilic acid application, promote application efficiency, and simultaneously, this technology has avoided a large amount of waste residues to produce, and the environment-friendly characteristics are showing.
Drawings
FIG. 1: does the utility model discloses a preparation facilities's of sulfanilic acid structure schematic diagram.
Detailed Description
The invention is further described and illustrated with reference to the accompanying drawings and specific embodiments.
The sulfanilic acid preparation device is shown in figure 1 and comprises a mixer 6, a double-screw extruder 1 and matched equipment, a powder cooler 7 and matched equipment; the mixer 6 is connected with the double-screw extruder 1 through a feed port 4, the double-screw extruder 1 is connected with the motor 3 through the transmission device 2, and the double-screw extruder 1 is connected with the powder cooler 7 through a feed port 10; the powder cooler 7 is connected with the motor 9 through the transmission device 8, the powder cooler 7 is connected with the double-screw extruder 1 through the feeding hole 10, the jacket of the powder cooler 7 is connected with the circulating water feeding and discharging hole through the feeding pipe 12 and the discharging pipe 11, and the powder cooler 1 is connected with the discharging device through the discharging hole 13.
The device is adopted to prepare sulfanilic acid.
Example 1
Mixing: aniline and concentrated sulfuric acid are respectively fed into a mixer 6 at a rate of 100kg/h, and the feeding rate of the concentrated sulfuric acid is controlled according to the temperature rise condition of the mixer;
reaction: starting the double-screw extruder 1, controlling the rotating speed at 10rpm, opening the electric heater of the barrel, controlling the temperature of the barrel to be 260 ℃, slowly injecting the mixed solution from the mixer 6, controlling the temperature of the feed solution to be 120-;
and (3) cooling: starting a powder cooler 7, controlling the rotating speed to be 5rpm, discharging materials from a discharge port 10 of an extruder to the powder cooler, opening feed pipes 12 and 11 of a circulating water inlet and outlet port, slowly introducing black powder from the feed port 10, and passing through the cooler until the temperature of the powder at the discharge port is about 80 ℃;
discharging: discharging through a discharge port 13 at the other end of the powder cooler 7, and receiving a powder deep cooling facility and a packaging device.
The test shows that the aniline conversion rate reaches 98 percent.
Example 2
Mixing: aniline and concentrated sulfuric acid are respectively fed into a mixer 6 at the speed of 200kg/h, and the feeding speed of the concentrated sulfuric acid is controlled according to the temperature rise condition of the mixer;
reaction: starting the double-screw extruder 1, controlling the rotating speed at 12rpm, opening the electric heater of the barrel, controlling the temperature of the barrel to be 270 ℃, slowly injecting a mixed solution from the mixer 6, controlling the temperature of a feed solution to be 120-;
and (3) cooling: starting the powder cooler 7, controlling the rotating speed to be 8rpm, discharging materials from a discharge port 10 of the extruder to the powder cooler, opening feed pipes 12 and 11 of a circulating water inlet and outlet port, slowly introducing black powder from the feed port 10, and passing through the cooler until the temperature of the powder at the discharge port is about 70 ℃;
discharging: discharging through a discharge port 13 at the other end of the powder cooler 7, and receiving a powder deep cooling facility and a packaging device.
The test shows that the aniline conversion rate reaches 97%.
Example 3
Mixing: aniline and concentrated sulfuric acid are respectively fed into a mixer 6 at the speed of 300kg/h, and the feeding speed of the concentrated sulfuric acid is controlled according to the temperature rise condition of the mixer;
reaction: starting the double-screw extruder 1, controlling the rotating speed at 15rpm, opening the electric heater of the barrel, controlling the temperature of the barrel at 280 ℃, slowly injecting a mixed solution from the mixer 6, controlling the temperature of a feed solution at 120-;
and (3) cooling: starting the powder cooler 7, controlling the rotating speed to be 10rpm, discharging materials from a discharge port 10 of the extruder to the powder cooler, opening feed pipes 12 and 11 of a circulating water inlet and outlet port, slowly introducing black powder from the feed port 10, and passing through the cooler until the temperature of the powder at the discharge port is about 60 ℃;
discharging: discharging through a discharge port 13 at the other end of the powder cooler 7, and receiving a powder deep cooling facility and a packaging device.
The test shows that the aniline conversion rate reaches 96%.
Example 4
Mixing: aniline and concentrated sulfuric acid are respectively fed into a mixer 6 at a rate of 250kg/h, and the feeding rate of the concentrated sulfuric acid is controlled according to the temperature rise condition of the mixer;
reaction: starting the double-screw extruder 1, controlling the rotating speed at 20rpm, opening the electric heater of the barrel, controlling the temperature of the barrel to be 275 ℃, slowly injecting a mixed solution from the mixer 6, controlling the temperature of a feed solution to be 120-;
and (3) cooling: starting the powder cooler 7, controlling the rotating speed to be 12rpm, discharging materials from a discharge port 10 of the extruder to the powder cooler, opening feed pipes 12 and 11 of a circulating water inlet and outlet port, slowly introducing black powder from the feed port 10, and passing through the cooler until the temperature of the powder at the discharge port is about 70 ℃;
discharging: discharging through a discharge port 13 at the other end of the powder cooler 7, and receiving a powder deep cooling facility and a packaging device.
The test shows that the aniline conversion rate reaches 96%.
Example 5
Mixing: aniline and concentrated sulfuric acid are respectively fed into a mixer 6 at the rate of 150kg/h, and the feeding rate of the concentrated sulfuric acid is controlled according to the temperature rise condition of the mixer;
reaction: starting the double-screw extruder 1, controlling the rotating speed at 20rpm, opening the electric heater of the barrel, controlling the temperature of the barrel to be 265 ℃, slowly injecting a mixed solution from the mixer 6, controlling the temperature of a feed solution to be 120-;
and (3) cooling: starting the powder cooler 7, controlling the rotating speed to be 12rpm, discharging materials from a discharge port 10 of the extruder to the powder cooler, opening feed pipes 12 and 11 of a circulating water inlet and outlet port, slowly introducing black powder from the feed port 10, and passing through the cooler until the temperature of the powder at the discharge port is about 75 ℃;
discharging: discharging through a discharge port 13 at the other end of the powder cooler 7, and receiving a powder deep cooling facility and a packaging device.
The test shows that the aniline conversion rate reaches 98 percent.
Example 6
Mixing: aniline and concentrated sulfuric acid are respectively fed into a mixer 6 at a rate of 180kg/h, and the feeding rate of the concentrated sulfuric acid is controlled according to the temperature rise condition of the mixer;
reaction: starting the double-screw extruder 1, controlling the rotating speed at 18rpm, opening the electric heater of the barrel, controlling the temperature of the barrel to be 270 ℃, slowly injecting a mixed solution from the mixer 6, controlling the temperature of a feed solution to be 120-;
and (3) cooling: starting the powder cooler 7, controlling the rotating speed to be 10rpm, discharging materials from a discharge port 10 of the extruder to the powder cooler, opening feed pipes 12 and 11 of a circulating water inlet and outlet port, slowly introducing black powder from the feed port 10, and passing through the cooler until the temperature of the powder at the discharge port is about 80 ℃;
discharging: discharging through a discharge port 13 at the other end of the powder cooler 7, and receiving a powder deep cooling facility and a packaging device.
The test shows that the aniline conversion rate reaches 97%.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, many variations and modifications can be made without departing from the inventive concept, and these should also be considered as within the scope of the present invention.
Claims (10)
1. The preparation device of sulfanilic acid is characterized by comprising a mixer, a double-screw extruder, a powder cooler and a power device;
the bottom of the mixer is provided with an opening which is a discharge hole;
the upper part of one end of the double-screw extruder is provided with an opening which is a feed inlet of the double-screw extruder; the discharge hole of the mixer is communicated with the feed inlet of the double-screw extruder;
the lower part of the other end of the double-screw extruder is provided with an opening which is a discharge hole; the discharge hole is communicated with the feed inlet of the powder cooler;
the mixer is internally made of lining enamel, the top end of the mixer is provided with a feeding pipeline of aniline and concentrated sulfuric acid, and a discharge hole at the bottom of the mixer is provided with a heat preservation device;
the double-screw extruder consists of a barrel and more than 2 steam vents; the steam vent is arranged at the top of the barrel and communicated with the barrel, and a waste gas treatment device is arranged at the top of the steam vent; the barrel of the double-screw extruder has a resistance wire heating function;
the powder cooler is internally provided with a circulating water coil pipe which is provided with a circulating water feeding hole and a discharging hole, and the bottom of the powder cooler is provided with the discharging hole.
2. The apparatus for preparing sulfanilic acid according to claim 1, wherein the twin-screw extruder is made of high temperature and corrosion resistant bicrystal steel.
3. The apparatus for preparing sulfanilic acid according to claim 1, wherein the power unit comprises two high-power explosion-proof motors and two transmission devices, and one high-power explosion-proof motor is connected with the screw of the twin-screw extruder by one transmission device; a high-power explosion-proof motor is connected with the powder cooler through a transmission device.
4. The apparatus for preparing sulfanilic acid as claimed in claim 1, wherein the mixer has two metering inlets.
5. The apparatus for preparing sulfanilic acid according to claim 1, wherein the mixer has a thermometer, and the thermometer is disposed at a connection portion of the mixer and the extruder barrel.
6. The apparatus for preparing sulfanilic acid according to claim 1, wherein the twin-screw extruder has a feed inlet and a discharge outlet at two ends, wherein the feed inlet is at the end far from the motor.
7. The apparatus for preparing sulfanilic acid according to claim 1, wherein a temperature gauge is provided at a feed port and a barrel of the twin-screw extruder.
8. The apparatus for preparing sulfanilic acid according to claim 1, wherein the powder cooler has a feed inlet and a discharge outlet at two ends, and the discharge outlet is far from the motor.
9. The apparatus for preparing sulfanilic acid according to claim 1, wherein the powder cooler is equipped with a temperature change meter for measuring the temperature of the powder in the cylinder and the temperature of the inlet and outlet of the circulating water.
10. The apparatus for preparing sulfanilic acid according to claim 1, wherein the twin-screw extruder and the powder cooler are arranged up and down.
Priority Applications (1)
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CN201921888247.6U CN211725783U (en) | 2019-11-05 | 2019-11-05 | Preparation facilities of sulfanilic acid |
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CN201921888247.6U CN211725783U (en) | 2019-11-05 | 2019-11-05 | Preparation facilities of sulfanilic acid |
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CN211725783U true CN211725783U (en) | 2020-10-23 |
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2019
- 2019-11-05 CN CN201921888247.6U patent/CN211725783U/en active Active
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