CN217287213U - Device of high-purity preparation of synthetic acetonitrile - Google Patents

Abstract

The utility model discloses a device of high-purity preparation of synthetic acetonitrile relates to chemical industry technical field, advance pipe and condenser including acetonitrile rectifying column, thick acetonitrile advances the middle part of fixed intercommunication in acetonitrile rectifying column of pipe, the fixed intercommunication in top of acetonitrile rectifying column has the delivery pipe. The utility model relates to a rational in infrastructure, it can utilize coupling adsorption process with the device, the way of control conductivity reduces the accumulation of acetonitrile rectifying column impurity component, reduce the decomposition of impurity such as acetic acid ammonia and smuggle the purity that improves the acetonitrile product secretly, the device's first adsorption column and second adsorption column are one and open one and be equipped with, through online steam and air desorption regeneration, the continuous use, reducible acetonitrile product acetonitrile rectifying column heavy component discharges, make acetonitrile rectifying column bottom combustion gas will sieve adsorption impurity acetic acid ammonia through the aluminium oxide molecule in the first adsorption column, impurity such as acetamide, and then the gathering of acetonitrile rectifying column has been reduced.

Description

Device of high-purity preparation of synthetic acetonitrile

Technical Field

The utility model relates to the technical field of chemical industry, specifically a device of high-purity preparation of synthetic acetonitrile.

Background

Acetonitrile is also called methyl cyanide, is colorless liquid, is extremely volatile, has special odor similar to ether, can dissolve various organic, inorganic and gaseous substances, is an organic solvent with excellent performance, is also an important raw material of fine chemical engineering, is also used as a mobile phase separation molecule, and is commonly used for column chromatography and more modern high performance liquid chromatography.

In the preparation method in the prior art, after acetic acid and ammonia are synthesized, the ammonia, ammonium carbonate and ammonium acetate in the reaction solution are neutralized by sulfuric acid, then rectification separation and dehydration are carried out, and acetonitrile is purified to more than 99.9%. Therefore, the device for synthesizing the high-purity acetonitrile is provided for solving the problems.

SUMMERY OF THE UTILITY MODEL

One) technical problem to be solved

The utility model aims at making up the defects of the prior art and providing a device for preparing synthetic acetonitrile with high purity.

II) technical scheme

In order to achieve the above object, the utility model provides a following technical scheme: a device for synthesizing acetonitrile and preparing the acetonitrile with high purity, which comprises an acetonitrile rectifying tower, a crude acetonitrile inlet pipe and a condenser, the crude acetonitrile inlet pipe is fixedly communicated with the middle part of the acetonitrile rectifying tower, the top end of the acetonitrile rectifying tower is fixedly communicated with a discharge pipe, the discharge pipe is communicated with the input end of the condenser, a reboiler is arranged outside the acetonitrile rectifying tower, the output end of the reboiler is fixedly communicated with a communicating pipe, the top end of the communicating pipe is communicated with the inside of the acetonitrile rectifying tower, the bottom end of the acetonitrile rectifying tower is fixedly communicated with a discharge pipe, the input end of the reboiler is fixedly communicated with a conveying pipe, and the bottom of discharge pipe is linked together with the conveyer pipe, the mid-mounting of conveyer pipe has the circulating pump, the fixed intercommunication in middle part of acetonitrile rectifying column has the circulating pipe, be provided with the adsorption apparatus who has adsorption function between conveyer pipe and the circulating pipe.

Further, the adsorption mechanism comprises a first adsorption column, a second adsorption column, a first through pipe, a first control valve, a second through pipe, a second control valve, a connecting pipe, a third control valve, a first fixing pipe, an acetonitrile synthesis pipe, an emptying pipe, a water vapor pipe, a hot air pipe and a second fixing pipe, wherein the two ends of the first adsorption column are fixedly communicated with the first through pipe, one ends of the two first through pipes, far away from the first adsorption column, are respectively communicated with the circulating pipe and the conveying pipe, the two ends of the second adsorption column are fixedly connected with the second through pipe, one ends of the two second through pipes, far away from the second adsorption column, are respectively communicated with the circulating pipe and the conveying pipe, the first control valve is arranged in the middle of each of the two first through pipes, the second control valve is arranged in the middle of each of the two second through pipes, the connecting pipe is arranged between each of the two first through pipes and the two second through pipes, and the mid-mounting of two connecting pipes has two third control valves, the bottom mounting of the fixed pipe of second communicates in the middle part that is located the top connecting pipe, the fixed middle part that communicates in the connecting pipe below that is located in top of the fixed pipe in top of first, steam pipe and hot-air line all fix the top that communicates in the fixed pipe of second, acetonitrile synthesis pipe and blow-down pipe all fix the bottom that communicates in first fixed pipe.

Thirdly), the beneficial effects are as follows:

compared with the prior art, the device for synthesizing the high-purity acetonitrile has the following beneficial effects:

the utility model discloses a under the cooperation setting between acetonitrile rectifying column, the reboiler, communicating pipe, the discharge pipe, the conveyer pipe, the circulating pump, adsorption mechanism and the circulating pipe, can utilize coupling adsorption process with the device, the method of control conductivity reduces the accumulation of acetonitrile rectifying column impurity component, reduce the decomposition of impurity such as acetic acid ammonia and smuggle secretly and improve the purity of acetonitrile product, the first adsorption column and the second adsorption column of the device are one division of one side and are equipped with, through online steam and air desorption regeneration, continuous use, reducible acetonitrile product acetonitrile rectifying column heavy component discharges, make the gas that acetonitrile rectifying column bottom gas discharged will pass through the alumina molecule in the first adsorption column with the sieve adsorption impurity such as acetic acid ammonia, acetamide, and so on, and then reduced the gathering of acetonitrile rectifying column, reduced the acetonitrile rectifying column and extracted, the yield of the product is improved, the decomposition of excessive acetic acid ammonia has also been avoided simultaneously, the purity of the acetonitrile product is ensured by entrainment of impurities at the top of the acetonitrile rectification tower, the rectification reflux ratio is effectively reduced, the steam energy consumption is saved, and compared with the traditional rectification separation process, the device can improve the product yield.

Drawings

Fig. 1 is a schematic structural diagram of the present invention.

In the figure: 1. an acetonitrile rectification column; 2. feeding crude acetonitrile into a pipe; 3. a discharge pipe; 4. a condenser; 5. a discharge pipe; 6. a delivery pipe; 7. a reboiler; 8. a communicating pipe; 9. an adsorption mechanism; 91. a first adsorption column; 92. a second adsorption column; 93. a first flow pipe; 94. a first control valve; 95. a second flow pipe; 96. a second control valve; 97. a connecting pipe; 98. a third control valve; 99. a first stationary tube; 901. an acetonitrile synthesis tube; 902. an emptying pipe; 903. a water vapor pipe; 904. a hot air pipe; 905. a second stationary tube; 10. a circulation pump; 11. a circulation pipe.

Detailed Description

The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.

As shown in fig. 1, the utility model provides a technical scheme: a device for synthesizing high-purity acetonitrile comprises an acetonitrile rectifying tower 1, a crude acetonitrile inlet pipe 2 and a condenser 4, wherein the crude acetonitrile inlet pipe 2 is fixedly communicated with the middle part of the acetonitrile rectifying tower 1, the top end of the acetonitrile rectifying tower 1 is fixedly communicated with a discharge pipe 3, the discharge pipe 3 is communicated with the input end of the condenser 4, a reboiler 7 is arranged outside the acetonitrile rectifying tower 1, the output end of the reboiler 7 is fixedly communicated with a communicating pipe 8, the top end of the communicating pipe 8 is communicated with the inside of the acetonitrile rectifying tower 1, the bottom end of the acetonitrile rectifying tower 1 is fixedly communicated with a discharge pipe 5, the input end of the reboiler 7 is fixedly communicated with a delivery pipe 6, the bottom end of the discharge pipe 5 is communicated with the delivery pipe 6, under the operation of the reboiler 7, the crude acetonitrile in the acetonitrile rectifying tower 1 is enabled to improve the rectifying efficiency, a circulating pump 10 is arranged in the middle part of the delivery pipe 6, and the middle part of the acetonitrile rectifying tower 1 is fixedly communicated with a circulating pipe 11, an adsorption mechanism 9 with an adsorption function is arranged between the conveying pipe 6 and the circulating pipe 11.

The adsorption mechanism 9 comprises a first adsorption column 91, a second adsorption column 92, a first through pipe 93, a first control valve 94, a second through pipe 95, a second control valve 96, a connecting pipe 97, a third control valve 98, a first fixing pipe 99, an acetonitrile synthesis pipe 901, an emptying pipe 902, a water vapor pipe 903, a hot air pipe 904 and a second fixing pipe 905, wherein the first through pipe 93 is fixedly communicated with two ends of the first adsorption column 91, one ends of the two first through pipes 93, which are far away from the first adsorption column 91, are respectively communicated with a circulating pipe 11 and a conveying pipe 6, the two ends of the second adsorption column 92 are respectively fixedly connected with the second through pipe 95, one ends of the two second through pipes 95, which are far away from the second adsorption column 92, are respectively communicated with the circulating pipe 11 and the conveying pipe 6, alumina molecules are arranged inside the first adsorption column 91 and the second adsorption column 92, and ammonia acetate, an impurity adsorption sieve, the ammonia acetate, the ammonia adsorption column 95 and the impurity adsorption column 92 can be adsorbed by using the first adsorption column 91 and the second adsorption column 92, Acetamide and other impurities, a first control valve 94 is installed in the middle of each of two first flow pipes 93, a second control valve 96 is installed in the middle of each of two second flow pipes 95, a connecting pipe 97 is arranged between each of the two first flow pipes 93 and each of the two second flow pipes 95, two third control valves 98 are installed in the middle of each of the two connecting pipes 97, the bottom end of a second fixing pipe 905 is fixedly communicated with the middle of the connecting pipe 97 positioned above, the top end of a first fixing pipe 99 is fixedly communicated with the middle of the connecting pipe 97 positioned below, a water vapor pipe 903 and a hot air pipe 904 are fixedly communicated with the top end of the second fixing pipe 905, an acetonitrile synthesis pipe 901 and an emptying pipe 902 are fixedly communicated with the bottom end of the first fixing pipe 99, so that the other end of the acetonitrile synthesis pipe 901 is communicated with an acetonitrile synthesis receiving tank outside, when the first adsorption column 91 is used alone, the third control valves 98 at the right ends of the two connecting pipes 97 are both closed, and close the second control valve 96 on two second flow pipes 95, can use the first adsorption column 91 alone, thus has promoted the flexibility of use of the apparatus, through the setting of the adsorption mechanism 9, make the apparatus utilize the coupling adsorption process, the method to control conductivity reduces the accumulation of impurity component of the rectification column 1 of acetonitrile, reduce the decomposition of impurity such as ammonium acetate and entrain and improve the purity of acetonitrile product and can reach above 99.99%, the first adsorption column 91 and the second adsorption column 92 of the apparatus are open one by one, through online steam and air desorption regeneration, use continuously, can reduce the heavy component emission of the rectification column 1 of acetonitrile product acetonitrile, through alumina molecule in the first adsorption column 91 will sieve and absorb impurity such as impurity of ammonium acetate, acetamide, etc., and then reduce the gathering of the rectification column 1 of acetonitrile, reduce the rectification column 1 to extract, has improved the yield of the product, also avoided the decomposition of excessive acetic acid ammonia simultaneously, the purity of acetonitrile product is ensured to smuggleing secretly of having reduced 1 top impurity of acetonitrile rectifying column, the while is also effectual to have reduced the rectification reflux ratio, the vapour energy consumption has been practiced thrift, compare in traditional rectification separation process, the device can improve the product yield, and the device still can be through the extraction volume that increases acetonitrile rectifying column 1, sacrifice the yield of product, reach the certain concentration of control acetonitrile rectifying column 1, increase the reflux volume at 1 top of acetonitrile rectifying column simultaneously, use more vapour to ensure the purity of product.

The working principle is as follows: when the device operates, the device utilizes a coupling adsorption process to reduce the accumulation of impurity components of the acetonitrile rectifying tower 1 by a method of controlling the conductivity, reduce the decomposition of impurities such as ammonium acetate and the like and improve the purity of acetonitrile products by entrainment to be more than 99.99 percent, the first adsorption column 91 and the second adsorption column 92 of the device are open and standby, and can reduce the emission of heavy components of the acetonitrile rectifying tower 1 of the acetonitrile products through online steam and air desorption regeneration and continuous use, so that gas discharged from the bottom of the acetonitrile rectifying tower 1 can be sieved by alumina molecules in the first adsorption column 91 to adsorb impurities such as ammonium acetate, acetamide and the like, further the accumulation of the acetonitrile rectifying tower 1 is reduced, the extraction of the acetonitrile rectifying tower 1 is reduced, the yield of the products is improved, meanwhile, the decomposition of excessive ammonium acetate is avoided, the entrainment of impurities at the top of the acetonitrile rectifying tower 1 is reduced, and the purity of the acetonitrile products is ensured, meanwhile, the rectification reflux ratio is effectively reduced, the steam energy consumption is saved, and compared with the traditional rectification separation process, the device can improve the product yield.

Claims (2)

1. The utility model provides a device of high-purity preparation of synthetic acetonitrile, advances pipe (2) and condenser (4) including acetonitrile rectifying column (1), crude acetonitrile advances the middle part of fixed intercommunication in acetonitrile rectifying column (1) of pipe (2), the fixed intercommunication in top of acetonitrile rectifying column (1) has delivery pipe (3), delivery pipe (3) are linked together its characterized in that with the input of condenser (4): the outside of acetonitrile rectifying column (1) is provided with reboiler (7), the fixed intercommunication of output of reboiler (7) has communicating pipe (8), the top of communicating pipe (8) is linked together with the inside of acetonitrile rectifying column (1), the bottom mounting intercommunication of acetonitrile rectifying column (1) has discharge pipe (5), the fixed intercommunication of input of reboiler (7) has conveyer pipe (6), and the bottom and conveyer pipe (6) of discharge pipe (5) are linked together, the mid-mounting of conveyer pipe (6) has circulating pump (10), the fixed intercommunication in middle part of acetonitrile rectifying column (1) has circulating pipe (11), be provided with adsorption apparatus (9) that have adsorption function between conveyer pipe (6) and circulating pipe (11).

2. The device for high-purity preparation of synthetic acetonitrile according to claim 1, wherein: the adsorption mechanism (9) comprises a first adsorption column (91), a second adsorption column (92), a first through pipe (93), a first control valve (94), a second through pipe (95), a second control valve (96), a connecting pipe (97), a third control valve (98), a first fixed pipe (99), an acetonitrile synthetic pipe (901), a vent pipe (902), a water vapor pipe (903), a hot air pipe (904) and a second fixed pipe (905), wherein the two ends of the first adsorption column (91) are fixedly communicated with the first through pipe (93), one ends of the two first through pipes (93) far away from the first adsorption column (91) are respectively communicated with a circulating pipe (11) and a conveying pipe (6), the two ends of the second adsorption column (92) are respectively and fixedly connected with the second through pipe (95), and one ends of the two second through pipes (95) far away from the second adsorption column (92) are respectively communicated with the circulating pipe (11) and the conveying pipe (6), first control valve (94) are all installed at the middle part of two first circulation pipes (93), second control valve (96) are all installed at the middle part of two second circulation pipes (95), all be provided with between two first circulation pipes (93) and two second circulation pipes (95) connecting pipe (97), and the mid-mounting of two connecting pipe (97) has two third control valve (98), the bottom mounting of the fixed pipe of second (905) communicates in the middle part that is located top connecting pipe (97), the fixed middle part that communicates in the below connecting pipe (97) in top of the top of first fixed pipe (99), the top of steam pipe (903) and hot air pipe (904) all fixed intercommunication in the top of the fixed pipe of second (905), acetonitrile synthesis pipe (901) and blow-down pipe (902) all fixed intercommunication in the bottom of first fixed pipe (99).

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