CN217901469U - Device for measuring ammonium carbonate content in ammonium bicarbonate - Google Patents
Device for measuring ammonium carbonate content in ammonium bicarbonate Download PDFInfo
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- CN217901469U CN217901469U CN202220790446.9U CN202220790446U CN217901469U CN 217901469 U CN217901469 U CN 217901469U CN 202220790446 U CN202220790446 U CN 202220790446U CN 217901469 U CN217901469 U CN 217901469U
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Abstract
The utility model relates to a measuring device. The utility model discloses a survey device of ammonium bicarbonate content: comprises a reaction vessel, a gas collecting bottle, a water receiving bottle and an automatic lifting interlocking system; the automatic lifting interlocking system comprises a laser liquid level monitor I, a laser liquid level monitor II, a linkage control slide block, an interlocking controller and a linkage control lifter. The utility model discloses a survey device of ammonium bicarbonate content is applicable to the ammonium bicarbonate and makes and the detection and the control in the use. Besides ammonium bicarbonate, the product can also be used for products such as sodium carbonate, potassium carbonate, calcium carbonate and the like.
Description
Technical Field
The utility model relates to a measuring device, especially a survey device of ammonium bicarbonate content of carbonic acid.
Background
The preparation method of ammonium bicarbonate generally takes ammonia water with certain concentration as raw material, and prepares ammonium bicarbonate by carbonation reaction of carbon dioxide, and then obtains ammonium bicarbonate products by centrifugal solid-liquid separation. Therefore, during carbonation, the degree of carbonation in the reaction system needs to be controlled to determine the endpoint. If the carbonization degree is insufficient, the content of ammonium carbonate in the produced ammonium bicarbonate is high, and the subsequent use performance is influenced; if the time for passing carbon dioxide is prolonged to ensure the degree of carbonization, the carbon dioxide is wasted and the environment is polluted.
Furthermore, during the use of ammonium bicarbonate, for example, in the production of potassium bicarbonate by ion exchange, if the ammonium carbonate in the ammonium bicarbonate solution is too high, the ammonium bicarbonate solution is not pure potassium bicarbonate but a mixture of potassium bicarbonate and potassium carbonate, which affects the evaporative crystallization of potassium bicarbonate and the product quality.
The content of ammonium carbonate in the ammonium bicarbonate is not a simple and feasible method at present; because ammonium bicarbonate and ammonium carbonate cannot be detected by an acid-base titration stepwise method, because the ammonium bicarbonate and ammonium carbonate are neutralized by hydrochloric acid or sulfuric acid and are reacted in an equimolar ratio, and ammonium chloride or ammonium sulfate formed after the reaction is also a buffer salt, the reaction endpoint is not obvious.
The literature reports that potassium carbonate in potassium bicarbonate can be obtained by removing carbonate by using barium chloride and then titrating by using a hydrochloric acid or sulfuric acid standard solution, so as to calculate the content of the potassium carbonate and the potassium bicarbonate. However, the content of ammonium carbonate in ammonium bicarbonate cannot be analyzed by a precipitation method, because ammonium bicarbonate is not stable, after the ammonium carbonate is precipitated by barium chloride, the ammonium bicarbonate is decomposed to form part of the ammonium carbonate, a certain balance is always formed, and the precipitation method is not applicable.
The literature reports that sodium carbonate in sodium bicarbonate or potassium carbonate in potassium bicarbonate can be analyzed by a high-temperature calcination method, and the content of the sodium bicarbonate or the potassium bicarbonate is calculated by weight loss during calcination, so that the content of the sodium carbonate or the potassium carbonate is obtained.
However, ammonium bicarbonate and ammonium carbonate are decomposed at high temperature, and thus the calcination method is not suitable. Therefore, a method and equipment for detecting the content of ammonium carbonate in ammonium bicarbonate are needed, and the problems in the existing production and quality detection are solved.
SUMMERY OF THE UTILITY MODEL
The to-be-solved technical problem of the utility model is to provide a simple and convenient, quick and low-cost survey device of ammonium bicarbonate ammonium carbonate content.
In order to solve the technical problem, the utility model provides a device for measuring the content of ammonium carbonate in ammonium bicarbonate, which comprises a reaction vessel, a gas collecting bottle, a water receiving bottle and an automatic lifting interlocking system;
the reaction container is provided with a feed inlet, a connecting port and an exhaust port and is arranged in the heating device; a constant pressure funnel for feeding is arranged at the feeding port, and the outlet of the constant pressure funnel is communicated with the feeding port through an adjusting valve;
the gas collecting bottle is a bottle body with scales and is in an inverted state, and a bottle mouth plug is arranged at the bottle mouth of the gas collecting bottle; the inner cavity of the bottle bottom of the gas collecting bottle is communicated with an exhaust pipe through an emptying valve;
the water receiving bottle is a bottle body with scales, a bottle plug is arranged at the bottle mouth of the water receiving bottle, and the exhaust pipe hermetically penetrates through the bottle plug and then is communicated with the inner cavity of the water receiving bottle; a connecting port is arranged on the side wall of the water receiving bottle close to the bottom; the water receiving bottle is arranged on the lifting platform, and a linkage control lifter with a lifting motor is arranged at the bottom of the lifting platform;
one end of the U-shaped pipeline is hermetically connected with the exhaust port, and the other end of the U-shaped pipeline hermetically penetrates through the bottle mouth plug and then reaches the bottle bottom of the gas collecting bottle;
the mounting height of the reaction vessel is higher than that of the gas collecting bottle;
one end of the liquid discharge pipe hermetically penetrates through the bottle mouth plug and then is communicated with the inner cavity of the gas collection bottle; the other end of the liquid discharge pipe is hermetically connected with a connecting port of the water receiving bottle;
the automatic lifting interlocking system comprises a laser liquid level monitor I, a laser liquid level monitor II, a linkage control slide block, an interlocking controller and a linkage control lifter; the laser liquid level monitor I is used for monitoring the liquid level of the gas collecting bottle, and the laser liquid level monitor II is used for monitoring the liquid level of the water receiving bottle; the linkage control sliding block is a sliding block with a motor and is sleeved on the second iron support and movably connected with the second iron support; the linkage control slide block is fixedly connected with a laser liquid level monitor I and a laser liquid level monitor II respectively;
the laser liquid level monitor I, the laser liquid level monitor II, a motor of the linkage control slide block and a lifting motor of the linkage control lifter are respectively connected with the interlocking controller through signals.
As the utility model discloses an improvement of ammonium bicarbonate content's survey device:
a thermometer is arranged at the connecting port; the inlet of the constant pressure funnel is provided with a ground plug.
As the further improvement of the measuring device for ammonium bicarbonate content of the utility model:
the bottom of the gas collecting bottle is respectively connected with a thermometer and a pressure gauge.
As the utility model discloses a further improvement of survey device of ammonium bicarbonate content:
the outer surface of the gas collection bottle is provided with a fixing ring, and the fixing ring is fixed with the iron support.
As the utility model discloses a further improvement of survey device of ammonium bicarbonate content:
a magnetic stirrer is arranged in the reaction vessel.
The utility model discloses in, the fluid-discharge tube that is used for connecting gas collecting bottle and water receiving bottle is transparent silica gel hose.
The utility model discloses still provide the survey method of ammonium bicarbonate ammonium carbonate content who utilizes above-mentioned survey device to go on simultaneously, including following step:
1) Filling water in the gas collecting bottle;
2) Starting a laser liquid level monitor I to track and monitor the liquid level in the gas collecting bottle, transmitting the liquid level information to an interlocking controller, and controlling a linkage control slider to move up and down along an iron support so as to ensure that the height of the laser liquid level monitor I is consistent with the actual liquid level height of the gas collecting bottle;
meanwhile, the laser liquid level monitor II is fixedly connected with the linkage control slide block, so that the laser liquid level monitor II also moves up and down correspondingly, the liquid level information is transmitted to the interlocking controller, and the interlocking controller controls the linkage control lifter to move up and down, so that the actual liquid level height of the water receiving bottle is ensured to be consistent with the height of the laser liquid level monitor II;
thereby realizing the liquid level of the gas collecting bottle and the water receiving bottle is kept equal;
3) Putting the ammonium bicarbonate solution serving as a to-be-detected product into the reaction container through the feeding hole;
4) Adding the sulfuric acid solution into a constant-pressure funnel; opening the regulating valve, and dripping the sulfuric acid solution into the reaction container through the feeding hole for reaction;
5) Carbon dioxide gas generated by reaction in the reaction container is led into the bottom of the gas collecting bottle through the exhaust port and the U-shaped pipeline, and water in the gas collecting bottle is discharged into the water receiving bottle through the liquid discharge pipe under the pushing of the carbon dioxide;
the liquid level in the gas collecting bottle is lowered along with the increase of the amount of carbon dioxide generated by the dropwise addition reaction of sulfuric acid, the liquid level in the gas collecting bottle is tracked and monitored by the laser liquid level monitor I, and the interlocking controller controls the linkage control slide block to move up and down so as to keep the liquid levels in the laser liquid level monitor I and the gas collecting bottle at a same height all the time;
meanwhile, the liquid level in the water receiving bottle rises along with the liquid level in the water receiving bottle with the scale, the laser liquid level monitor II tracks and monitors the liquid level in the water receiving bottle with the scale, and the interlocking controller controls the linkage control lifter to rise and fall so as to keep the liquid levels in the laser liquid level monitor II and the water receiving bottle with the scale at a height all the time;
6) Stopping dripping sulfuric acid when carbon dioxide bubbles are not generated any more after the sulfuric acid is dripped into the reaction container, and reading liquid levels in the gas collecting bottle and the water receiving bottle through scales;
7) And calculating to obtain the ammonium carbonate content in the ammonium bicarbonate.
As the improvement of the determination method of the ammonium carbonate content in the ammonium bicarbonate of the utility model:
the step 7) comprises the following steps:
7.1 Calculating the molar concentration of carbon dioxide according to formula (1):
in formula (1):
C 1 -the molar concentration of carbon dioxide in the ammonium bicarbonate solution as the sample to be tested, in mol/L;
T 0 -standard condition temperature, value 273.15K;
t-temperature of gas in gas collection bottle, unit ℃;
r-gas molar volume (gas constant) under standard conditions, 22.4L/mol;
v-measured displacement, in mL;
V 1 -the volume of ammonium bicarbonate solution as the test substance;
description of the drawings: the measured water discharge, namely the falling number of the liquid in the gas collecting bottle or the rising volume of the water in the water receiving bottle, should be equal, if the deviation of the two is more than 3%, the experiment needs to be repeated;
7.2 C), total ammonia content C of ammonium bicarbonate solution as a sample to be tested 3 Measurement of (1) (Formaldehyde legal ammonia method);
7.3 And calculating the concentration of ammonium carbonate in the ammonium bicarbonate solution:
ammonium carbonate concentration is as follows 1 Expressed (in g/L) and calculated according to formula (3); ammonium bicarbonate concentration in A 2 Expressed (in g/L) and calculated according to equation (4).
A 1 ＝(C 3 -C 1 )×96.09…………(3)
A 2 ＝(C 1 ×79.06)-(A 1 ×79.06÷96.09)…………(4)。
As a further improvement of the determination method of ammonium carbonate content in ammonium bicarbonate of the utility model: c 3 The calculation formula of (2) is as follows:
C 3 ＝C 2 ×V 2 /V 1 …………………………(2)
C 3 the unit of (A) is mol/L;
in formula (2):
C 2 -sodium hydroxide standard titration solution concentration in mol/L;
V 2 titration volume of sodium hydroxide standard solution in mL;
V 1 the volume of the ammonium bicarbonate solution measured is in mL.
The utility model discloses a large amount of experiments prove that firstly adopt formaldehyde to decide ammonium method survey NH 4 + Content or concentration of (A), and measuring CO by acid reaction and water discharge method 2 The contents or concentrations of the components of ammonium carbonate and ammonium bicarbonate are obtained by calculation. But at present also do not have comparatively simple and convenient suitable drainage method to survey the equipment of volume, consequently the utility model discloses a large amount of research and design develop one set of special equipment.
The utility model discloses a survey device and method of ammonium bicarbonate content is applicable to ammonium bicarbonate and detects and control in manufacturing and the use to simple and convenient quick, with low costs moreover, the suitability is very strong. Besides ammonium bicarbonate, the product can also be used for products such as sodium carbonate, potassium carbonate, calcium carbonate and the like.
Drawings
The following describes the embodiments of the present invention in further detail with reference to the attached drawings.
Fig. 1 is a schematic structural diagram of the device for determining the content of ammonium carbonate in ammonium bicarbonate according to the present invention.
In the figure: the device comprises a ground plug 1, a constant pressure funnel 2, a thermometer 3, a valve 4, a feed inlet 5, a connecting port 6, an exhaust port 7, a three-port reaction bottle 8, a U-shaped pipeline 9 and a thermometer 10; a connecting port 11, a pressure gauge 12, a valve 13, an exhaust pipe 14, an emptying valve 15, a gas collecting bottle 16, a fixing ring 17, a bottle mouth plug 18, an iron stand 19 and a liquid discharge pipe 20; the device comprises a laser liquid level monitor I21, a laser liquid level monitor II 23, a linkage control slide block 22, an interlocking controller 24, an iron stand 25, an exhaust pipe 26, a valve 27, a bottle plug 28, a water receiving bottle 29 and a connecting port 30; a lifting platform 31 and a linkage control lifter 32.
Detailed Description
The invention will be further described with reference to specific examples, but the scope of protection of the invention is not limited thereto:
embodiment 1, a device for measuring ammonium carbonate content in ammonium bicarbonate comprises a reaction vessel, a gas collecting bottle 16, a water receiving bottle 29 and an automatic lifting interlocking system. The reaction vessel is a three-mouth reaction bottle 8.
The three-mouth reaction bottle 8 is provided with a feed inlet 5, a connecting port 6 and an exhaust port 7, and the three-mouth reaction bottle 8 is arranged in an oil bath pan; a thermometer 3 is arranged at the connecting port 6; the constant pressure funnel 2 for feeding is arranged at the position of the feeding hole 5, the ground plug 1 is arranged at the inlet of the constant pressure funnel 2, the outlet of the constant pressure funnel 2 is communicated with the feeding hole 5 through the adjusting valve 4, the thermometer 3 is a mercury thermometer with the measuring range of 0-100 ℃ and the graduation of 1 ℃, the volume of the constant pressure funnel 2 is 50ml, the volume of the three-mouth reaction bottle 8 is 250ml, and the material is colorless transparent hard glass.
The gas collecting bottle 16 is a gas collecting bottle with scales and is in an inverted state, so that the bottle opening of the gas collecting bottle 16 faces downwards, and a bottle opening plug 18 is arranged at the bottle opening of the gas collecting bottle 16.
The thermometer 10 is communicated with the bottle bottom inner cavity of the gas collecting bottle 16 through a connecting port 11, and the bottle bottom inner cavity of the gas collecting bottle 16 is communicated with a pressure gauge 12 through a valve 13; the inner cavity at the bottom of the gas collecting bottle 16 is also communicated with the exhaust pipe 14 through an emptying valve 15. The pressure gauge 12 is an absolute pressure gauge (the measuring range is 0-10 Kpa); a mercury thermometer with a measuring range of 0-50 ℃ and graduation of 0.1 ℃ for the thermometer 10; the gas collecting bottle 16 is a graduated gas collecting bottle with a volume of 5L (the minimum graduation is 50 ml) and is made of colorless transparent hard glass. The outer surface of the gas collecting bottle 16 is provided with a fixing ring 17, and the fixing ring 17 is fixed with an iron stand 19, so that the gas collecting bottle 16 is vertically and stably fixed.
The water receiving bottle 29 is a bottle body with scales, a bottle stopper 28 is arranged at the bottle mouth of the water receiving bottle 29, and the exhaust pipe 26 hermetically penetrates through the bottle stopper 28 and then is communicated with the inner cavity of the water receiving bottle 29; a valve 27 is arranged on the exhaust pipe 26; a connection port 30 is provided at the side wall of the water receiving bottle 29 near the bottom. The water receiving bottle 29 is a graduated bottle having a volume of 5L (the minimum graduation is 50 ml) and is made of colorless transparent hard glass. The water receiving bottle 29 is arranged on a lifting platform 31, and a linkage control lifter 32 is arranged at the bottom of the lifting platform 31. The coordinated control lifter 32 is a coordinated control lifter 32 with a lifting motor.
One end of the U-shaped pipeline 9 is hermetically connected with the exhaust port 7 of the three-port reaction bottle 8, and the other end of the U-shaped pipeline hermetically penetrates through the bottle mouth plug 18 and then reaches the bottom of the gas collecting bottle 16.
The three-mouth reaction bottle 8 should be installed at a height higher than that of the gas collection bottle 16, that is, the lowest part of the three-mouth reaction bottle 8 should be higher than the highest part of the gas collection bottle 16 to prevent the liquid in the gas collection bottle 16 from flowing backwards.
One end of the liquid discharge pipe 20 hermetically penetrates through the bottle mouth plug 18 and then is communicated with the inner cavity of the gas collecting bottle 16; the other end of the drain pipe 20 is connected to the connection port 30 of the water receiving bottle 29 in a sealing manner so as to communicate with the bottom of the inner cavity of the water receiving bottle 29. The liquid discharge pipe 20 with scales is a transparent silica gel hose, so that the liquid discharge pipe is convenient to stretch and descend.
The automatic lifting interlocking system comprises a laser liquid level monitor I21, a laser liquid level monitor II 23, a linkage control slide block 22, an interlocking controller 24 and a linkage control lifter 32; the linkage control slider 22 is a slider with a motor, and the linkage control slider 22 is sleeved on the iron support 25 and can move up and down along the iron support 25. The linkage control slide block 22 is fixedly connected with the laser liquid level monitor I21 and the laser liquid level monitor II 23 respectively.
The laser liquid level monitor I21 and the laser liquid level monitor II 23 are respectively connected with the interlocking controller 24 through signals, and the interlocking controller 24 is respectively connected with the motor of the linkage control slide block 22 and the lifting motor of the linkage control lifter 32 through signals.
The laser liquid level monitor I21 monitors the liquid level of the gas collecting bottle 16, the liquid level information is transmitted to the interlocking controller 24, and the interlocking controller 24 controls the interlocking control slide block 22 to move up and down along the iron stand 25, so that the height of the laser liquid level monitor I21 is ensured to be consistent with the actual liquid level of the gas collecting bottle 16.
Meanwhile, because the laser liquid level monitor II 23 is fixedly connected with the linkage control slide block 22, the laser liquid level monitor II 23 correspondingly moves up and down, the liquid level information is transmitted to the interlocking controller 24, and the interlocking controller 24 controls the linkage control lifter 32 to move up and down, so that the actual liquid level height of the water receiving bottle 29 is ensured to be consistent with the height of the laser liquid level monitor II 23.
Thereby realizing that the liquid level of the gas collecting bottle 16 is equal to that of the water receiving bottle 29.
Namely, the laser liquid level monitor I21 tracks and monitors the liquid level in the gas collecting bottle 16 with scales, and controls the linkage control slide block 22 to move up and down through the interlocking controller 24 so as to keep the liquid level in the laser liquid level monitor I21 and the gas collecting bottle 16 at a height all the time.
The laser liquid level monitor II 23 tracks and monitors the liquid level in the water receiving bottle 29 with the scale marks, and controls the lifting and the descending of the lifting device 32 in a linkage manner through the interlocking controller 24, so that the liquid levels in the laser liquid level monitor II 23 and the water receiving bottle 29 with the scale marks are always kept at one height.
In the utility model, all the parts can be obtained in a conventional commercial form, for example, the laser liquid level monitor I21 and the laser liquid level monitor II 23 can be selected from a GOLDY-10G type laser glass liquid level meter produced by Beijing Hamman electronics company Limited; the interlock controller 24 can be purchased from a DKC-220 programmable step servo motor controller (PLC motion controller) produced by Shanghai Yigao science and technology; the linkage control lifter 32 is commercially available from 150mm stroke step push rods (gears) manufactured by yoyo louis electric push rod ltd; the linkage control slide block 22 can be purchased from RXP60-300 synchronous belt linear numerical control electric sliding table guide module produced by metropolis linkage Rui-Chi science and technology Limited.
The thermometer 3 measures the reaction temperature of the contents of the three-necked reaction flask 8.
The thermometer 10 measures the temperature of the gas in the gas collection bottle 16, that is, the temperature corresponding to t (gas in the gas collection bottle 16) in the following equation (1).
The emptying valve 15 is used for emptying when the gas collecting bottle 16 is filled with water; that is, when water is filled in the air collector 16 through the exhaust pipe 14, the air vent valve 15 is opened, and the air in the air collector 16 is exhausted.
The pressure gauge 12 is used for measuring the pressure of the gas collecting bottle 16; thus, when the pressure of the gas collection bottle 16 needs to be measured, the valve 13 is opened.
The valve 27 and vent tube 26 function to vent the gas in the water receiving bottle 29 when the measurement is being made, to equalize the pressure in the bottle to atmospheric pressure.
Example 2, a method for determining ammonium carbonate content in ammonium bicarbonate, using the apparatus described in example 1, the actual procedure was as follows:
1. when the test is started, three openings of the three-opening reaction bottle 8 are all in an open state; namely, the connection between the exhaust port 7 and the U-shaped pipeline 9 is disconnected, and the connection between the feeding constant-pressure funnel 2 and the feeding port 5 is disconnected;
the air collecting bottle 16 with scales is filled with water through the air release valve 15 and the exhaust pipe 14, then the air release valve 15 is closed, the exhaust port 7 and the U-shaped pipeline 9 are connected in a sealing mode, and the air release valve 27 is opened.
2. The laser liquid level monitor I21 is started to track and monitor the liquid level in the gas collecting bottle 16 with scales, the liquid level information is transmitted to the interlocking controller 24, and the interlocking controller 24 controls the interlocking control slide block 22 to move up and down along the iron support 25, so that the height of the laser liquid level monitor I21 is consistent with the actual liquid level height of the gas collecting bottle 16.
Meanwhile, because the laser liquid level monitor II 23 is fixedly connected with the linkage control slide block 22, the laser liquid level monitor II 23 correspondingly moves up and down, the liquid level information is transmitted to the interlocking controller 24, and the interlocking controller 24 controls the linkage control lifter 32 to move up and down, so that the actual liquid level height of the water receiving bottle 29 is ensured to be consistent with the height of the laser liquid level monitor II 23.
Thereby realizing that the liquid level of the gas collecting bottle 16 is equal to that of the water receiving bottle 29.
When the reaction has not proceeded, the water receiving bottle 29 is empty of water, and therefore the connection port 30 of the water receiving bottle 29 is far higher than the opening of the gas collection bottle 16, and therefore the water in the gas collection bottle 16 cannot be drained into the water receiving bottle 29 through the drain pipe 20.
3. Through a feed inlet 5 of a three-mouth reaction bottle 8, putting a proper amount of ammonium bicarbonate solution serving as a product to be detected into the three-mouth reaction bottle 8, adding a magnetic stirrer into the three-mouth reaction bottle 8, connecting a feeding constant-pressure funnel 2 with the feed inlet 5, and connecting a thermometer 3 with a connecting port 6;
4. the grinding plug 1 is opened, 50ml of sulfuric acid with the mass concentration of 50% is added into the constant pressure funnel 2, and after the addition of the sulfuric acid is finished, the grinding plug 1 is covered.
The magnetic stirrer is started, the regulating valve 4 is slowly opened, and the sulfuric acid is dripped into the three-mouth reaction bottle 8 through the feeding hole 5 for reaction.
5. Carbon dioxide gas generated by reaction in the three-mouth reaction bottle 8 is guided into the bottom of the gas collecting bottle 16 with scales through the exhaust port 7 and the U-shaped pipeline 9, and water in the gas collecting bottle 16 is discharged into the water receiving bottle 29 with scales through the liquid discharge pipe 20 under the pushing of the carbon dioxide.
Along with the increase of the amount of carbon dioxide generated by the dropwise adding reaction of sulfuric acid, the liquid level in the gas collecting bottle 16 descends, the liquid level in the gas collecting bottle 16 with scales is tracked and monitored by the laser liquid level monitor I21, and the interlocking controller 24 controls the linkage control slide block 22 to move up and down so as to keep the liquid levels in the laser liquid level monitor I21 and the gas collecting bottle 16 at a same height all the time.
Meanwhile, the liquid level in the water receiving bottle 29 with the scales also rises, the laser liquid level monitor II 23 tracks and monitors the liquid level in the water receiving bottle 29 with the scales, and the interlocking controller 24 controls the lifting and the descending of the lifting device 32 in a linkage manner so as to keep the liquid levels in the laser liquid level monitor II 23 and the water receiving bottle 29 with the scales at a same height all the time.
6. When no carbon dioxide bubbles are generated after sulfuric acid is dripped (namely, no bubbles are generated in the three-mouth reaction bottle 8, and the liquid level in the gas collecting bottle 16 does not drop), the dripping of the sulfuric acid is stopped, the liquid levels in the gas collecting bottle 16 and the water receiving bottle 29 are read through scales, the reading volume of the carbon dioxide is calculated, and the temperature is read at the same time.
From PV = nRT, the carbon dioxide molarity can be calculated from equation (1) as the same number of moles of gas volume is directly proportional to temperature at the same pressure:
in formula (1):
C 1 -the molar concentration of carbon dioxide in the ammonium bicarbonate solution as the sample to be tested, in mol/L;
T 0 standard temperature, value 273.15K.
t-temperature of gas in the gas collection bottle 16 in units;
r-gas molar volume (gas constant) under standard conditions, 22.4L/mol;
v-measured Water displacement, in mL
V 1 -the volume of the ammonium bicarbonate solution of the test substance;
description of the drawings: the measured displacement, which is the number of drops of the liquid in the gas collecting bottle 16 or the volume of the water in the water receiving bottle 29, should be equal, and if the deviation between the two is more than 3%, the experiment needs to be repeated;
7. measuring total ammonia content (ammonia method by formaldehyde method), accurately transferring ammonium bicarbonate solution (ammonium bicarbonate solution in step 3) as to-be-measured product by using pipette, and measuring volume by V 1 Transferring into 250mL conical flask, adding water to 80mL, adding 3 drops of methyl red indicator (0.1%, m/m), adjusting to red with 30% sulfuric acid solution, heating and boiling for 3min, cooling to room temperature, adjusting to red with sodium hydroxide solution (about 0.5N) and just disappearing, adding 10mL of neutral formaldehyde solution (20%, m/m), standing for 5min, adding 3 drops of phenolphthalein indicator (0.1%, m/m)), and adding sodium hydroxide standard solution (concentration is C) 2 ) Titrating until the solution does not fade within 30 seconds to reddish color, and recording the consumed hydrogen and oxygenThe volume of the sodium hydroxide standard solution (the titrated amount of 0.5mol/L of the sodium hydroxide standard solution) is calculated as V 2 。
The total ammonia content in the ammonium bicarbonate solution as the sample to be measured is C 3 In terms of mol/L, calculated according to formula (2)
C 3 ＝C 2 ×V 2 /V 1 …………………………(2)
In the formula:
C 2 -sodium hydroxide standard titration solution concentration in mol/L;
V 2 titration volume of sodium hydroxide standard solution in mL;
V 1 the volume of the ammonium bicarbonate solution is measured in mL;
8. calculation of ammonium carbonate concentration in ammonium bicarbonate solution, ammonium carbonate concentration is expressed as A 1 Expressed (in g/L) and calculated according to formula (3); ammonium bicarbonate concentration in A 2 Expressed (in g/L) and calculated according to equation (4).
A 1 ＝(C 3 -C 1 )×96.09…………(3)
A2＝C 1 ×79.06-A 1 ×79.06÷96.09…………(4)
In the formula:
96.09-ammonium carbonate molar mass value, wherein the unit is g/moL;
79.06-ammonium bicarbonate molar mass value, and the unit is g/moL.
Experiment 1, determination of ammonium carbonate content in ammonium bicarbonate, according to the method described in example 2, the following is specified:
1. 1.5152g ammonium carbonate (content 99.0%) and 29.2308g ammonium bicarbonate (content 97.5%) were transferred into a 100ml volumetric flask, and distilled water was added at room temperature to dissolve and fix the volume to 100ml, the ammonium carbonate in the obtained ammonium bicarbonate solution was 15.00g/L, and the ammonium bicarbonate was 285.00g/L. The sample solution is used as a sample to be detected, namely an ammonium bicarbonate sample solution.
2. The air collecting bottle 16 with scales is filled with water firstly through the air release valve 15 and the exhaust pipe 14, then the air release valve 15 is closed, the exhaust port 7 is connected with the U-shaped pipeline 9, and the air release valve 27 is opened. The laser liquid level monitor I21 is started to track and monitor the liquid level in the gas collecting bottle 16 with scales, and the interlocking controller 24 controls the linkage control slide block 22 to move up and down so as to keep the liquid level in the laser liquid level monitor I21 and the gas collecting bottle 16 at a same height all the time. Meanwhile, the laser liquid level monitor II 23 is opened to track and monitor the liquid level in the water receiving bottle 29 with the scale marks, and the interlocking controller 24 controls the linkage control lifter 32 to ascend and descend so as to keep the liquid levels in the laser liquid level monitor II 23 and the water receiving bottle 29 with the scale marks at a same height all the time.
3. Sucking 50ml of the ammonium bicarbonate sample solution obtained in the step 1, putting the ammonium bicarbonate sample solution into a three-port reaction bottle 8, adding a magnetic stirrer, connecting a feeding constant-pressure funnel 2 with a feeding port 5, and connecting a thermometer 3 with a connecting port 6; the grinding plug 1 is opened, 50ml of sulfuric acid with the mass concentration of 50% is added into the constant pressure funnel 2, and after the addition of the sulfuric acid is finished, the grinding plug 1 is covered. The magnetic stirrer is started, the regulating valve 4 is slowly opened, and the sulfuric acid is dripped into the three-mouth reaction bottle 8 through the feeding hole 5 for reaction. Carbon dioxide gas generated by reaction in the three-mouth reaction bottle 8 is introduced into the bottom of the gas collecting bottle 16 with scales through the exhaust port 7 and the U-shaped pipeline 9, and water in the gas collecting bottle 16 is discharged into the water receiving bottle 29 with scales through the liquid discharge pipe 20 under the pushing of the carbon dioxide. Along with the increase of the amount of carbon dioxide generated by the dropwise adding reaction of sulfuric acid, the liquid level in the gas collecting bottle 16 descends, the liquid level in the gas collecting bottle 16 with scales is tracked and monitored by the laser liquid level monitor I21, and the interlocking controller 24 controls the linkage control slide block 22 to move up and down so as to keep the liquid levels in the laser liquid level monitor I21 and the gas collecting bottle 16 at a same height all the time. Meanwhile, the liquid level in the water receiving bottle 29 with the scales also rises, the laser liquid level monitor II 23 tracks and monitors the liquid level in the water receiving bottle 29 with the scales, and the interlocking controller 24 controls the lifting and the descending of the lifting device 32 in a linkage manner so as to keep the liquid levels in the laser liquid level monitor II 23 and the water receiving bottle 29 with the scales at a same height all the time.
4. Stopping adding the sulfuric acid when no carbon dioxide bubbles are generated after the sulfuric acid is addedBy reading the levels in the gas collection vial 16 and the water receiving vial 29 by a scale, a reading volume of 4.58L (4580 ml) of carbon dioxide was calculated, while the reading temperature was 24.5 ℃. Calculating the molar concentration C of carbon dioxide in the ammonium bicarbonate solution as the sample according to the formula (1) 1 Is 3.7526mol/L.
C1＝273.15×4580/((273.15+24.5)×22.4×50)＝3.7526mol/L。
5. Accurately transferring 5.0mL of the ammonium bicarbonate sample by using a pipette, transferring the ammonium bicarbonate sample into a 250mL conical flask, adding water to 80mL, adding 3 drops of methyl red indicator (0.1 percent, m/m), adjusting the solution to become red by using a 30 percent sulfuric acid solution, heating and boiling for 3min, cooling to room temperature, adjusting the solution to be red by using 0.5012mol/L sodium hydroxide solution and just disappear, adding 10mL of neutral formaldehyde solution (20 percent, m/m), standing for 5min, adding 3 drops of phenolphthalein indicator (0.1 percent, m/m)), titrating by using 0.5012mol/L sodium hydroxide standard solution until the solution does not fade within 30 seconds of reddish color, and recording the volume of the consumed sodium hydroxide standard solution to be 39.08mL. Calculated according to formula (2), C 3＝ (0.5012×39.08)/5＝3.9174mol/L；
Thus, the total ammonia content C in the sample 3 Is 3.9174mol/L.
6. Calculating the concentration of ammonium carbonate in the ammonium bicarbonate solution:
calculated according to equation (3), A 1 ＝(3.9174-3.7526)×96.09＝15.8356
Calculated according to equation (4), A 2 ＝(C 1 ×79.06)-(A 1 ×79.06÷96.09)＝(3.7526×79.06)-(15.8356×79.06÷96.09)＝283.65。
Thus, the ammonium carbonate concentration is given as A 1 Is 15.8356g/L; calculating the ammonium bicarbonate concentration according to formula (4) as A 2 Is 283.69g/L. The relative deviation of the ammonium bicarbonate concentration is only about 0.47 percent, and the relative deviation of the ammonium carbonate is about 5.33 percent, thereby meeting the production control requirement.
Experiment 2, determination of ammonium carbonate content in ammonium bicarbonate according to the method described in example 2, specifically as follows:
1. 7.576g ammonium carbonate (content 99.0%) and 23.0769g ammonium bicarbonate (content 97.5%) were transferred into a 100ml volumetric flask, and distilled water was added at room temperature to dissolve and fix the volume to 100ml, and the ammonium bicarbonate solution obtained was 75.00g/L ammonium carbonate and 225.00g/L ammonium bicarbonate.
2. The air collecting bottle 16 with scales is filled with water through the air release valve 15 and the exhaust pipe 14, then the air release valve 15 is closed, the exhaust port 7 is connected with the U-shaped pipeline 9, and the air release valve 27 is opened. And starting the laser liquid level monitor I21 to track and monitor the liquid level in the gas collecting bottle 16 with scales, and controlling the linkage control slider 22 to move up and down through the interlocking controller 24 so as to keep the liquid level in the laser liquid level monitor I21 and the gas collecting bottle 16 at a same height all the time. Meanwhile, the laser liquid level monitor II 23 is opened to track and monitor the liquid level in the water receiving bottle 29 with the scale marks, and the interlocking controller 24 controls the linkage control lifter 32 to ascend and descend so as to keep the liquid levels in the laser liquid level monitor II 23 and the water receiving bottle 29 with the scale marks at a same height all the time.
3. Sucking 50ml of the ammonium bicarbonate sample solution obtained in the step 1) and putting the ammonium bicarbonate sample solution into a three-port reaction bottle 8, adding a magnetic stirrer, connecting a feeding constant-pressure funnel 2 with a feeding port 5, and connecting a thermometer 3 with a connecting port 6; the grinding plug 1 is opened, 50ml of 50% sulfuric acid with mass concentration is added into the feeding constant pressure funnel 2, and after the addition of the sulfuric acid is finished, the grinding plug 1 is covered. The magnetic stirrer is started, the regulating valve 4 is slowly opened, and the sulfuric acid is dripped into the three-mouth reaction bottle 8 through the feeding hole 5 for reaction. Carbon dioxide gas generated by reaction in the three-mouth reaction bottle 8 is introduced into the bottom of the gas collecting bottle 16 with scales through the exhaust port 7 and the U-shaped pipeline 9, and water in the gas collecting bottle 16 is discharged into the water receiving bottle 29 with scales through the liquid discharge pipe 20 under the pushing of the carbon dioxide. Along with the increase of the amount of carbon dioxide generated by the dropwise adding reaction of sulfuric acid, the liquid level in the gas collecting bottle 16 descends, the liquid level in the gas collecting bottle 16 with scales is tracked and monitored by the laser liquid level monitor I21, and the interlocking controller 24 controls the linkage control slide block 22 to move up and down so as to keep the liquid levels in the laser liquid level monitor 21 and the gas collecting bottle 16 at a height all the time. Meanwhile, the liquid level in the graduated water receiving bottle 29 rises, the laser liquid level monitor II 23 tracks and monitors the liquid level in the graduated water receiving bottle 29, and the interlocking controller 24 controls the linkage control lifter 32 to rise and fall so as to keep the liquid levels in the laser liquid level monitor II 23 and the graduated water receiving bottle 29 at a same height all the time.
4. When no carbon dioxide bubbles are generated after the sulfuric acid is dripped, the dripping of the sulfuric acid is stopped, the liquid levels in the gas collecting bottle 16 and the water receiving bottle 29 are read through scales, the reading volume of the carbon dioxide is calculated to be 4.45L, and the reading temperature is 25.3 ℃. According to PV = nRT, under the same pressure, the gas volume of the same mole number is in direct proportion to the temperature relationship, and the molar concentration C1 of the carbon dioxide is 3.6363mol/L according to the formula (1).
5. Accurately transferring 5.0mL of the ammonium bicarbonate sample by using a pipette, transferring the ammonium bicarbonate sample into a 250mL conical flask, adding water to 80mL, adding 3 drops of methyl red indicator (0.1 percent, m/m), adjusting the solution to become red by using a 30 percent sulfuric acid solution, heating and boiling for 3min, cooling to room temperature, adjusting the solution to be red by using 0.5012mol/L sodium hydroxide solution and just disappear, adding 10mL of neutral formaldehyde solution (20 percent, m/m), standing for 5min, dropwise adding 3 drops of phenolphthalein indicator (0.1 percent, m/m), titrating by using 0.5012mol/L sodium hydroxide standard solution until the solution does not fade within 30 seconds of reddish color, and recording the volume of the consumed sodium hydroxide standard solution to be 43.96mL. The total ammonia content C in the sample was calculated according to the formula (2) 3 Is 4.4065mol/L;
6. calculation of ammonium carbonate concentration in ammonium bicarbonate solution according to equation (3) with ammonium carbonate concentration as A 1 Is 74.01g/L; calculating the ammonium bicarbonate concentration according to equation (4) as A 2 Is 226.60g/L. The relative deviation of the ammonium bicarbonate concentration is only 0.71 percent, and the relative deviation of the ammonium carbonate is 1.32 percent, thereby meeting the production control requirement.
Finally, it is also noted that the above-mentioned list is only a few specific embodiments of the present invention. Obviously, the present invention is not limited to the above embodiments, and many modifications are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the invention should be considered as within the scope of the invention.
Claims (5)
1. The measuring device for the ammonium carbonate content in the ammonium bicarbonate is characterized in that: comprises a reaction vessel, a gas collecting bottle (16), a water receiving bottle (29) and an automatic lifting interlocking system;
the reaction container is provided with a feed inlet (5), a first connecting port (6) and an exhaust port (7), and is arranged in the heating device; a constant pressure funnel (2) for feeding is arranged at the feed inlet (5), and an outlet of the constant pressure funnel (2) is communicated with the feed inlet (5) through an adjusting valve (4);
the gas collecting bottle (16) is a bottle body with scales and is in an inverted state, and a bottle mouth plug (18) is arranged at the bottle mouth of the gas collecting bottle (16); the inner cavity of the bottle bottom of the gas collecting bottle (16) is communicated with a first exhaust pipe (14) through a vent valve (15);
the water receiving bottle (29) is a bottle body with scales, a bottle stopper (28) is arranged at the bottle mouth of the water receiving bottle (29), and the exhaust pipe II (26) penetrates through the bottle stopper (28) in a sealing manner and is communicated with the inner cavity of the water receiving bottle (29); a second connecting port (30) is arranged on the side wall of the water receiving bottle (29) close to the bottom; the water receiving bottle (29) is arranged on a lifting platform (31), and a linkage control lifter (32) with a lifting motor is arranged at the bottom of the lifting platform (31);
one end of the U-shaped pipeline (9) is hermetically connected with the exhaust port (7), and the other end of the U-shaped pipeline hermetically penetrates through the bottle mouth plug (18) and then reaches the bottom of the gas collecting bottle (16);
the mounting height of the reaction vessel is higher than that of the gas collecting bottle (16);
one end of the liquid discharge pipe (20) hermetically penetrates through the bottle mouth plug (18) and then is communicated with the inner cavity of the gas collection bottle (16); the other end of the liquid discharge pipe (20) is hermetically connected with a second connecting port (30) of the water receiving bottle (29);
the automatic lifting interlocking system comprises a laser liquid level monitor I (21), a laser liquid level monitor II (23), a linkage control slide block (22), an interlocking controller (24) and a linkage control lifter (32); the laser liquid level monitor I (21) is used for monitoring the liquid level of the gas collecting bottle (16), the laser liquid level monitor II (23) is used for monitoring the liquid level of the water receiving bottle (29), the linkage control slide block (22) is a slide block with a motor, and the linkage control slide block (22) is sleeved on the iron support platform II (25) and is movably connected with the iron support platform II (25); the linkage control slide block (22) is fixedly connected with the laser liquid level monitor I (21) and the laser liquid level monitor II (23) respectively;
the laser liquid level monitor I (21), the laser liquid level monitor II (23), a motor of the linkage control slide block (22) and a lifting motor of the linkage control lifter (32) are respectively connected with the interlocking controller (24) through signals.
2. The apparatus for determining the ammonium carbonate content in ammonium bicarbonate according to claim 1, wherein:
a thermometer is arranged at the first connecting port (6);
the inlet of the constant pressure funnel (2) is provided with a grinding plug (1).
3. The apparatus for determining the ammonium carbonate content in ammonium bicarbonate according to claim 2, wherein:
the bottom of the gas collecting bottle (16) is respectively connected with a thermometer and a pressure gauge.
4. The apparatus for determining the ammonium carbonate content in ammonium bicarbonate according to claim 3, wherein:
a fixing ring (17) is arranged on the outer surface of the gas collecting bottle (16), and the fixing ring (17) is fixed with a first iron support (19).
5. The apparatus for determining the ammonium carbonate content in ammonium bicarbonate according to claim 4, wherein:
a magnetic stirrer is arranged in the reaction vessel.
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