Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a urea hydrolysate measuring system and method, which are simple in structure, reasonable in design, convenient to operate, accurate and efficient in grading measurement.
The invention is realized by the following technical scheme:
a urea hydrolysate measuring system comprises a high-temperature heat tracing sampling pipe, a steam absorption tank group, an ammonia absorption tank group, a carbon dioxide absorption tank group, a first wastewater pool, a second wastewater pool, an ice water bath pool, a valve group and a metering group;
the inlet end of the high-temperature heat tracing sampling pipe is connected with an ammonia supply mother pipe of the urea hydrolysis reactor, the first outlet end of the high-temperature heat tracing sampling pipe is connected with a first wastewater pool, and the second outlet end of the high-temperature heat tracing sampling pipe is sequentially connected with a steam absorption pool group, an ammonia absorption pool group, a carbon dioxide absorption pool group and a second wastewater pool; the first wastewater pool, the ammonia absorption pool group, the carbon dioxide absorption pool group and the second wastewater pool are respectively arranged in the ice water bath pool;
the valves in the valve group are respectively arranged on the pipelines between the inlet end of the high-temperature heat tracing sampling pipe and the first outlet end and the second outlet end;
the metering group comprises a pressure gauge and a mass flowmeter; the pressure gauge and the mass flow meter are sequentially arranged on a pipeline between the inlet end and the first outlet end of the high-temperature heat tracing sampling pipe.
Further, the valve group comprises a first ball valve, a second ball valve, a third ball valve, a fourth ball valve and a pressure reducing valve; the first ball valve, the pressure reducing valve and the second ball valve are sequentially arranged on the high-temperature heat tracing sampling pipe in front of the pressure gauge along the gas flowing direction; and the third ball valve and the fourth ball valve are respectively arranged on the first outlet end and the second outlet end of the high-temperature heat tracing sampling pipe.
Furthermore, the steam absorption tank is arranged in the heat preservation groove and comprises a first steam absorption tank and a second steam absorption tank which are connected in sequence, and color-changing silica gel absorbents are filled in the first steam absorption tank and the second steam absorption tank.
Furthermore, the first steam absorption tank and the second steam absorption tank are both arranged in a U-shaped pipe.
Furthermore, the ammonia gas absorption tank group comprises a first ammonia gas absorption tank and a second ammonia gas absorption tank, wherein dilute sulfuric acid absorption liquid is filled in the first ammonia gas absorption tank and the second ammonia gas absorption tank, and the first ammonia gas absorption tank and the second ammonia gas absorption tank are respectively arranged in the ice water bath; the first ammonia absorption tank and the second ammonia absorption tank are sequentially connected through a siphon; the first ammonia absorption tank is connected with the second steam absorption tank through a siphon.
Still further, the carbon dioxide absorption tank group comprises a first carbon dioxide absorption tank and a second carbon dioxide absorption tank, wherein calcium hydroxide absorption liquid is filled in the first carbon dioxide absorption tank and the second carbon dioxide absorption tank, and the first carbon dioxide absorption tank and the second carbon dioxide absorption tank are respectively arranged in the ice water bath; the first carbon dioxide absorption tank and the second carbon dioxide absorption tank are sequentially connected through a siphon pipe; the first carbon dioxide absorption tank is connected with the second ammonia absorption tank through a siphon.
A method for measuring urea hydrolysate comprises the following steps,
step one, using a urea solution with the mass fraction of 50%, keeping the temperature and the pressure of a urea hydrolysis reactor stable, and controlling a ball valve group to enable mixed gas to flow into a first wastewater tank through a regulating pressure gauge and a mass flow meter;
after the pressure and the flow are stable, the control ball valve group enables the mixed gas to sequentially pass through the steam absorption pool group, the ammonia absorption pool group, the carbon dioxide absorption pool group and the second wastewater pool, sampling and collection are carried out for a fixed time, and the accumulated mass and the volume of the mixed gas are calculated through a mass flow meter; respectively obtaining the volume fractions of water vapor, ammonia gas and carbon dioxide in the mixed gas through a vapor absorption tank group, an ammonia gas absorption tank group and a carbon dioxide absorption tank group;
and step three, changing the mass fraction of the proportioned urea solution and the operating pressure and temperature of the urea hydrolysis reactor, repeating the step one and the step two to measure the volume fraction ratio of the vapor, the ammonia gas and the carbon dioxide gas in the mixed gas, and finding out the reasonable operating parameter of the maximum ammonia production ratio.
Further, the volume fraction of the water vapor in the mixed gas is obtained through the steam absorption tank group, and the volume fraction of the water vapor in the mixed gas is obtained by specifically adopting the weight difference before and after the steam absorption tank group absorbs the mixed gas.
Further, the volume fraction of the carbon dioxide in the mixed gas is respectively obtained through the carbon dioxide absorption tank group, and specifically, the volume fraction of the carbon dioxide in the mixed gas is obtained through the weight difference before and after the carbon dioxide absorption tank group absorbs the mixed gas.
Further, the volume fraction of the ammonia gas in the mixed gas is obtained through an ammonia gas absorption tank, the concentration of ammonium ions in the ammonia gas absorption liquid is obtained by specifically adopting an ammonia electrode measurement method, and then the volume fraction of the ammonia gas in the mixed gas is obtained.
Compared with the prior art, the invention has the following beneficial technical effects:
according to the system, a high-temperature heat tracing sampling pipe is connected with an ammonia supply main pipe of a urea hydrolysis reactor, and the high-temperature heat tracing sampling pipe passes through a steam absorbent in a steam absorption tank set, an ammonia absorption liquid in the ammonia absorption tank set and a carbon dioxide absorption liquid in the carbon dioxide absorption tank set in sequence, and the maximum ammonia production ratio under the economical efficiency and the coordination of the hydrolysis reactor is finally obtained by matching a pressure gauge and a mass flow meter according to the difference of the concentration of urea solutions and the difference of the reaction temperature and the reaction pressure of the hydrolysis reactor, so that the measurement problem of the components and the concentration of urea hydrolysis products is solved, the ammonia production under the economical efficiency and the coordination of the urea hydrolysis reactor is realized, and the stable flue gas denitration of a boiler unit is realized; meanwhile, waste water can be effectively collected by adopting a mode of arranging the first waste water tank and the second waste water tank, and the ice water bath tank is arranged at the waste water tank, the ammonia absorption tank group and the carbon dioxide absorption tank group, so that the temperature can be controlled to be favorable for absorbing gas by the absorption liquid.
Furthermore, the system controls the flow condition of the mixed gas in the high-temperature heat tracing sampling pipe before the pressure gauge by arranging the first ball valve, the pressure reducing valve and the second ball valve, controls the flow condition of the mixed gas in the first outlet end of the high-temperature heat tracing sampling pipe by the third ball valve, and controls the flow condition of the mixed gas in the second outlet end of the high-temperature heat tracing sampling pipe by the fourth ball valve, so that corresponding pipelines can be opened and closed in time as required, and the high efficiency and accuracy of measurement are ensured.
Furthermore, the system adopts two steam absorption tanks which are sequentially connected in series, and the allochroic silica gel absorbent is arranged in the steam absorption tanks, so that the steam in the mixed gas can be absorbed more fully and effectively, and the accuracy of the measurement result is ensured; meanwhile, the heat-insulating material is placed in a heat-insulating groove, so that the heat loss of gas is reduced.
Furthermore, the system of the invention can ensure that the steam in the mixed gas is effectively dried by adopting the two steam absorption tanks which are arranged in the shape of the U-shaped pipe.
Furthermore, the system adopts two ammonia absorption tanks which are sequentially connected in series and are internally provided with dilute sulfuric acid absorption liquid, so that ammonia in the mixed gas can be absorbed more fully and effectively, and the accuracy of a measurement result is ensured; meanwhile, the first ammonia absorption tank and the second steam absorption tank are connected through the siphon, and therefore continuous subsequent side measurement is convenient to carry out.
Furthermore, the system adopts two carbon dioxide absorption tanks which are sequentially connected in series and are internally provided with calcium hydroxide absorption liquid, so that the carbon dioxide in the mixed gas can be absorbed more fully and effectively, and the accuracy of the measurement result is ensured; meanwhile, the first carbon dioxide absorption tank and the second ammonia absorption tank are connected through the siphon, and therefore continuous subsequent side measurement is conveniently carried out.
The method provided by the invention comprises the steps of analyzing the proportion of each component and volume fraction in the urea hydrolysate mixed gas by adopting a gravimetric analysis method and an ammonium ion electrode method, finding out the reasonable operation parameter of the maximum ammonia yield ratio through the test of a urea hydrolysate measuring system, obtaining the maximum ammonia yield ratio under the economical efficiency and coordination of a hydrolysis reactor, and realizing the ammonia yield under the economical efficiency and coordination of the urea hydrolysis system.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
In order to achieve the above object, the present invention provides a urea hydrolysate measurement system, as shown in fig. 1, comprising a urea hydrolysis reactor 1, an ammonia supply main pipe 2, a high temperature heat tracing sampling pipe 11, a valve group consisting of first, second, third and fourth ball valves 3, 5, 8 and 10 and a pressure reducing valve 4, an ice water bath tank 19 and a heat preservation tank 20, a metering group consisting of a pressure gauge 6 and a mass flow meter 7, a first wastewater tank 9, a second wastewater tank 18, a vapor absorption tank group consisting of a first vapor absorption tank 12 and a second vapor absorption tank 13 respectively filled with a allochroic silica gel absorbent (desiccant) and placed in the heat preservation tank 20, an ammonia absorption tank group consisting of a first ammonia absorption tank 14 and a second ammonia absorption tank 15 respectively filled with a dilute sulfuric acid absorption liquid, and a carbon dioxide absorption tank group consisting of a first carbon dioxide absorption tank 16 and a second carbon dioxide absorption tank 17 respectively filled with a calcium hydroxide absorption liquid, the first wastewater pool 9, the ammonia absorption pool group, the carbon dioxide absorption pool group and the second wastewater pool 18 are respectively placed in an ice-water bath pool 19, and a high-temperature heat tracing heat preservation mode is adopted before the pipeline enters the U-shaped pipe, so that the temperature of the sampled gas is kept as much as possible;
an ammonia supply main pipe 2 of the urea hydrolysis reactor 1 is connected with the inlet end of a high-temperature heat tracing sampling pipe 11, and a first ball valve 3, a pressure reducing valve 4, a second ball valve 5, a pressure gauge 6 and a mass flow meter 7 are sequentially arranged on a pipeline between the high-temperature heat tracing sampling pipe and the pressure reducing valve along the gas flowing direction; a first outlet end of the high-temperature heat tracing sampling pipe 11 is connected with a first wastewater pool 9, a third ball valve 8 is arranged on a pipeline between the high-temperature heat tracing sampling pipe and the wastewater pool, and a second outlet end of the high-temperature heat tracing sampling pipe is sequentially connected with a first steam absorption pool 12, a second steam absorption pool 13, a first ammonia absorption pool 14, a second ammonia absorption pool 15, a first carbon dioxide absorption pool 16, a second carbon dioxide absorption pool 17 and a second wastewater pool 18.
The first steam absorption tank 12 and the second steam absorption tank 13 are both arranged in a U-shaped pipe; the first steam absorption tank 12, the second steam absorption tank 13, the first ammonia absorption tank 14, the second ammonia absorption tank 15, the first carbon dioxide absorption tank 16, the second carbon dioxide absorption tank 17 and the second wastewater tank 18 are connected in sequence through siphons respectively.
In practical application, in the preferred embodiment, a urea solution with a mass fraction of 50% is used, when the temperature of the urea hydrolysis reactor 1 is stabilized at 130 ℃ and the pressure is stabilized at 0.60MPa, the first ball valve 3, the high-temperature pressure reducing valve 4, the second ball valve 5 and the third ball valve 8 are opened, the fourth ball valve 10 is closed, the mixed gas flows into the first wastewater tank 9, when the pressure and the flow are stabilized, the third ball valve 8 is closed, and the fourth ball valve 10 is opened, so that the mixed gas sequentially passes through the allochroic silica gel absorbent in the U-shaped first steam absorption tank 12 and the U-shaped second steam absorption tank 13, the dilute sulfuric acid absorption liquid in the first ammonia absorption tank 14 and the second ammonia absorption tank 15, and the calcium hydroxide absorption liquid in the first carbon dioxide absorption tank 16 and the second carbon dioxide absorption tank 17;
sampling and collecting for 5-10 minutes, and calculating the accumulated mass and volume of the mixed gas through a mass flowmeter 7;
the weight difference before and after the mixed gas is absorbed by the allochroic silica gel absorbent in the first steam absorption tank 12 and the second steam absorption tank 13 and the calcium hydroxide absorption liquid in the first carbon dioxide absorption tank 16 and the second carbon dioxide absorption tank 17 is used for further obtaining the volume fraction of the water vapor and the carbon dioxide in the mixed gas, and the ammonium ion concentration in the ammonia absorption liquid is obtained by an ammonia electrode measurement method so as to obtain the volume fraction of the ammonia in the mixed gas; specifically, the dilute sulfuric acid solution absorbing ammonia gas is obtained by measuring in a chemical laboratory through an ammonia gas sensitive electrode method;
and then changing the mass fraction of the urea solution to be proportioned and the operating pressure and temperature of the urea hydrolysis reactor 1, measuring the volume fraction ratio of the vapor, the ammonia gas and the carbon dioxide gas in the mixed gas, finding out the reasonable operating parameters of the maximum ammonia production ratio, further realizing the ammonia production of the urea hydrolysis system under the conditions of economy and coordination, and achieving the flue gas denitration of the stability of the coal-fired unit.
On the basis of the system, the invention also provides a urea hydrolysate measuring method, which comprises the following steps,
in the first step of the method,
using a urea solution with the mass fraction of 50%, keeping the temperature and the pressure of the urea hydrolysis reactor 1 stable, and controlling a ball valve group to enable mixed gas to flow into a first wastewater tank 9 through a regulating pressure gauge 6 and a mass flow meter 7;
after the pressure and the flow are stable, the control ball valve group enables the mixed gas to sequentially pass through the steam absorption tank group, the ammonia absorption tank group, the carbon dioxide absorption tank group and the second wastewater tank 18, sampling and collection are carried out for a fixed time, and the accumulated mass and the volume of the mixed gas are calculated through the mass flowmeter 7; respectively obtaining the volume fractions of water vapor, ammonia gas and carbon dioxide in the mixed gas through a vapor absorption tank group, an ammonia gas absorption tank group and a carbon dioxide absorption tank group;
and step three, changing the mass fraction of the proportioned urea solution and the operating pressure and temperature of the urea hydrolysis reactor 1, repeating the step one and the step two to measure the volume fraction ratio of the vapor, the ammonia gas and the carbon dioxide gas in the mixed gas, and finding out the reasonable operating parameter of the maximum ammonia production ratio.
The steam volume fraction in the mixed gas is obtained through the steam absorption tank group, and the steam volume fraction in the mixed gas is obtained through the weight difference before and after the steam absorption tank group absorbs the mixed gas.
The carbon dioxide volume fraction in the mixed gas is obtained through the carbon dioxide absorption tank group, and the carbon dioxide volume fraction in the mixed gas is obtained through the weight difference before and after the carbon dioxide absorption tank group absorbs the mixed gas.
And specifically, the ammonia gas volume fraction in the mixed gas is obtained by adopting an ammonia electrode measurement method, and the ammonia gas volume fraction in the mixed gas is obtained.