CN114570183B - Derivatization reaction device for urea hydrolysis sediment - Google Patents

Derivatization reaction device for urea hydrolysis sediment Download PDF

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CN114570183B
CN114570183B CN202210199610.3A CN202210199610A CN114570183B CN 114570183 B CN114570183 B CN 114570183B CN 202210199610 A CN202210199610 A CN 202210199610A CN 114570183 B CN114570183 B CN 114570183B
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end cover
section
derivatization reaction
reaction tube
silane
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CN114570183A (en
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向小凤
张向宇
张波
刘雯
王志超
姚伟
徐宏杰
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Xian Thermal Power Research Institute Co Ltd
Huaneng Group Technology Innovation Center Co Ltd
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Xian Thermal Power Research Institute Co Ltd
Huaneng Group Technology Innovation Center Co Ltd
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/77—Liquid phase processes
    • B01D53/78—Liquid phase processes with gas-liquid contact
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/26—Drying gases or vapours
    • B01D53/28—Selection of materials for use as drying agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/30—Controlling by gas-analysis apparatus
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/54—Nitrogen compounds
    • B01D53/56—Nitrogen oxides
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • B01J19/2415—Tubular reactors
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
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    • B01D2253/102—Carbon
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    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
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    • B01D2253/104—Alumina
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B01D2253/106—Silica or silicates
    • B01D2253/108—Zeolites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/40011—Methods relating to the process cycle in pressure or temperature swing adsorption
    • B01D2259/40043—Purging
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D2259/00—Type of treatment
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    • B01D2259/40011—Methods relating to the process cycle in pressure or temperature swing adsorption
    • B01D2259/40043—Purging
    • B01D2259/4005—Nature of purge gas
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Abstract

The invention provides a derivatization reaction device for urea hydrolysis sediment, which is simple to operate, obvious in effect, capable of improving the safety and stability of the derivatization reaction, economical and feasible. Comprises a silane derivatization reaction tube and an end cover arranged at the top of the silane derivatization reaction tube; the end cover is of a three-section type and comprises a first end cover section, a second end cover section and a third end cover section which are sequentially and rotatably connected, the bottom of the third end cover section is connected with the top of the silane derivatization reaction tube, and each section of end cover is correspondingly provided with two through holes which are respectively used for injecting nitrogen and reagents.

Description

Derivatization reaction device for urea hydrolysis sediment
Technical Field
The invention relates to the technical field of flue gas denitration of thermal power plants, in particular to a derivatization reaction device for urea hydrolysis sediments.
Background
The urea solution forms solid crystal components mainly comprising urea in the hot air atmosphere at the temperature of 150 ℃; biuret (biuret), cyanuric acid, ammelide are predominant at 150-250 ℃; above 250 ℃ predominantly ammelide. Under the action of the catalyst, the rate of the isocyanate substance undergoing hydrolysis reaction in the urea aqueous solution is greatly increased, and the biuret produced by the reaction with the urea also undergoes hydrolysis reaction under the action of the hydrolysis catalyst.
Aiming at the complexity of byproducts in the catalytic hydrolysis process of urea, the addition of the catalyst promotes the hydrolysis reaction and incomplete decomposition of the byproducts, so that the generated byproducts deposit and block pipelines, even corrosion faults occur, and the generated byproducts (such as isocyanic acid deposits caused by biuret) cause pipeline blocking and corrosion faults. Complex deposits are difficult to detect using analytical instruments such as GC-MS. In particular, cyanuric acid homologues (such as cyanuric acid, ammelide, ammeline and the like) have the problems of high boiling point, poor thermal stability and easy decomposition by heating in the detection process of a gas chromatograph, and are difficult to detect.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides the derivatization reaction device for the urea hydrolysis sediment, which has the advantages of simple operation and obvious effect, improves the safety and stability of the derivatization reaction, and is economical and feasible.
In order to achieve the purpose, the invention provides the following technical scheme:
a derivatization reaction device for urea hydrolysis sediment comprises a silane derivatization reaction tube and an end cover arranged at the top of the silane derivatization reaction tube;
the end cover is of a three-section type and comprises a first end cover section, a second end cover section and a third end cover section which are sequentially and rotatably connected, the bottom of the third end cover section is connected with the top of the silane derivatization reaction tube, and each end cover section is correspondingly provided with two through holes which are respectively used for injecting nitrogen and reagents.
Preferably, the first end cover section, the second end cover section and the third end cover section are all of cylindrical structures with the same diameter, wherein the first end cover section and the second end cover section are solid, the third end cover section is hollow, a drying agent is filled in the third end cover section, and a plurality of small holes are uniformly distributed in the end face of the bottom of the third end cover section.
Preferably, the desiccant is physically adsorbed desiccant selected from silica gel, alumina gel, molecular sieve, activated carbon, bone charcoal and mineral desiccant.
Preferably, the silane derivatization reaction tube adopts a cylindrical sharp-bottomed glass tube with a pointed bottom.
Preferably, the diameter of the silane derivatization reaction tube ranges from 10 to 20mm.
Preferably, the end caps are of a size that is consistent with the size of the silane derivatization reaction tubes.
Preferably, the through hole is filled with sealing rubber.
Preferably, the through-hole includes a nitrogen purge needle insertion hole for injecting nitrogen, the size of which is determined according to the selected nitrogen gas needle specification, and a reagent needle insertion hole for injecting a reagent, the size of which is determined according to the selected reagent needle specification.
Preferably, the end cover is made of brown light-proof glass material.
Preferably, the through hole is a circular through hole.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a derivatization reaction device of urea hydrolysis sediment, which designs a silane derivatization reaction tube with a special structure, the top of the silane derivatization reaction tube is provided with an end cover with a three-section structure, the end cover comprises a first end cover section, a second end cover section and a third end cover section, two through holes are respectively arranged at the corresponding positions of each end cover section and are respectively used for injecting nitrogen and reagents, a urea hydrolysis sediment sample is extracted by a solvent and then inserted into the through holes through a reagent needle to complete injection, the end cover with the three-section structure can ensure the sealing property of the injected reagent, simultaneously, the water removal and purging process of pretreatment is carried out on the extracted reagent before the extracted reagent enters a silane derivatization reaction tube for silanization reaction, after the pretreatment of nitrogen purging and concentration is carried out on the extracting solution, the dust which can pollute the extracting solution and possibly exists in the pipeline before the reaction can be removed, the subsequent silanization reaction influenced by the reaction of the air remained in the pipeline and the extracting solution is avoided, in addition, the volatile matter of the extracting solution and the air are prevented from forming explosive mixture, the safety of the reaction is improved, the accuracy and the stability of the silanization reaction are further improved, after the silanization reaction is carried out by the derivatization reaction device of the urea hydrolysis sediment, polar groups such as-NH, -OH and the like contained in the molecular structure of the derivative sediment of the silanization reagent are utilized to avoid the problems of high boiling point and difficult vaporization, improve the thermal stability of the silanization derivative, when the gas chromatography-mass spectrometer is used for detecting the sediment subsequently, the sediment components which are easy to capture are subjected to chromatographic analysis of the relevant sediment components, so that the sediment components are subjected to peak appearance in a GC-MS monitoring ion mode, the chromatographic behavior is improved, and the main components of the sediment are subjected to quantitative analysis and judgment.
According to the derivatization reaction device for urea hydrolysis sediment, the three sections of end covers can be opened and closed in a rotating mode, the nitrogen inlet path of the reaction tube can be closed when any more than one section of end cover rotates, and the nitrogen inlet path is opened by three sections of rotation consistently. The mode of opening and closing the end cover at will can meet the requirements of storing and sealing the silane reagent in the reaction tube and sealing the sample after the derivatization treatment.
Furthermore, the third section of the end cover is a drying agent filling section, and the cross section of the bottom end of the third section of the end cover is provided with a plurality of uniformly distributed small holes so as to facilitate water adsorption, inhibit hydrolysis reaction of urea hydrolysis byproducts and avoid the problems that the generated byproducts are hydrolyzed or incompletely decomposed to cause deposit to block a pipeline and even cause corrosion faults as far as possible.
Drawings
FIG. 1 is a schematic structural view of a derivatization reaction apparatus according to the present invention;
FIG. 2 is a schematic view of a third segment of the end cap with a through hole in the top end face;
FIG. 3 is a schematic view of a bottom end face through hole of a third section of an end cap;
FIG. 4 is a schematic view of a three-section end cap opening;
FIG. 5 is a schematic closure of one embodiment of a three-piece end cap.
In the figure, a silane derivatization reaction tube 1, an end cover first section 2, an end cover second section 3, an end cover third section 4, a nitrogen purging needle insertion hole 5, a reagent needle insertion hole 6, a top end face 7 of the end cover third section 4 and a bottom end face 8 of the end cover third section 4.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the accompanying drawings:
as shown in fig. 1, the derivatization reaction device for urea hydrolysis sediment according to the present invention includes a silane derivatization reaction tube 1 and an end cap disposed on the top of the silane derivatization reaction tube 1;
the end cover is of a three-section type and comprises an end cover first section 2, an end cover second section 3 and an end cover third section 4 which are sequentially and rotatably connected, as shown in fig. 2, the bottom of the end cover third section 4 is connected with the top of the silane derivatization reaction tube 1, and each end cover is correspondingly provided with two through holes which are respectively used for injecting nitrogen and reagents.
The invention provides a derivatization reaction device of urea hydrolysis sediment, which is characterized in that a silane derivatization reaction tube with a special structure is designed, an end cover with a three-section structure is arranged at the top of the silane derivatization reaction tube, the end cover comprises an end cover first section 2, an end cover second section 3 and an end cover third section 4, two through holes are respectively arranged at the corresponding positions of each section of the end cover and are respectively used for injecting nitrogen and an injection reagent, a urea hydrolysis sediment sample is extracted by a solvent and then inserted into the through holes through a reagent needle head to complete injection, the end cover with the three-section structure can ensure the sealing property of the injection reagent, simultaneously, a water removal and purging process of pretreatment is carried out before the extracted reagent enters the silane derivatization reaction tube for silanization reaction, and after the extraction solution is pretreated by nitrogen purging and concentration, dust which can pollute the extraction solution and possibly exist in the pipeline before the reaction can be removed, the subsequent silanization reaction is prevented from being influenced by the reaction of air and the extracting solution which are reserved in a pipeline, in addition, the volatile matter of the extracting solution and the air are prevented from forming an explosive mixture, the safety of the reaction is improved, the accuracy and the stability of the silanization reaction are further improved, after the silanization reaction is carried out by the derivatization reaction device of the urea hydrolysis sediment, polar groups such as-NH, -OH and the like in the molecular structure of the sediment component are derived by using a silanization reagent, the problems of high boiling point and difficult vaporization are avoided, the thermal stability of the silanization derivative can be improved, when the sediment is detected by using a gas chromatography-mass spectrometer in the subsequent process, the chromatographic analysis of related sediment components is captured more easily, so that the peak is generated under the monitoring ion mode of GC-MS, and the chromatographic behavior is improved, and (4) carrying out quantitative analysis and judgment on the main components of the deposit.
As shown in fig. 4 and 5, the three end caps of the derivatization reaction device for urea hydrolysis sediment according to the present invention can be opened and closed by rotation, and when a sealed closed state is required, only one or more end caps need to be rotated to allow two through holes of the three end caps to be not communicated with each other, thereby closing the nitrogen inlet path of the reaction tube, and when a gas and a reagent need to be introduced for reaction, only the through holes of the three end caps need to be rotated uniformly and are completely communicated with each other, thereby opening the nitrogen inlet path. The mode of opening and closing the end cover at will can meet the requirements of storing and sealing the silane reagent in the reaction tube and sealing a sample after derivatization treatment, and has simple and convenient operation and strong practicability.
Further, the first end cover section 2, the second end cover section 3 and the third end cover section 4 are all of cylindrical structures with the same diameter, wherein the first end cover section 2 and the second end cover section 3 are made of common glass solids, two through holes are formed from the top end surface to the bottom end surface of the first end cover section 2, and are respectively a first nitrogen purging needle hole 5 and a first reagent needle insertion hole 6, two through holes are formed from the top end surface to the bottom end surface of the second end cover section 3, and are respectively a second nitrogen purging needle hole 5 and a second reagent needle insertion hole 6, the third end cover section 4 is hollow, a drying agent is filled in the third end cover section 4, two through holes corresponding to the two end covers are formed from the top end surface 7 of the third end cover section 4, and are respectively a third nitrogen purging needle hole 5 and a third reagent needle insertion hole 6, and as shown in fig. 3, a plurality of small holes are uniformly distributed on the bottom end surface 8 of the third end cover section 4. The third section 4 of the end cover is a drying agent filling section, and a plurality of small holes which are uniformly distributed are arranged on the bottom end face 8 of the third section 4 of the end cover, so that water is adsorbed, hydrolysis reaction of urea hydrolysis byproducts is inhibited, and the problems that the pipeline is blocked by sediments and even corrosion faults are caused due to incomplete hydrolysis or decomposition of the generated byproducts are avoided as far as possible.
Preferably, the desiccant is one of physically adsorbed desiccants such as silica gel, alumina gel, molecular sieves, activated carbon, bone charcoal and mineral desiccants, and is used for adsorbing moisture of introduced gas, keeping reaction dryness on the basis of not influencing chemical reaction and inhibiting hydrolysis. In this embodiment, the third section 4 of the end cap is filled with physically adsorbed silica gel desiccant.
In this embodiment, the silane derivatization reaction tube 1 is a cylindrical sharp-bottomed glass tube with a pointed bottom.
Preferably, the diameter of the silane derivatization reaction tube 1 is in the range of 10-20mm, and the silane derivatization reaction is carried out by adopting a glass reaction tube with the diameter of 10-20mm through experimental judgment and empirical judgment of actual working condition requirements.
The size specification of the end cover is consistent with that of the silane derivatization reaction tube 1, and the sealing performance of the whole derivatization reaction device can be ensured.
And sealing rubber is filled in the through hole, so that the sealing performance of the whole derivatization reaction device is further ensured, and other impurities cannot be introduced.
The through hole comprises a nitrogen purging needle inserting hole 5 for injecting nitrogen and a reagent needle inserting hole 6 for injecting a reagent, wherein the aperture size of the nitrogen purging needle inserting hole 5 is determined according to the selected nitrogen gas needle specification, the aperture size of the reagent needle inserting hole 6 is determined according to the selected reagent needle specification, and the selected nitrogen gas needle specification and the selected reagent needle specification are selected according to actual working condition requirements.
Preferably, the end cover is made of brown light-proof glass material.
The through hole is a circular through hole, the diameter of the through hole is slightly larger than the selected nitrogen gas needle specification and the selected reagent needle head specification, the through hole is matched with the nitrogen gas needle reagent needle head, and the through hole can be just inserted into the through hole.
The invention relates to a derivatization reaction device of urea hydrolysis sediment, which uses the working principle as follows:
centrifuging and standing the prepared sediment solution in a laboratory to layer the solution, and extracting supernatant liquid as a sample;
performing silanization water removal pretreatment on the sample, injecting an extracting solution from a through hole of the reagent needle insertion hole 6 through a needle, and injecting nitrogen into a through hole of the nitrogen purging needle insertion hole 5 for drying;
after the pretreatment is finished, the derivatization reaction device is placed in a constant-temperature heating device, excessive silanization reagent is injected into a silane derivatization reaction tube 1 through a needle head according to the amount of a sample for derivatization reaction, the excessive silanization reagent can reduce the adsorption on the surface of a container and a small amount of water which possibly exists, and after the derivatization reaction is finished, the solution is sent to GC-MS for detecting the components of the sediment.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (6)

1. A derivatization reaction device for urea hydrolysis sediment is characterized by comprising a silane derivatization reaction tube (1) and an end cover arranged at the top of the silane derivatization reaction tube (1);
the end cover is of a three-section type and comprises an end cover first section (2), an end cover second section (3) and an end cover third section (4) which are sequentially and rotatably connected, the bottom of the end cover third section (4) is connected with the top of the silane derivatization reaction tube (1), and each end cover is correspondingly provided with two through holes which are respectively used for injecting nitrogen and reagents;
the first end cover section (2), the second end cover section (3) and the third end cover section (4) are all of cylindrical structures with the same diameter, wherein the first end cover section (2) and the second end cover section (3) are solid, the third end cover section (4) is hollow, a drying agent is filled in the third end cover section (4), and a plurality of small holes are uniformly distributed on the bottom end face (8) of the third end cover section (4);
the desiccant is physically adsorbed by any one of silica gel, alumina gel, molecular sieve, active carbon, bone charcoal and mineral desiccant;
the size specification of the end cover is consistent with that of the silane derivatization reaction tube (1);
sealing rubber is filled in the through hole;
the three-section type end covers can be opened and closed in a rotating mode, the nitrogen inlet path of the reaction tube can be closed by rotating more than one section of end cover, the nitrogen inlet path can be opened by rotating the three sections consistently, and the storage and sealing of a silane reagent in the reaction tube and the sealing of a sample after derivative treatment can be met by opening the closed end cover at will.
2. The apparatus for derivatization of urea-hydrolyzed deposits according to claim 1, wherein the silane derivatization reaction tube (1) is a cylindrical sharp-bottomed glass tube with a pointed bottom.
3. The apparatus for derivatization of urea hydrolysis deposits according to claim 2, wherein the diameter of the silane derivatization reaction tube (1) is in the range of 10-20mm.
4. The apparatus for derivatization reaction of urea hydrolysis sediment according to claim 1, wherein the through holes comprise a nitrogen purge needle hole (5) for injecting nitrogen and a reagent needle insertion hole (6) for injecting a reagent, wherein the nitrogen purge needle hole (5) has a pore size determined according to the selected nitrogen needle specification, and the reagent needle insertion hole (6) has a pore size determined according to the selected reagent needle specification.
5. The apparatus for the derivatization reaction of urea hydrolysis deposits according to claim 1, wherein the end cap is made of brown light-resistant glass.
6. The apparatus for the derivatization reaction of urea-hydrolyzed sediment according to claim 1, wherein the through-holes are circular.
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