CN114715915A - Novel urea catalytic hydrolysis method and device - Google Patents

Novel urea catalytic hydrolysis method and device Download PDF

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Publication number
CN114715915A
CN114715915A CN202210498858.XA CN202210498858A CN114715915A CN 114715915 A CN114715915 A CN 114715915A CN 202210498858 A CN202210498858 A CN 202210498858A CN 114715915 A CN114715915 A CN 114715915A
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urea
hydrolyzer
phosphate
pipeline
solution
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CN202210498858.XA
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Chinese (zh)
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西孟颖
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Beijing Xinye Technology Co ltd
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Beijing Xinye Technology Co ltd
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Priority to CN202210498858.XA priority Critical patent/CN114715915A/en
Publication of CN114715915A publication Critical patent/CN114715915A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00Ammonia; Compounds thereof
    • C01C1/02Preparation, purification or separation of ammonia
    • C01C1/08Preparation of ammonia from nitrogenous organic substances
    • C01C1/086Preparation of ammonia from nitrogenous organic substances from urea
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/52Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Exhaust Gas After Treatment (AREA)

Abstract

The invention discloses a novel urea catalytic hydrolysis method and a device, wherein a phosphate mixture is added into a urea hydrolysis reactor as a catalyst, a urea solution with the mass concentration of 50% is sent to the urea hydrolysis reactor, the temperature of the urea hydrolysis reactor is controlled at 140 ℃ and the pressure is controlled at 0.35-0.55MPa, urea is subjected to catalytic hydrolysis, the phosphate mixture is a mixture of potassium dihydrogen phosphate, ammonium dihydrogen phosphate and diammonium hydrogen phosphate with different proportions, the filling amount is 5-10% of the volume of a hydrolyzer, the loading amount of the urea solution is 50% of the volume of the hydrolyzer, the proportion of the ammonium dihydrogen phosphate in the phosphate mixture is 50-70%, the proportion of the potassium dihydrogen phosphate in the phosphate mixture is 10-20%, and the proportion of the diammonium hydrogen phosphate in the phosphate mixture is 20-30%, a urea feeding pipeline is improved, so that the urea is heated more uniformly. The invention has high reaction speed and can meet the requirement of denitration on ammonia; reducing the operating temperature and the operating pressure; the defects that the urea is heated unevenly and the solution scours the wall of the container are reduced.

Description

Novel urea catalytic hydrolysis method and device
Technical Field
The invention belongs to the technical field of chemical material preparation, and particularly relates to a novel urea catalytic hydrolysis method and device.
Background
Currently, there are various commercially available processes for producing ammonia from urea: direct urea injection, urea pyrolysis, common urea hydrolysis and urea catalytic hydrolysis. At present, the urea catalytic hydrolysis has single catalyst, the urea solution enters a hydrolyzer to be heated unevenly, and certain response time is needed in a short time. Meanwhile, the problem of nonuniform heating during the use of the catalyst can affect the urea hydrolysis speed and increase the energy consumption.
The present invention has been made to solve the above problems.
Disclosure of Invention
The invention aims to provide a novel urea catalytic hydrolysis method.
In order to achieve the purpose, the invention adopts the following technical scheme:
a novel urea catalytic hydrolysis method comprises the steps of adding a phosphate mixture serving as a catalyst into a urea hydrolysis reactor, sending a urea solution with the mass concentration of 50% to the urea hydrolysis reactor, controlling the temperature of the urea hydrolysis reactor at 140 ℃ and the pressure of the urea hydrolysis reactor at 0.35-0.55MPa, and carrying out catalytic hydrolysis on urea, wherein the phosphate mixture is a mixture of potassium dihydrogen phosphate, ammonium dihydrogen phosphate and diammonium hydrogen phosphate with different proportions, the filling amount is 5-10% of the volume of a hydrolyzer, the loading amount of the urea solution is 50% of the volume of the hydrolyzer, the proportion of the ammonium dihydrogen phosphate in the phosphate mixture is 50-70%, the proportion of the potassium dihydrogen phosphate in the phosphate mixture is 10-20%, and the proportion of the diammonium hydrogen phosphate in the phosphate mixture is 20-30%. The purities of the potassium dihydrogen phosphate, the ammonium dihydrogen phosphate and the diammonium hydrogen phosphate are more than 99%.
The invention also aims to provide a novel urea catalytic hydrolysis device, which further accelerates the reaction speed, reduces the energy consumption, saves the energy and improves the utilization rate of equipment.
In order to achieve the purpose, the invention adopts the following technical scheme:
the utility model provides a novel urea catalytic hydrolysis device, includes hydrolysising ware, catch water, urea pipeline and heat exchanger, catch water is located the top of hydrolysising ware, is linked together with the hydrolysising ware, and the heat exchanger passes through bolt fastening and fixes inside the hydrolysising ware, and the urea pipeline sets up in the hydrolysising ware, is provided with the pipeline trompil on the urea pipeline, and the pipeline trompil is linked together with the hydrolysising ware, and the urea pipeline is connected with the solution entry, and catalyst solution and urea solution loop through the solution entry and enter into the hydrolysising ware in.
Preferably, the opening position of the opening of the pipeline forms an angle of 40-50 degrees with the vertical direction, the direction of the impact is the direction of the heat exchange pipe, the opening size is phi 10-15mm, and the number of the openings is 10-20.
Preferably, an angle steel bracket is arranged in the hydrolyzer to support a urea pipeline, and the urea pipeline and the heat exchanger are arranged below one-half liquid level of the hydrolyzer 1; the heat exchanger is fixed in the hydrolyzer through a bolt fastener.
Further, a steam inlet is arranged above the heat exchanger, a hydrophobic outlet is arranged below the heat exchanger, a gas-phase pressure relief outlet is arranged above the hydrolyzer, a safety valve is arranged on the gas-phase pressure relief outlet and used for performing gas-phase pressure relief on the hydrolyzer, and a waste liquid outlet is arranged below the hydrolyzer.
Further, a guided wave radar liquid level meter I, a guided wave radar liquid level meter II and a guided wave radar liquid level meter III are installed on the hydrolyzer and used for monitoring the liquid level; the hydrolyzer is provided with a thermal resistor I, a thermal resistor II and a thermal resistor III for monitoring temperature; the hydrolyzer is provided with a first pressure transmitter, a second pressure transmitter and a third pressure transmitter.
Furthermore, the urea pipeline on the hydrolyzer is in flange connection with the urea pipeline of an external system through a flange.
Further, the urea pipeline of the outer system is connected with a tee joint on the urea pipeline in the hydrolyzer sequentially through a flange, a reinforcing pipe, a connecting pipe, an elbow 23 and the connecting pipe.
Furthermore, the urea pipeline sequentially comprises a first connecting pipe, a second connecting pipe and a pipe cap.
Further, a catalyst solution and a urea solution sequentially enter the hydrolyzer through solution inlets respectively, then saturated steam at 165-180 ℃ enters the heat exchanger through a steam inlet, and the drained water after heat exchange is discharged through a drain outlet; the urea solution in the hydrolyzer is heated to 130-150 ℃ to decompose and generate product gas, and the components are as follows: ammonia, carbon dioxide and water vapor; and discharging the product gas through a product gas outlet, and entering a denitration system. When the pressure on the hydrolyzer is over 1.2MPa, a safety valve on the gas-phase pressure relief outlet is opened to perform gas-phase pressure relief on the hydrolyzer; and the hydrolyzer needs bottom pollution discharge when running for a period of time, and substances such as urea waste liquid and the like are discharged from a waste liquid outlet.
The invention has the beneficial technical effects that:
the method and the device disclosed by the invention have high reaction speed and can meet the requirement of denitration on ammonia; reducing the operating temperature and the operating pressure; the defects that urea is heated unevenly and the solution scours the wall of the container are overcome, and the urea catalytic hydrolysis method and the urea catalytic hydrolysis device provided by the invention have higher superiority.
Drawings
The invention will be further described with reference to the accompanying drawings.
FIG. 1 is a schematic diagram of the structure of the novel urea catalytic hydrolysis device of the invention.
FIG. 2 is a schematic sectional view of the arrangement of urea pipes in the hydrolyzer according to the present invention.
FIG. 3 is a schematic structural diagram of the arrangement of urea pipes in the hydrolyzer according to the present invention.
FIG. 4 is a schematic structural diagram of the design of the opening of the urea pipeline in the hydrolyzer according to the present invention.
The following is a reference number of the attached drawings of the novel urea catalytic hydrolysis device, and the product can be clearly understood through the description of the attached drawings and the corresponding reference number.
In the figure: 1-hydrolyzer; 2-a steam-water separator; 3-a heat exchanger; 32-opening the pipeline; 4-urea line; 5-bolt fasteners; 6-a steam inlet; 7-a hydrophobic outlet; 8-gas phase pressure relief outlet; 9-a waste liquid outlet; 10-guided wave radar level gauge one; 11-a second guided wave radar level gauge; 12-guided wave radar level gauge three; 13-thermal resistance one; 14-a second thermal resistor; 15-thermal resistance III; 16-a pressure transmitter I; 17-a second pressure transmitter; 18-pressure transmitter three; 19-a solution inlet; 20-a flange; 21-a reinforced pipe; 22-connection pipe; 23-bending the pipe; 24-take over; 25-a tee joint; 26-angle steel brackets; 27-take over one; 28-connecting pipe II; 29-a tube cap; a 30-U-shaped bolt; 31-nut.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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.
Example 1
A novel urea catalytic hydrolysis method comprises the steps of adding a phosphate mixture serving as a catalyst into a urea hydrolysis reactor, sending a urea solution with the mass concentration of 50% to the urea hydrolysis reactor, controlling the temperature of the urea hydrolysis reactor at 140 ℃ and the pressure of the urea hydrolysis reactor at 0.35-0.55MPa, and carrying out catalytic hydrolysis on urea, wherein the phosphate mixture is a mixture of potassium dihydrogen phosphate, ammonium dihydrogen phosphate and diammonium hydrogen phosphate with different proportions, the filling amount is 5-10% of the volume of a hydrolyzer, the loading amount of the urea solution is 50% of the volume of the hydrolyzer, the proportion of the ammonium dihydrogen phosphate in the phosphate mixture is 50-70%, the proportion of the potassium dihydrogen phosphate in the phosphate mixture is 10-20%, and the proportion of the diammonium hydrogen phosphate in the phosphate mixture is 20-30%.
Example 2
Referring to fig. 1, a novel urea catalytic hydrolysis device includes hydrolyzer 1, catch water 2, urea pipeline 4 and heat exchanger 3, catch water 2 is located the top of hydrolyzer 1, is linked together with hydrolyzer 1, heat exchanger 3 is fixed inside hydrolyzer 1 through bolt fastener 5, urea pipeline 4 sets up in hydrolyzer 1, be provided with pipeline trompil 32 on urea pipeline 4, pipeline trompil 32 is linked together with hydrolyzer 1, urea pipeline 4 is connected with solution entry 19, catalyst solution and urea solution loop through solution entry 19 and enter into hydrolyzer 1.
The opening position of the pipeline opening 32 forms an angle of 40-50 degrees with the vertical direction, the impact direction is the direction of the heat exchange pipe 3, the opening size is phi 10-15mm, and the number of the openings is 10-20.
The urea solution enters the hydrolyzer 1 through the pipeline openings 32, and because the urea solution is close to the heat exchanger and has a large number of openings, the urea solution is heated uniformly, and meanwhile, the solution is prevented from directly scouring the wall of the hydrolyzer 1.
The urea pipeline 4 and the heat exchanger 3 are arranged in parallel, the urea pipeline 4 and the heat exchanger 3 are located below the side of the heat exchanger 3, the length of the urea pipeline is basically equal to that of the heat exchanger, an angle steel bracket 26 is arranged in the hydrolyzer 1 to support the urea pipeline 4, and the urea pipeline 4 and the heat exchanger 3 are arranged below one-half liquid level of the hydrolyzer 1.
The heat exchanger 3 is fixed in the hydrolyzer 1 through a bolt fastener 5, so that the heat exchanger 3 is convenient to overhaul.
The bolt fastener 5 is a U-shaped bolt.
A steam inlet 6 is arranged above the heat exchanger 3, a hydrophobic outlet 7 is arranged below the heat exchanger 3, a gas-phase pressure relief outlet 8 is arranged above the hydrolyzer 1, and a safety valve is arranged on the gas-phase pressure relief outlet 8 and used for performing gas-phase pressure relief on the hydrolyzer 1. A waste liquid outlet 9 is arranged below the hydrolyzer 1 and used for discharging sewage at the bottom of the hydrolyzer 1.
The hydrolyzer 1 is provided with a guided wave radar liquid level meter I10, a guided wave radar liquid level meter II 11 and a guided wave radar liquid level meter III 12 for monitoring the liquid level; the hydrolyzer 1 is provided with a first thermal resistor 13, a second thermal resistor 14 and a third thermal resistor 15 for monitoring temperature; the hydrolyzer 1 is provided with a first pressure transmitter 16, a second pressure transmitter 17 and a third pressure transmitter 18 for monitoring pressure.
The urea pipeline 4 on the hydrolyzer 1 is connected with the urea pipeline of an external system through a flange 20. Specifically, the urea pipeline of the external system is connected with a tee 25 on the urea pipeline 4 in the hydrolyzer 1 through a flange 20, a reinforcing pipe 21, a connecting pipe 22, an elbow 23 and a connecting pipe 24 in sequence. The urea pipeline 4 is fixed with an angle iron support 26 welded on the hydrolyzer 1 through a U-shaped bolt 30 and a nut 31; the urea pipeline 4 comprises a first connecting pipe 27, a second connecting pipe 28 and a pipe cap 29 in sequence.
The catalyst solution and the urea solution enter the hydrolyzer 1 through a solution inlet 19, then saturated steam at 165-180 ℃ enters the heat exchanger 3 through a steam inlet 6, the hydrophobic water after heat exchange is discharged through a hydrophobic outlet 7, and the urea solution in the hydrolyzer 1 is heated to 130-140 ℃ to be decomposed to generate product gas, wherein the components are as follows: ammonia gas, carbon dioxide and water vapor, and simultaneously controlling the pressure to be 0.35-0.55 MPa. The product gas is discharged through the product gas outlet 32 and enters the denitrification system. When the pressure on the hydrolyzer 1 is more than 1.2MPa, the safety valve on the gas-phase pressure relief outlet 8 is opened to perform gas-phase pressure relief on the hydrolyzer 1. The hydrolyzer needs bottom pollution discharge when running for a period of time, and substances such as urea waste liquid and the like are discharged from a waste liquid outlet 9.
While there have been shown and described what are at present considered the fundamental principles and essential features of the invention and its advantages, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (10)

1. A novel urea catalytic hydrolysis method is characterized in that a phosphate mixture is added into a urea hydrolysis reactor as a catalyst, a urea solution with the mass concentration of 50% is sent to the urea hydrolysis reactor, the temperature of the urea hydrolysis reactor is controlled to be 130-140 ℃, the pressure is 0.35-0.55MPa, urea is subjected to catalytic hydrolysis, the phosphate mixture is a mixture of potassium dihydrogen phosphate, ammonium dihydrogen phosphate and diammonium hydrogen phosphate with different proportions, the filling amount is 5-10% of the volume of a hydrolyzer, the loading amount of the urea solution is 50% of the volume of the hydrolyzer, the proportion of the ammonium dihydrogen phosphate in the phosphate mixture is 50-70%, the proportion of the potassium dihydrogen phosphate in the phosphate mixture is 10-20%, and the proportion of the diammonium hydrogen phosphate in the phosphate mixture is 20-30%.
2. The utility model provides a novel urea catalytic hydrolysis device, a serial communication port, including hydrolysising ware (1), catch water (2), urea pipeline (4) and heat exchanger (3), catch water (2) are located the top of hydrolysising ware (1), be linked together with hydrolysising ware (1), heat exchanger (3) are fixed inside hydrolysising ware (1) through bolt fastener (5), urea pipeline (4) set up in hydrolysising ware (1), be provided with pipeline trompil (32) on urea pipeline (4), pipeline trompil (32) are linked together with hydrolysising ware (1), urea pipeline (4) are connected with solution entry (19), catalyst solution and urea solution loop through solution entry (19) and enter into hydrolysising ware (1).
3. The novel urea catalytic hydrolysis device as recited in claim 2, wherein the opening direction of the pipeline opening (32) is 40-50 ° from the vertical direction, the impact direction is the direction of the heat exchange pipe (3), the opening size is phi 10-15mm, and the number of the openings is 10-20.
4. A novel urea catalytic hydrolysis device as claimed in claim 2, wherein an angle iron bracket (26) is arranged in the hydrolyzer (1) to support the urea pipeline (4), and the urea pipeline (4) and the heat exchanger (3) are arranged below the half liquid level of the hydrolyzer (1); the heat exchanger (3) is fixed in the hydrolyzer (1) through a bolt fastener (5).
5. A novel urea catalytic hydrolysis device as claimed in claim 2, characterized in that a steam inlet (6) is arranged above the heat exchanger (3), a hydrophobic outlet (7) is arranged below the heat exchanger (3), a gas phase pressure relief outlet (8) is arranged above the hydrolyzer (1), a safety valve is arranged on the gas phase pressure relief outlet (8), and a waste liquid outlet (9) is arranged below the hydrolyzer (1).
6. The novel urea catalytic hydrolysis device as claimed in claim 2, wherein the hydrolyzer (1) is provided with a first guided wave radar level gauge (10), a second guided wave radar level gauge (11) and a third guided wave radar level gauge (12); the hydrolyzer (1) is provided with a first thermal resistor (13), a second thermal resistor (14 and a third thermal resistor (15), and the hydrolyzer (1) is provided with a first pressure transmitter (16), a second pressure transmitter (17) and a third pressure transmitter (18).
7. A novel urea catalytic hydrolysis device as claimed in claim 2, characterized in that the urea line (4) of the hydrolyzer (1) is flanged to the urea line of the external system via a flange (20).
8. A novel urea catalytic hydrolysis device as claimed in claim 2, characterized in that the urea line of the external system is connected with the tee (25) on the urea line (4) in the hydrolyzer (1) sequentially through the flange (20), the reinforced pipe (21), the connecting pipe (22), the elbow (23) and the connecting pipe (24).
9. A novel urea catalytic hydrolysis device as claimed in claim 2, characterized in that said urea line (4) comprises in sequence a first connection pipe (27), a second connection pipe (28) and a pipe cap (29).
10. The novel urea catalytic hydrolysis device as set forth in claim 2, characterized in that the using method is: the catalyst solution and the urea solution sequentially enter the hydrolyzer (1) through a solution inlet (19) respectively, then saturated steam with the temperature of 165-180 ℃ enters the heat exchanger (3) through a steam inlet (6), and the drained water after heat exchange is discharged through a drain outlet (7); the urea solution in the hydrolyzer (1) is heated to 130-140 ℃ to be decomposed to generate product gas, and the product gas is discharged through a product gas outlet (32); when the pressure on the hydrolyzer (1) is over 1.2MPa, a safety valve on a gas-phase pressure relief outlet (8) is opened to perform gas-phase pressure relief on the hydrolyzer (1); the hydrolyzer runs for a period of time, bottom pollution is discharged, and substances such as urea waste liquid and the like are discharged from a waste liquid outlet (9).
CN202210498858.XA 2022-05-09 2022-05-09 Novel urea catalytic hydrolysis method and device Pending CN114715915A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5543123A (en) * 1990-08-01 1996-08-06 Nalco Fuel Tech Low pressure formation of a urea hydrolysate for nitrogen oxides reduction
CN201978740U (en) * 2011-02-24 2011-09-21 成都锐思环保工程有限公司 Urea solution hydrolytic ammonia preparing kettle type reactor
US20120067094A1 (en) * 2010-03-25 2012-03-22 Taylor Pursell Urea fertilizer containing central volatilization inhibitor particles to reduce release of ammonia and processes for making same
CN103395801A (en) * 2013-08-08 2013-11-20 中国大唐集团环境技术有限公司 Method and device for catalytic hydrolysis of urea
CN103740764A (en) * 2013-12-27 2014-04-23 西安建筑科技大学 Functional biocatalyst for biogas fermentation and method for fermenting using catalyst
CN111921547A (en) * 2020-08-20 2020-11-13 浙江师范大学 Catalyst for preparing methyl glycolate by hydrogenating dimethyl oxalate and synthetic method and application thereof
CN212450660U (en) * 2020-09-14 2021-02-02 中国华电科工集团有限公司 Urea hydrolysis device

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5543123A (en) * 1990-08-01 1996-08-06 Nalco Fuel Tech Low pressure formation of a urea hydrolysate for nitrogen oxides reduction
US20120067094A1 (en) * 2010-03-25 2012-03-22 Taylor Pursell Urea fertilizer containing central volatilization inhibitor particles to reduce release of ammonia and processes for making same
CN201978740U (en) * 2011-02-24 2011-09-21 成都锐思环保工程有限公司 Urea solution hydrolytic ammonia preparing kettle type reactor
CN103395801A (en) * 2013-08-08 2013-11-20 中国大唐集团环境技术有限公司 Method and device for catalytic hydrolysis of urea
CN103740764A (en) * 2013-12-27 2014-04-23 西安建筑科技大学 Functional biocatalyst for biogas fermentation and method for fermenting using catalyst
CN111921547A (en) * 2020-08-20 2020-11-13 浙江师范大学 Catalyst for preparing methyl glycolate by hydrogenating dimethyl oxalate and synthetic method and application thereof
CN212450660U (en) * 2020-09-14 2021-02-02 中国华电科工集团有限公司 Urea hydrolysis device

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Title
王德汉等: "含氮木质素作为尿素控释材料提高水稻、玉米氮肥利用率研究" *

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