CN113353886B - Method for preparing biological hydrogen and biological ammonia - Google Patents
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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
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- C01C1/04—Preparation of ammonia by synthesis in the gas phase
- C01C1/0405—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst
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Abstract
The invention discloses a method for preparing biological hydrogen and biological ammonia, which comprises the following steps: subjecting lignocellulose biomass raw material to gas explosion and crushingProducing methylated biomass slurry by a base boiling hydrolysis process; production of bio-H using methylated biomass slurry 2 Biological H 2 And N 2 Producing biological ammonia. The method takes the biomass raw material as the raw material for synthesizing ammonia, has the characteristics of cheap and easily obtained raw materials, simple process, environmental protection, energy conservation, high conversion rate, high product purity and the like, and is suitable for industrial production.
Description
Technical Field
The invention belongs to the field of synthetic ammonia, and particularly relates to a preparation method of biological hydrogen and biological ammonia.
Background
Ammonia is a compound of nitrogen and hydrogen, and its role is of considerable importance, being an important component of many foods and fertilizers, well known as a basic raw material for chemicals, textiles, explosives, refrigerants and fertilizers, and is one of the most productive inorganic compounds in the world. The synthetic ammonia industry was developed in the early 20 th century, ammonia was used as a raw material in the explosive industry for war service, and after world war for the first time, ammonia was turned to agricultural and industrial service. With the development of scientific technology, the demand of ammonia is increasing; the ammonia can also be used as a general carbon-free fuel to replace fossil fuels such as diesel oil, aviation kerosene, natural gas and the like.
The raw materials for synthesizing ammonia are hydrogen and nitrogen, and the key point is hydrogen. Hydrogen is widely distributed in nature, and petroleum, natural gas, coal, biomass, water and the like all contain hydrogen. The main industrial starting materials for hydrogen gas are stone-based materials such as natural gas, petroleum and coal, which are also the main starting materials for ammonia synthesis. The Chinese energy structure has the characteristics of more coal, oil shortage and less gas, and the coal is the main starting material of synthetic ammonia at present. Although the industrial history of ammonia synthesis is long, the synthesis technology is mature, and the application is wide, the research on the types of the starting materials is rarely reported, and the research is limited to stone-based raw materials such as natural gas, petroleum and coal, and the research on biomass as the starting material is not reported.
In recent years, as research and application of new energy automobiles using hydrogen fuel cells as power are developed greatly, hydrogen is taken as fuel, and new technologies such as hydrogen production by large-scale electrolysis of water and hydrogen production by plasma bombardment of biomass begin to appear, but non-fossil-based hydrogen is not produced in large scale for various reasons, and the new technologies cannot be popularized and popularized due to high cost, low cost performance and other factors, and are not used in the field of ammonia synthesis.
The ammonia can be combusted in an internal combustion engine, a gas turbine, a turbine engine and the like to replace fossil fuels such as diesel oil, aviation kerosene, natural gas and the like, is a carbon-free fuel commonly used in land, sea and air, and is an expression form of hydrogen energy.
The hydrogen production by biomass and the further synthesis of ammonia are the future development of the field of ammonia synthesis. The biomass mainly refers to lignocellulose such as urban landscaping residues, agricultural and forestry wastes, resource crops and the like, is the most extensive resource in the nature and the strongest renewable capability, has the global yield of over 1000 hundred million tons/year and over the current oil storage capacity, and can be lost as wastes by people when the yield in China reaches 100 million tons/year. The biological hydrogen is hydrogen produced by using lignocellulose biomass as a raw material, adopting the processes of revolutionary gas explosion crushing, gasification and the like to produce biological synthesis gas, and then carrying out the processes of transformation, separation and the like on the biological synthesis gas. The biological ammonia is ammonia synthesized by taking biological hydrogen as a raw material. The development of the method for synthesizing ammonia by using lignocellulose biomass as a starting material is based on coal reduction strategy, carbon neutralization strategy and the like, and the method is very in line with the national situation of China.
Disclosure of Invention
The invention aims to provide a preparation method of biological hydrogen and biological ammonia, which takes a biomass raw material as a raw material for synthesizing ammonia, has the characteristics of cheap and easily obtained raw materials, simple process, environmental protection, energy conservation, high conversion rate, high product purity and the like, and is suitable for industrial production.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for producing biological hydrogen and biological ammonia, comprising:
performing gas explosion crushing and methylation boiling hydrolysis on a lignocellulose biomass raw material to produce methylated biomass slurry;
production of bio-H using methylated biomass slurry 2 Biological H 2 And N 2 Producing biological ammonia.
Further, the gas explosion crushing comprises: placing the lignocellulose biomass raw material after mechanical crushing into a tubular gas explosion reactor, introducing superheated steam, wherein the temperature of the superheated steam is 240-280 ℃, the pressure is 2.4-3.1 MPa, and the time is 0.5-5 minutes, opening a valve of the tubular gas explosion reactor, and exploding the material into a methylation boiling hydrolysis reactor; methylation boiling hydrolysis comprises: the temperature is 160-220 ℃, the pressure is 1.4-1.6 MPa, the time is 5-30 minutes, the methylation boiling hydrolysis reaction converts hemicellulose in the biomass raw material into methylated xylo-oligosaccharide, the cellulose into methylated fiber oligosaccharide, and the lignin is converted into methylated oligo-lignin, so as to prepare methylated biomass slurry.
Further, the water content of the methylated biomass slurry is more than 30%.
Further, the methylated biomass slurry comprises: 5 to 36 weight percent of methylated xylo-oligosaccharide, 15 to 65 weight percent of methylated cello-oligosaccharide, 10 to 55 weight percent of methylated oligo lignin and 15 to 60 weight percent of water, and the compaction density range of the methylated biomass slurry is controlled to be 1.2 to 1.6g/cm 3 The heat value range is 20.50-33.10 MJ/kg.
Further, a pressurized entrained-flow bed gasification furnace device is adopted, the methylated biomass slurry is pumped into a gasification furnace, and the solid content of the methylated biomass slurry is 60-65 wt%; then gasifying agent O 2 The mixture is sent into a gasification furnace device through a nozzle to start gasification, the gasification temperature is 1200-1350 ℃, the pressure is 1.2-2.5 MPa, and the product mainly containing H is prepared 2 CO and CO 2 The ratio of the biological synthesis gas is 32-36 percent of H 2 38 to 41 weight percent of CO and 10 to 12 weight percent of CO 2 (ii) a Adjusting H by adopting steam conversion process for biological synthesis gas 2 And CO in a ratio of 7-10, and preparing biological H from the transformed biological synthesis gas by a pressure swing adsorption separation device 2 And by-product biological CO.
Further, an organism H 2 And purified air separation N 2 The biological ammonia is synthesized by the ammonia synthesis process through a medium pressure method, the pressure is controlled to be 25-35 MPa, the reaction temperature is 450-550 ℃, and the catalyst is an iron catalyst.
Further, a living organism H 2 And N 2 The molar ratio of (a) to (b) is 3 to 4.
The invention has the technical effects that:
the method utilizes lignocellulose biomass such as agricultural and forestry waste and the like as raw materials to serve as the starting raw material for synthesizing ammonia, belongs to biomass raw materials, has the characteristics of cheap and easily-obtained raw materials, simple process, environmental protection, high conversion rate, high product purity, low cost and the like, and is suitable for industrial production. The biological ammonia can directly replace fossil-based ammonia, is used in the fields of chemicals, textiles, explosives, refrigerants, chemical fertilizers and the like, and can also be used as a general carbon-free fuel to replace fossil fuels such as diesel oil, aviation kerosene, natural gas and the like.
(1) The raw material is lignocellulose biomass (urban landscaping residues, agricultural and forestry wastes, resource crops and the like), is cheap, easy to obtain and renewable, is mostly a waste resource, and belongs to waste utilization.
(2) And converting hemicellulose, cellulose and lignin into methylated xylo-oligosaccharide, methylated cello-oligosaccharide and methyl oligomeric lignin respectively by adopting a gas explosion crushing-methylation boiling hydrolysis process to prepare methylated biomass, so that the full component utilization of lignocellulose biomass resources is realized.
(3) The pressurized entrained flow bed gasification process is used for producing the biological hydrogen from the methylated biomass slurry, the investment is low, the efficiency is high, the process has the characteristics of pure gas, no sulfur, simple and stable gasification process and the like, and the comprehensive cost-efficiency ratio is superior to that of non-biological hydrogen such as fossil-based hydrogen, hydrogen production by water electrolysis and the like.
(4) The biological hydrogen is used as the raw material of the biological ammonia, has the characteristics of cheap and easily obtained and reproducible raw materials, simple and quick process, reliable product performance and the like, and is suitable for rapid arrangement industrial production.
Detailed Description
The following description sufficiently illustrates specific embodiments of the invention to enable those skilled in the art to practice and reproduce it.
The invention takes lignocellulose biomass as raw materials (urban landscaping residues, agricultural and forestry wastes, resource crops and the like), methylated biomass slurry is obtained after gas explosion crushing and methylation boiling hydrolysis, the slurry is gasified to produce bio-based synthesis gas, the bio-based synthesis gas is separated and purified to produce bio-hydrogen, and then the bio-hydrogen and air separation nitrogen are used for synthesizing bio-ammonia.
The preparation method of the biological hydrogen and the biological ammonia comprises the following specific steps:
step 1: producing methylated biomass slurry by performing gas explosion crushing and methylation boiling hydrolysis on a lignocellulose biomass raw material;
gas explosion and crushing: the lignocellulose biomass raw material after mechanical crushing is placed into a tubular gas explosion reactor, superheated steam is introduced into the tubular gas explosion reactor at the temperature of 240-280 ℃, the pressure of 2.4-3.1 MPa and the time of 0.5-5 minutes, a valve is opened, and the material is exploded into a methylation boiling hydrolysis reactor.
Methylation boiling hydrolysis: the reaction is carried out at the temperature of 160-220 ℃ and the pressure of 1.4-1.6 MPa for 5-30 minutes to convert hemicellulose in the wood fiber biomass raw material into methylated xylo-oligosaccharide, convert cellulose into methylated cello-oligosaccharide and convert lignin into methylated oligo-lignin, thus preparing the methylated biomass. Methylated biomass comprises: 5 to 36 weight percent of methylated xylo-oligosaccharide, 15 to 65 weight percent of methylated cello-oligosaccharide, 10 to 55 weight percent of methylated oligomeric lignin and 15 to 60 weight percent of water, and the compaction density range of the methylated biomass is controlled to be 1.2 to 1.6g/cm 3 The heat value range is 20.50-33.10 MJ/kg. Methylated biomass having a water content of greater than 30% is referred to as methylated biomass slurry.
Step 2: production of bio-H using methylated biomass slurry 2 ；
A pressurized entrained-flow bed gasification furnace device is adopted, methylated biomass slurry (solid content is 60-65 wt%) is pumped into a gasification furnace, and then a gasification agent O is added 2 The mixture is sent into a gasification furnace device through a nozzle to start gasification, the gasification temperature is 1200-1350 ℃, the pressure is 1.2-2.5 MPa, and the product mainly containing H is prepared 2 CO and CO 2 The proportion of the biological synthesis gas is H of 32-36 percent 2 38 to 41 weight percent of CO and 10 to 12 weight percent of CO 2 。
Adjusting H by adopting steam conversion process for biological synthesis gas 2 And CO in the ratio of 7-10, and preparing biological H from the transformed biological synthesis gas by a Pressure Swing Adsorption (PSA) separation device 2 And by-product biological CO.
And 3, step 3: biological H 2 And N 2 (molar ratio 3-4).
Biological H 2 And purified air separation N 2 (separation from air)Of free N 2 ) The biological ammonia is synthesized by the ammonia synthesis process by the medium pressure method, the pressure is controlled to be 25-35 MPa, the reaction temperature is 450-550 ℃, and the catalyst is an iron catalyst.
Example 1
(1) 200kg of corn straws (with the water content of 25 wt%) are crushed to be less than 1cm, the crushed materials are sent into a gas explosion crushing-methylation boiling hydrolysis reactor, superheated steam is introduced for gas explosion crushing, the temperature is 245-250 ℃, the pressure is 2.4-2.5 MPa, and the time is 0.5 minute, the materials are blasted and crushed into nano-micron particles, the nano-micron particles are sent into a methylation boiling hydrolysis device, the temperature is 180-190 ℃, the pressure is 1.4-1.5 MPa, and the time is 10-15 minutes, the reaction converts hemicellulose in the straws into methylated xylo-oligosaccharides, the cellulose into methylated fibers, and the lignin is converted into methylated lignin oligosaccharides, so that methylated biomass slurry containing 35-40% of water is generated.
(2) 130.2kg of methylated biomass slurry is fed by adopting a pressurized entrained-flow bed gasification furnace device, the content of lignin semicoke in the slurry is 61-63 wt%, and the gasification agent is O 2 The pressurized slurry and high-pressure oxygen are fed into gasification furnace device by means of nozzle, and the gasification temperature is 1250-1280 deg.C, and pressure is 1.2-1.3 MPa so as to obtain the invented product mainly containing H 2 CO and CO 2 The ratio of (2) is 32 to 36wt% 2 38 to 41 weight percent of CO and 10 to 12 weight percent of CO 2 . Adjusting H of the biological synthesis gas by a steam shift reaction device 2 And CO in a ratio of 7 2 And by-product biological CO.
(3) H, organism 2 And space division N 2 The biological ammonia is synthesized by the ammonia synthesis process through a medium pressure method, the pressure is 25-27 MPa, the reaction temperature is 450-470 ℃, and the catalyst is an iron catalyst.
Example 2
(1) 200kg of tree prunes (with the water content of 20 wt%) are crushed to be less than 1cm, the crushed tree prunes are sent into a gas explosion crushing-methylation boiling hydrolysis reactor, superheated steam is introduced for gas explosion crushing, the temperature is 240-245 ℃, the pressure is 2.5-2.6 MPa, the time is 1 minute, the materials are exploded and crushed into nano-micron particles, the nano-micron particles are sent into a methylation boiling hydrolysis device, the temperature is 190-200 ℃, the pressure is 1.5-1.6 MPa, the time is 20-25 minutes, the reaction converts hemicellulose in the tree prunes into methylated xylo-oligosaccharides, cellulose into methylated cello-oligosaccharides, and lignin is converted into methylated lignin to generate methylated biomass slurry containing 37-40 wt% of water.
(2) 132.1kg of methylated biomass slurry is fed by adopting a pressurized entrained flow gasifier device, the content of lignin and semicoke in the slurry is 60-62 wt%, and the gasifying agent is O 2 The pressurized slurry and high-pressure oxygen are fed into a gasification furnace device through a nozzle, the gasification temperature is 1270-1290 ℃, the pressure is 1.5-1.6 MPa, and the slurry mainly containing H is prepared 2 CO and CO 2 The ratio of the biological synthesis gas is 32-36 wt% of H 2 38 to 41 weight percent of CO and 10 to 12 weight percent of CO 2 . Adjusting H of the biological synthesis gas by a steam shift reaction device 2 And CO in a ratio of 8 2 And by-product biological CO.
(3) H, organism 2 And space division N 2 The biological ammonia is synthesized by the ammonia synthesis process by a medium pressure method, the pressure is 26-28 MPa, the reaction temperature is 480-500 ℃, and the catalyst is an iron catalyst.
Example 3
(1) 200kg of landscaping waste branches (with the water content of 25 wt%) are crushed to be less than 1cm, the crushed branches are sent to a gas explosion crushing-methylation boiling hydrolysis reactor, superheated steam is introduced for gas explosion crushing at the temperature of 260-270 ℃ and the pressure of 2.7-2.8 MPa for 2 minutes, the materials are blasted and crushed into nano-micron particles and then sent to a methylation boiling hydrolysis device at the temperature of 160-170 ℃ and the pressure of 1.4-1.5 MPa for 15-20 minutes, the reaction converts hemicellulose in the landscaping waste branches into methylated xylo-oligosaccharides, converts cellulose into methylated cello-oligosaccharides, and converts lignin into methylated lignin to generate methylated biomass slurry containing 35-37 wt% of water.
(2) 132.1kg of methylated biomass slurry is fed by a pressurized entrained flow gasifier device, and lignin in the slurry is a halfThe coke content is 62-64 wt%, and the gasifying agent is O 2 The pressurized slurry and high-pressure oxygen are fed into a gasification furnace device through a nozzle, the gasification temperature is 1280-1300 ℃, the pressure is 1.7-1.8 MPa, and the slurry mainly containing H is prepared 2 CO and CO 2 The ratio of (3) is 32 to 36wt%, the content of H2, 38 to 41wt% of CO, 10 to 12wt% of CO 2 . Adjusting H of the biological synthesis gas by a steam shift reaction device 2 And CO in a ratio of 9 2 And by-product biological CO.
(3) H, organism 2 And space division N 2 The biological ammonia is synthesized by the ammonia synthesis process through a medium pressure method, the pressure is 30-32 MPa, the reaction temperature is 470-490 ℃, and the catalyst is an iron catalyst.
Example 4
(1) 200kg of moso bamboo (with the water content of 23 wt%) is crushed to be less than 1cm, the moso bamboo is sent into a gas explosion crushing-methylation boiling hydrolysis reactor, superheated steam is introduced for gas explosion crushing, the temperature is 260-270 ℃, the pressure is 3.0-3.1 MPa, the time is 2.5 minutes, the materials are blasted and crushed into nano-micron particles, the nano-micron particles are sent into a methylation boiling hydrolysis device, the temperature is 200-210 ℃, the pressure is 1.5-1.6 MPa, and the time is 20-25 minutes, the reaction is carried out to convert hemicellulose in the moso bamboo into methylated xylo-oligosaccharide, cellulose into methylated cello-oligosaccharide, and lignin is converted into methylated lignin, so that methylated biomass slurry containing 35-37% of water is generated.
(2) 130.8kg of methylated biomass slurry is fed by adopting a pressurized entrained-flow bed gasification furnace device, the content of lignin semicoke in the slurry is 62-64 wt%, and the gasification agent is O 2 The pressurized slurry and high-pressure oxygen are fed into gasification furnace device by means of nozzle, and the gasification temperature is 1300-1320 deg.C, pressure is 1.2-1.3 MPa, so that the invented product mainly contains H 2 CO and CO 2 The proportion of the biological synthesis gas is 32-36 wt% of H 2 38-41 wt% of CO, 10-12 wt% of CO 2 . Adjusting H of the biological synthesis gas by a steam shift reaction device 2 And CO in a ratio of 10 2 And by-product biological CO.
(3) H, organism 2 And space division N 2 The biological ammonia is synthesized by the ammonia synthesis process through a medium pressure method, the pressure is 32-34 MPa, the reaction temperature is 460-480 ℃, and the catalyst is an iron catalyst.
The terminology used herein is for the purpose of description and illustration, and is not intended to be limiting. As the present invention may be embodied in several forms without departing from the spirit or essential characteristics thereof, it should also be understood that the above-described embodiments are not limited by any of the details of the foregoing description, but rather should be construed broadly within its spirit and scope as defined in the appended claims, and therefore all changes and modifications that fall within the meets and bounds of the claims, or equivalences of such meets and bounds are therefore intended to be embraced by the appended claims.
Claims (5)
1. A method for producing biohydrogen and bioammonia, comprising:
producing methylated biomass slurry by performing gas explosion crushing and methylation boiling hydrolysis on a lignocellulose biomass raw material; placing the lignocellulose biomass raw material after mechanical crushing into a tubular gas explosion reactor, introducing superheated steam, wherein the temperature of the superheated steam is 240-280 ℃, the pressure is 2.4-3.1 MPa, and the time is 0.5-5 minutes, opening a valve of the tubular gas explosion reactor, and exploding the material into a methylation boiling hydrolysis reactor; methylation boiling hydrolysis comprises: the temperature is 160-220 ℃, the pressure is 1.4-1.6 MPa, the time is 5-30 minutes, the methylation boiling hydrolysis reaction converts hemicellulose in the biomass raw material into methylated xylo-oligosaccharide, the cellulose into methylated fiber oligosaccharide, and the lignin is converted into methylated oligomeric lignin to prepare methylated biomass slurry;
production of bio-H using methylated biomass slurry 2 : firstly, pumping the methylated biomass slurry into a gasification furnace by adopting a pressurized entrained flow gasification furnace device, wherein the solid content of the methylated biomass slurry is 60-65 wt%; then gasifying agent O 2 The mixture is sent into a gasification furnace device through a nozzle to start gasification, the gasification temperature is 1200-1350 ℃, the pressure is 1.2-2.5 MPa, and the product mainly containing H is prepared 2 CO and CO 2 The ratio of the biological synthesis gas is 32-36 percent of H 2 38 to 41 weight percent of CO and 10 to 12 weight percent of CO 2 (ii) a Adjusting H by adopting steam conversion process for biological synthesis gas 2 And CO in a ratio of 7-10, and preparing biological H from the transformed biological synthesis gas by a pressure swing adsorption separation device 2 By-production of biological CO and biological H 2 And N 2 Producing biological ammonia.
2. The method of claim 1, wherein the methylated biomass slurry has a water content of greater than 30%.
3. The method of claim 1, wherein methylating a biomass slurry comprises: 5 to 36 weight percent of methylated xylo-oligosaccharide, 15 to 65 weight percent of methylated cello-oligosaccharide, 10 to 55 weight percent of methylated oligo lignin and 15 to 60 weight percent of water, and the compaction density range of the methylated biomass slurry is controlled to be 1.2 to 1.6g/cm 3 The heat value range is 20.50-33.10 MJ/kg.
4. The method of claim 1, wherein the biological H is selected from the group consisting of 2 And purified air separation N 2 The biological ammonia is synthesized by the ammonia synthesis process through a medium pressure method, the pressure is controlled to be 25-35 MPa, the reaction temperature is 450-550 ℃, and the catalyst is an iron catalyst.
5. The method for producing biohydrogen and bioammonia according to claim 4, wherein the bioH is 2 And N 2 3 to 4.
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