CN112358408A - Production process and device of glycine - Google Patents
Production process and device of glycine Download PDFInfo
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- CN112358408A CN112358408A CN202011381322.7A CN202011381322A CN112358408A CN 112358408 A CN112358408 A CN 112358408A CN 202011381322 A CN202011381322 A CN 202011381322A CN 112358408 A CN112358408 A CN 112358408A
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- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 239000004471 Glycine Substances 0.000 title claims abstract description 41
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 75
- 238000007670 refining Methods 0.000 claims abstract description 62
- JVTAAEKCZFNVCJ-UHFFFAOYSA-M Lactate Chemical compound CC(O)C([O-])=O JVTAAEKCZFNVCJ-UHFFFAOYSA-M 0.000 claims abstract description 43
- 239000002994 raw material Substances 0.000 claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- 239000007788 liquid Substances 0.000 claims abstract description 34
- 239000003054 catalyst Substances 0.000 claims abstract description 33
- 238000003860 storage Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims description 21
- 239000002184 metal Substances 0.000 claims description 13
- 229910052751 metal Inorganic materials 0.000 claims description 13
- 229910021529 ammonia Inorganic materials 0.000 claims description 12
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims description 4
- 238000001179 sorption measurement Methods 0.000 claims description 4
- 239000005909 Kieselgur Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 239000002041 carbon nanotube Substances 0.000 claims description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- 239000002808 molecular sieve Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052763 palladium Inorganic materials 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 229910052707 ruthenium Inorganic materials 0.000 claims description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 2
- 150000001721 carbon Chemical class 0.000 claims 1
- 238000005915 ammonolysis reaction Methods 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 208000012839 conversion disease Diseases 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 46
- 239000000463 material Substances 0.000 description 8
- 238000011084 recovery Methods 0.000 description 6
- 239000007795 chemical reaction product Substances 0.000 description 5
- 238000000975 co-precipitation Methods 0.000 description 5
- 239000012043 crude product Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 description 4
- 229910017121 AlSiO Inorganic materials 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 150000001413 amino acids Chemical class 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 229940106681 chloroacetic acid Drugs 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000005576 amination reaction Methods 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- GSJFXBNYJCXDGI-UHFFFAOYSA-N methyl 2-hydroxyacetate Chemical compound COC(=O)CO GSJFXBNYJCXDGI-UHFFFAOYSA-N 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000003408 phase transfer catalysis Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/04—Formation of amino groups in compounds containing carboxyl groups
- C07C227/06—Formation of amino groups in compounds containing carboxyl groups by addition or substitution reactions, without increasing the number of carbon atoms in the carbon skeleton of the acid
- C07C227/08—Formation of amino groups in compounds containing carboxyl groups by addition or substitution reactions, without increasing the number of carbon atoms in the carbon skeleton of the acid by reaction of ammonia or amines with acids containing functional groups
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a glycine production device, which comprises a methyl glycolate raw material tank, a preheater, a reactor, a gas-liquid separator, a first temporary storage tank, a product refining tower, a product tank, a pump set and an accessory group, wherein an outlet of the methyl glycolate raw material tank is communicated with an inlet of the preheater through the pump set, an outlet of the preheater is communicated with an inlet of the reactor, and an outlet of the reactor is communicated with an inlet of the gas-liquid separator through the accessory group. Preparing a catalyst; putting methyl glycolate and ammonia gas; the glycine can be prepared by reaction according to preset conditions, a new synthesis route is provided on the basis of the existing glycine synthesis route, glycine is synthesized by catalyzing and ammonolysis by taking easily available methyl glycolate as a raw material, and compared with other routes, the route has the advantages of mild reaction conditions, high reaction conversion rate, no participation of other solvents and less emission.
Description
Technical Field
The invention relates to the technical field of chemical processes, in particular to a process and a device for producing glycine.
Background
Glycine, also known as glycine, is the simplest of amino acids in the amino acid series. The glycine has acidic and basic functional groups in the molecule, can be made to present different molecular forms by adjusting the acidity and the basicity of an aqueous solution, is an important chemical intermediate, and is widely applied to the fields of food, medicine, agriculture, industry, reagents and the like. There are ten or more synthetic routes reported in the literature, and they can be classified into two types, i.e., a chemical synthetic route represented by the Schwerk method (Strecker), the Bucherer method, the monochloroacetic acid amination method, and the phase transfer catalysis method, and a biological method using catalysis of a specific genus. At present, most of domestic industrial production still adopts a chloroacetic acid ammonolysis method for obtaining glycine by catalytic ammonolysis by taking ammonia water and monochloroacetic acid as raw materials, the method can only obtain crude products, further refining is needed, the consumption of a catalyst is high, and a large amount of waste liquid is generated, so researchers provide a plurality of synthetic routes and methods, and most of the synthetic routes and methods are modified around the chloroacetic acid ammonolysis method.
Disclosure of Invention
The invention provides a production process and a device for glycine, aiming at solving the problems that only crude glycine can be obtained in a synthetic route of glycine in the prior art, a large amount of catalyst is consumed during purification, and a large amount of waste liquid is generated.
The utility model provides a apparatus for producing of glycine, includes methyl glycolate head tank, pre-heater, reactor, vapour and liquid separator, first jar, product refining tower, product jar, pump package and accessory group of keeping in, the export of methyl glycolate head tank pass through the pump package with the entry intercommunication of pre-heater, the export of pre-heater then with the entry intercommunication of reactor, the export of reactor pass through the accessory group with the entry intercommunication of vapour and liquid separator, the liquid export of vapour and liquid separator with the entry intercommunication of first jar of keeping in, the export of first jar of keeping in pass through the pump package with the entry intercommunication of product refining tower, the bottom export of product refining tower pass through the accessory group with the product jar intercommunication.
The glycine production device further comprises a liquid ammonia tank, a buffer tank and an ammonia refining tower, wherein a gas outlet of the gas-liquid separator is communicated with an inlet of the ammonia refining tower, an outlet of the ammonia refining tower is communicated with an inlet of the liquid ammonia tank through the pump set, an outlet of the liquid ammonia tank is communicated with an inlet of the buffer tank, and an outlet of the buffer tank is communicated with the reactor through the pump set.
Wherein, the pump package includes feedstock pump, booster pump, compressor and delivery pump, feedstock pump's input with the exit linkage of methyl glycolate head tank, feedstock pump's output with the entry intercommunication of pre-heater, the input of booster pump with the export intercommunication of buffer tank, the output of booster pump with the reactor intercommunication, the input of compressor with the export intercommunication of ammonia refining tower, the output of compressor with the entry intercommunication of liquid ammonia jar, the input of delivery pump with the export intercommunication of first jar of keeping in, the output of delivery pump with the entry intercommunication of product refining tower.
The auxiliary assembly comprises a first heat exchanger, a second temporary storage tank, a condenser and a reboiler, wherein an inlet of the first heat exchanger is communicated with the reactor, an outlet of the first heat exchanger is communicated with an inlet of the gas-liquid separator, the second heat exchanger is communicated with the product tank and a bottom outlet of the product refining tower respectively, the condenser is arranged at a joint of an upper outlet of the product refining tower and the second temporary storage tank, an inlet of the second temporary storage tank is communicated with an upper outlet of the product refining tower, and the reboiler is arranged at a joint of the second heat exchanger and the bottom outlet of the product refining tower.
The reactor is a fixed bed reactor and comprises a reactor shell, a tube plate and a reaction tube, wherein the reaction tube is fixed in the reactor shell through the tube plate, a plurality of grooves are formed in the peripheral side of the reaction tube, the grooves are formed in the length extending direction of the reaction tube, and the tube plate is fixedly connected with the reactor shell and arranged at two ends of the reactor shell.
The invention also provides a glycine production process adopting the glycine production device, which comprises the following steps:
preparing a catalyst by adopting physical precipitation adsorption or sintering, wherein the catalyst comprises a carrier and a metal active component, and the metal active component accounts for 0.1-40% of the catalyst in percentage by weight;
filling the catalyst into the fixed bed reactor, and reducing by using hydrogen;
feeding the methyl glycolate in the methyl glycolate raw material tank into a fixed bed reactor by using the raw material pump;
feeding the ammonia gas in the buffer tank into a fixed bed reactor by using the booster pump;
after the ammonia gas and the methyl glycolate are added, the glycine can be prepared by reacting according to preset conditions.
Wherein the metal active component is selected from at least one metal simple substance in the group consisting of Ru, Pd, Pt, Co, Ni, Cu, Al and La, an oxide thereof or a combination thereof.
Wherein the carrier is selected from the group consisting of SiO2、Al2O3Activated carbon, ZrO2、TiO2At least one of the group consisting of diatomaceous earth, molecular sieves, and carbon nanotubes.
Wherein the carrier is selected from the group consisting of SiO2、Al2O3Activated carbon, ZrO2And TiO2At least one of the group consisting of.
The preset conditions are that the reaction temperature is 100-250 ℃, the reaction pressure is 1-3 MPa, and the mass ratio of methyl glycolate to ammonia gas is 1: 5-10.
The invention has the beneficial effects that: on the basis of the existing glycine synthesis route, a new synthesis route is provided, glycine is synthesized by taking easily available methyl glycolate as a raw material and performing catalytic ammonolysis, and compared with other routes, the route has the advantages of mild reaction conditions, high reaction conversion rate, no participation of other solvents and less emission.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic view of a glycine production apparatus according to the present invention.
FIG. 2 is a schematic view showing the structure of a reactor of a glycine production apparatus of the present invention.
FIG. 3 is a flow chart of the process steps of a method for producing glycine according to the present invention.
1-methyl glycolate raw material tank, 2-preheater, 3-reactor, 4-gas-liquid separator, 5-first temporary storage tank, 6-product refining tower, 7-product tank, 8-pump set, 9-accessory group, 10-liquid ammonia tank, 11-buffer tank, 12-ammonia refining tower, 31-reactor shell, 32-tube plate, 33-reaction tube, 81-raw material pump, 82-booster pump, 83-compressor, 84-transfer pump, 91-first heat exchanger, 92-second heat exchanger, 93-second temporary storage tank, 94-condenser and 95-reboiler.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In the description of the present invention, it is to be understood that the terms "length", "width", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships illustrated in the drawings, and are used merely for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed as limiting the present invention. Further, in the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
Referring to fig. 1 to 3, the present invention provides a technical solution:
a glycine production device comprises a methyl glycolate raw material tank 1, a preheater 2, a reactor 3, a gas-liquid separator 4, a first temporary storage tank 5, a product refining tower 6, a product tank 7, a pump set 8 and an accessory set 9, wherein an outlet of the methyl glycolate raw material tank 1 is communicated with an inlet of the preheater 2 through the pump set 8, an outlet of the preheater 2 is communicated with an inlet of the reactor 3, an outlet of the reactor 3 is communicated with an inlet of the gas-liquid separator 4 through the accessory set 9, a liquid outlet of the gas-liquid separator 4 is communicated with an inlet of the first temporary storage tank 5, an outlet of the first temporary storage tank 5 is communicated with an inlet of the product refining tower 6 through the temporary storage pump set 8, and a bottom outlet of the product refining tower 6 is communicated with the product tank 7 through the accessory set 9.
In this embodiment, the methyl glycolate raw material tank 1 is used to store a methyl glycolate raw material, the preheater 2 is used to heat the methyl glycolate, the reactor 3 is used to fully react the methyl glycolate with ammonia gas, the gas-liquid separator 4 is used to separate ammonia gas and liquid crude products, the first temporary storage tank 5 is used to temporarily store the liquid crude products, the product refining tower 6 is used to refine the crude products, the product tank 7 is used to store the products processed by the product refining tower 6, and the pump unit 8 and the kit unit 9 are used to cooperate with each component.
Further, the glycine production device further comprises a liquid ammonia tank 10, a buffer tank 11 and an ammonia refining tower 12, wherein a gaseous outlet of the gas-liquid separator 4 is communicated with an inlet of the ammonia refining tower 12, an outlet of the ammonia refining tower 12 is communicated with an inlet of the liquid ammonia tank 10 through the pump unit 8, an outlet of the liquid ammonia tank 10 is communicated with an inlet of the buffer tank 11, and an outlet of the buffer tank 11 is communicated with the reactor 3 through the pump unit 8.
In the present embodiment, the liquid ammonia tank 10 is used for storing liquid ammonia gas, the ammonia gas refining tower 12 is used for purifying ammonia gas and sending ammonia gas into the liquid ammonia tank 10, and the buffer tank 11 is used for helping the ammonia gas in the liquid ammonia tank 10 to be slowly released.
Further, pump package 8 includes raw material pump 81, booster pump 82, compressor 83 and delivery pump 84, raw material pump 81 the input with methyl glycolate raw material tank 1's exit linkage, raw material pump 81 the output with pre-heater 2's entry intercommunication, booster pump 82's input with buffer tank 11's export intercommunication, booster pump 82's output with reactor 3 intercommunication, compressor 83's input with the export intercommunication of ammonia refining tower 12, compressor 83's output with the entry intercommunication of liquid ammonia jar 10, delivery pump 84's input with the export intercommunication of first jar 5, delivery pump 84's output with the entry intercommunication of product refining tower 6.
In this embodiment, the raw material pump 81 is used for pumping out the raw material in the methyl glycolate raw material tank 1, the booster pump 82 is used for boosting the pressure of ammonia gas, the compressor 83 is used for liquefying the ammonia gas from the ammonia gas refining tower 12 so as to be transported to the liquid ammonia tank 10 for storage, and the transport pump 84 is used for transporting the crude product in the first temporary storage tank 5.
Further, the kit 9 includes a first heat exchanger 91, a second heat exchanger 92, a second temporary storage tank 93, a condenser 94 and a reboiler 95, an inlet of the first heat exchanger 91 is communicated with the reactor 3, an outlet of the first heat exchanger 91 is communicated with an inlet of the gas-liquid separator 4, the second heat exchanger 92 is respectively communicated with the product tank 7 and a bottom outlet of the product refining tower 6, the condenser 94 is disposed at a junction of an upper outlet of the product refining tower 6 and the second temporary storage tank 93, an inlet of the second temporary storage tank 93 is communicated with an upper outlet of the product refining tower 6, and the reboiler 95 is disposed at a junction of the second heat exchanger 92 and the bottom outlet of the product refining tower 6.
In this embodiment, the first heat exchanger 91 is used to lower the temperature of the material discharged from the reactor 3, the second heat exchanger 92 is used to lower the temperature of the material discharged from the lower outlet of the product refining column 6, the second temporary storage tank 93 is used to store a small amount of unreacted material and byproducts discharged from the upper outlet of the product refining column 6, the condenser 94 is used to lower the temperature of a small amount of unreacted material and byproducts, and the reboiler 95 is used to partially vaporize the material in the bottom of the product refining column 6 to maintain the rectification operation.
Further, the reactor 3 is a fixed bed reactor 3, and includes a reactor shell 31, a tube plate 32 and a reaction tube 33, the reaction tube 33 is fixed in the reactor shell 31 by the tube plate 32, a plurality of grooves are provided on the outer peripheral side of the reaction tube 33, the grooves are arranged along the length extending direction of the reaction tube 33, and the tube plate 32 is fixedly connected with the reactor shell 31 and is arranged at two ends of the reactor shell 31.
In this embodiment, the reactor shell 31 is used to support the components, the tube plate 32 is used to fix the reaction tube 33 in the reactor shell 31, and the reaction tube 33 is used to fix the catalyst.
The invention also provides a glycine production process adopting the glycine production device, which comprises the following steps:
s101: preparing a catalyst by adopting physical precipitation adsorption or sintering, wherein the catalyst comprises a carrier and a metal active component, and the metal active component accounts for 0.1-40% of the catalyst in percentage by weight;
s102: the catalyst is filled into the fixed bed reactor 3 and is reduced by hydrogen;
s103: feeding the methyl glycolate in the methyl glycolate raw material tank 1 to the fixed bed reactor 3 by the raw material pump 81;
s104: feeding the ammonia gas in the buffer tank 11 into the fixed bed reactor 3 by using the booster pump 82;
s105: after the ammonia gas and the methyl glycolate are added, the glycine can be prepared by reacting according to preset conditions.
In this embodiment, the weight percentage of the metal active component is preferably 5 to 20% of the catalyst, a supported catalyst is prepared by physical precipitation adsorption or sintering, the catalyst is filled in the reactor 3, methyl glycolate in the methyl glycolate raw material tank 1 is heated to a specified value by the raw material pump 81 through the preheater 2 and then is fed into the reactor 3, the liquid ammonia tank 10 is connected with the buffer tank 11, ammonia gas is fed into the reactor 3 by the booster pump 82, after the reaction is finished, the material in the reactor 3 is depressurized and then is cooled by the first heat exchanger 91 and enters the gas-liquid separator 4, the gas phase of the gas-liquid separator 4 is discharged and enters the ammonia refining tower 12, and the ammonia gas discharged from the ammonia refining tower 12 is liquefied by the compressor 83 and then enters the liquid ammonia tank 10. 4 liquid phase ejection of compact of vapour and liquid separator gets into first jar 5 of keeping in, the crude in the first jar 5 of keeping in by the delivery pump 84 pump feed in product refining tower 6, the ejection of compact warp at the bottom of the product refining tower 6 second heat exchanger 92 cools off the back and sends into product jar 7, the ejection of compact of 6 tops of product refining tower is a small amount of unreacted material and accessory substance, gets into the second jar 93 of keeping in.
Further, the metal active component is selected from at least one simple metal substance in the group consisting of Ru, Pd, Pt, Co, Ni, Cu, Al, La, an oxide thereof, or a combination thereof.
Further, the carrier is selected from the group consisting of SiO2、Al2O3Activated carbon, ZrO2、TiO2At least one of the group consisting of diatomaceous earth, molecular sieves, and carbon nanotubes.
Further, the carrier is selected from the group consisting of SiO2、Al2O3Activated carbon, ZrO2And TiO2Group ofAt least one of (1).
Further, the preset conditions are that the reaction temperature is 100-250 ℃, the reaction pressure is 1-3 MPa, and the mass ratio of methyl glycolate to ammonia gas is 1: 5-10.
Specific example 1:
a coprecipitation method is adopted to prepare a Ni/AlSiO catalyst, 50g of the catalyst (Ni content is 10 wt%) is filled into a fixed bed reactor 3, and the catalyst is reduced by hydrogen (450 ℃) before use. Methyl glycolate was fed into the fixed bed reactor 3 by a raw material pump 81, ammonia gas was fed into the fixed bed reactor 3 by a booster pump 82, and the ratio of methyl glycolate: ammonia gas 1: 6, the weight space-time speed is 1h, the reaction temperature is 140 ℃, the conversion rate is 62 percent, the selectivity is 92 percent, the reaction product is separated by a gas-liquid separator 4 and refined by a product refining tower 6, and the product refining recovery rate is 98 percent.
Specific example 2:
a coprecipitation method is adopted to prepare a Ni/AlSiO catalyst, 50g of the catalyst (Ni content is 10 wt%) is filled into a fixed bed reactor 3, and the catalyst is reduced by hydrogen (450 ℃) before use. Methyl glycolate was fed into the fixed bed reactor 3 by a raw material pump 81, ammonia gas was fed into the fixed bed reactor 3 by a booster pump 82, and the ratio of methyl glycolate: ammonia gas 1: 6, the weight space-time speed is 1h, the conversion rate is 98 percent and the selectivity is 92 percent when the reaction temperature is 180 ℃, the reaction product is separated by a gas-liquid separator 4 and refined by a product refining tower 6, and the product refining recovery rate is 98 percent.
Specific example 3:
a coprecipitation method is adopted to prepare a Ni/AlSiO catalyst, 50g of the catalyst (Ni content is 10 wt%) is filled into a fixed bed reactor 3, and the catalyst is reduced by hydrogen (450 ℃) before use. Methyl glycolate was fed into the fixed bed reactor 3 by a raw material pump 81, ammonia gas was fed into the fixed bed reactor 3 by a booster pump 82, and the ratio of methyl glycolate: ammonia gas 1: 6, the weight space-time speed is 4 hours, the reaction temperature is 180 ℃, the conversion rate is 90 percent, the selectivity is 98 percent, the reaction product is separated by a gas-liquid separator 4 and refined by a product refining tower 6, and the product refining recovery rate is 98 percent.
Specific example 4:
the Ni/LaAlSiO catalyst was prepared by coprecipitation method, 50g of catalyst (Ni content 10 wt%) was packed in fixed bed reactor 3, and the catalyst was reduced with hydrogen (450 ℃ C.) before use. Methyl glycolate was fed into the fixed bed reactor 3 by a raw material pump 81, ammonia gas was fed into the fixed bed reactor 3 by a booster pump 82, and the ratio of methyl glycolate: ammonia gas 1: 6, the weight space-time speed is 1h, the reaction temperature is 180 ℃, the conversion rate is 65 percent, the selectivity is 96 percent, the reaction product is separated by a gas-liquid separator 4 and refined by a product refining tower 6, and the product refining recovery rate is 98 percent.
Specific example 5:
preparation of Ni/SiO by coprecipitation method2The catalyst, 50g of catalyst (Ni content 10 wt%), was charged into the fixed bed reactor 3 and reduced with hydrogen (450 ℃ C.) before use. Methyl glycolate was fed into the fixed bed reactor 3 by a raw material pump 81, ammonia gas was fed into the fixed bed reactor 3 by a booster pump 82, and the ratio of methyl glycolate: ammonia gas 1: 6, the weight space-time speed is 1h, the reaction temperature is 140 ℃, the conversion rate is 60 percent, the selectivity is 90 percent, the reaction product is separated by a gas-liquid separator 4 and refined by a product refining tower 6, and the product refining recovery rate is 98 percent.
In each embodiment, the product purification recovery rate is the same, but the conversion rate and the selectivity of embodiment 2 are the highest, and the material ratio of embodiment 2 can be selected as the preferable ratio.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The glycine production device is characterized by comprising a methyl glycolate raw material tank, a preheater, a reactor, a gas-liquid separator, a first temporary storage tank, a product refining tower, a product tank, a pump set and an accessory set, wherein an outlet of the methyl glycolate raw material tank is communicated with an inlet of the preheater through the pump set, an outlet of the preheater is communicated with an inlet of the reactor, an outlet of the reactor is communicated with an inlet of the gas-liquid separator through the accessory set, a liquid outlet of the gas-liquid separator is communicated with an inlet of the first temporary storage tank, an outlet of the first temporary storage tank is communicated with an inlet of the product refining tower through the pump set, and a bottom outlet of the product refining tower is communicated with the product tank through the accessory set.
2. The glycine production device as claimed in claim 1, further comprising a liquid ammonia tank, a buffer tank and an ammonia gas refining tower, wherein the gaseous outlet of the gas-liquid separator is communicated with the inlet of the ammonia gas refining tower, the outlet of the ammonia gas refining tower is communicated with the inlet of the liquid ammonia tank through the pump set, the outlet of the liquid ammonia tank is communicated with the inlet of the buffer tank, and the outlet of the buffer tank is communicated with the reactor through the pump set.
3. The apparatus for producing glycine as claimed in claim 2, wherein the pump set comprises a raw material pump, a booster pump, a compressor and a delivery pump, the input end of the raw material pump is connected with the outlet of the methyl glycolate raw material tank, the output end of the raw material pump is communicated with the inlet of the preheater, the input end of the booster pump is communicated with the outlet of the buffer tank, the output end of the booster pump is communicated with the reactor, the input end of the compressor is communicated with the outlet of the ammonia refining tower, the output end of the compressor is communicated with the inlet of the liquid ammonia tank, the input end of the delivery pump is communicated with the outlet of the first temporary storage tank, and the output end of the delivery pump is communicated with the inlet of the product refining tower.
4. The apparatus for producing glycine as claimed in claim 3, wherein the set of components includes a first heat exchanger, a second temporary storage tank, a condenser and a reboiler, the inlet of the first heat exchanger is connected to the reactor, the outlet of the first heat exchanger is connected to the inlet of the gas-liquid separator, the second heat exchanger is connected to the product tank and the bottom outlet of the product refining tower, the condenser is disposed at the junction of the upper outlet of the product refining tower and the second temporary storage tank, the inlet of the second temporary storage tank is connected to the upper outlet of the product refining tower, and the reboiler is disposed at the junction of the second heat exchanger and the bottom outlet of the product refining tower.
5. The apparatus for producing glycine as claimed in claim 4 wherein the reactor is a fixed bed reactor comprising a reactor shell, a tube plate and a reaction tube, the reaction tube is fixed in the reactor shell by the tube plate, the outer periphery of the reaction tube has a plurality of grooves, the grooves are arranged along the length extension direction of the reaction tube, the tube plate is fixedly connected with the reactor shell and is arranged at two ends of the reactor shell.
6. A process for producing glycine using the apparatus for producing glycine as claimed in claim 5, comprising the steps of:
preparing a catalyst by adopting physical precipitation adsorption or sintering, wherein the catalyst comprises a carrier and a metal active component, and the metal active component accounts for 0.1-40% of the catalyst in percentage by weight;
filling the catalyst into the fixed bed reactor, and reducing by using hydrogen;
feeding the methyl glycolate in the methyl glycolate raw material tank into a fixed bed reactor by using the raw material pump;
feeding the ammonia gas in the buffer tank into a fixed bed reactor by using the booster pump;
after the ammonia gas and the methyl glycolate are added, the glycine can be prepared by reacting according to preset conditions.
7. The process for producing glycine as claimed in claim 6, wherein the metal active component is at least one metal selected from the group consisting of Ru, Pd, Pt, Co, Ni, Cu, Al, La, an oxide thereof or a combination thereof.
8. Process for the production of glycine as claimed in claim 7 wherein the support is selected from the group consisting of SiO2、Al2O3Activated carbon, ZrO2、TiO2At least one of the group consisting of diatomaceous earth, molecular sieves, and carbon nanotubes.
9. The process for producing glycine as claimed in claim 8, wherein the carrier is selected from the group consisting of SiO2、Al2O3Activated carbon, ZrO2And TiO2At least one of the group consisting of.
10. The process for producing glycine as claimed in claim 9, wherein the predetermined conditions are a reaction temperature of 100 to 250 ℃, a reaction pressure of 1 to 3MPa, and a mass ratio of methyl glycolate to ammonia gas of 1:5 to 10.
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Cited By (1)
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