CN107098824B - A kind of device and production method using supergravity reactor production oxamides - Google Patents
A kind of device and production method using supergravity reactor production oxamides Download PDFInfo
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- CN107098824B CN107098824B CN201710407343.3A CN201710407343A CN107098824B CN 107098824 B CN107098824 B CN 107098824B CN 201710407343 A CN201710407343 A CN 201710407343A CN 107098824 B CN107098824 B CN 107098824B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/02—Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines
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- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/30—Loose or shaped packing elements, e.g. Raschig rings or Berl saddles, for pouring into the apparatus for mass or heat transfer
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- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00002—Chemical plants
- B01J2219/00027—Process aspects
- B01J2219/00033—Continuous processes
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Abstract
The invention belongs to a kind of devices and production method using supergravity reactor production oxamides；Including dimethyl oxalate storage tank, methanol tank, ammonia tank and sink, dimethyl oxalate storage tank is connected by solids delivery device with the solids inlet of batching kettle, the outlet of methanol tank is connected by the first pump with the liquid-inlet of batching kettle, batching kettle outlet is connected by the second pump with the liquid-inlet of hypergravity reaction kettle, ammonia tank is connected by pressure reducing valve with the gas feed of hypergravity reaction kettle, the outlet of hypergravity reaction kettle is connected with equipment for separating liquid from solid, equipment for separating liquid from solid solid outlet is connected with drying device, the solid outlet of drying device is connected with oxamides finished product storage tank, the gas vent of hypergravity reaction kettle and the gas vent of drying device are connected with sink respectively；Have the advantages that can continuous production, small in size, reaction temperature is low low with production cost.
Description
Technical field
The invention belongs to oxamides production technical fields, and in particular to a kind of to produce oxamides using supergravity reactor
Device and production method.
Background technique
Oxamides, molecular formula (CONH2)2, molecular weight 88.1, nitrogenous 31.8%, white powder, nonhygroscopic in air,
It is nontoxic, be easy to store, solubility in water is 0.016%, in hydrolysis or biological decomposition process, gradually releases ammoniacal nitrogen and two
Carbonoxide is a kind of good ureaformaldehyde class slow release fertilizer, compared with current quick-acting fertilizer such as ammonium bicarbonate, sulphur ammonium, urea, it just like
Lower advantage:
(1) solubility of particle oxamides in water is small, is not easy to be taken away by water flow after fertilising, is lost few, hydrolysis or biology
The nitrogen that plant is easy to absorb form is gradually released in decomposable process, is made to apply fertilizer and is expected to be fully absorbed by crop, can improve fertilizer efficiency,
Waste is reduced, pollution of waterhead is avoided.
(2) oxamides can make base manure and largely apply burn out crop or cause certain crops to absorb excessive nitrogen and lopsided
Growth, since fertilizer efficiency period is long, nitrogenous fertilizer needed for crop, which can make base manure, once have been applied, and can reduce fertilizer application frequency, saves labour, can avoid
Because applying fertilizer not in time, the crop fertilizer deficiency underproduction.
The synthetic method of oxamides has: using hydrogen cyanide as the preparation method of raw material, ammonium oxalate pyrolysismethod, carbon monoxide coupling method
(dimethyl oxalate ammonolysis process).Wherein hydrogen cyanide is severe poisonous chemicals, and its higher cost, this method produce the cost of oxamides compared with
It is high.Equally, with ammonium oxalate pyrolysismethod production oxamides there is also disadvantage at high cost, practical value is little.The synthesis of oxamides
There is prospect the most in method with dimethyl oxalate ammonolysis process, and with the development of synthesis gas preparing ethylene glycol technology, by carbon monoxide
The technology for being coupled synthesizing dimethyl oxalate is mature, solves the problems, such as the raw material of dimethyl oxalate ammonolysis production oxamides, cost
Also it declines to a great extent, is a kind of more promising synthetic method.
According to document " new type nitrogen fertilizer oxamides and its synthesis ", the technique of dimethyl oxalate ammonolysis synthesis oxamides can be borrowed
The technique for grease ammonolysis of reflecting, i.e., by after liquefied ammonia and grease pressurization, 100-120 DEG C reaction 5-6 hour, recycling ammonia and alcohol is washed
After fatty acid amide can be obtained.The disadvantages of the method are as follows require that reaction temperature is high, reaction time is long, can only interval into
Row.
Summary of the invention
The purpose of the present invention is to overcome the defects in the prior art, and inventing one kind can continuous production, small in size, production
A kind of device and production method using supergravity reactor production oxamides at low cost.
The object of the present invention is achieved like this: including dimethyl oxalate storage tank, methanol tank, ammonia tank and sink, grass
Dimethyl phthalate storage tank is connected by solids delivery device with the solids inlet of batching kettle, the outlet of methanol tank by the first pump and
The liquid-inlet of batching kettle is connected, and batching kettle outlet is connected by the second pump with the liquid-inlet of hypergravity reaction kettle, ammonia tank
It is connected by pressure reducing valve with the gas feed of hypergravity reaction kettle, the outlet of hypergravity reaction kettle is connected with equipment for separating liquid from solid,
Equipment for separating liquid from solid solid outlet is connected with drying device, and the solid outlet of drying device is connected with oxamides finished product storage tank, surpasses
The gas vent of gravity reaction kettle and the gas vent of drying device are connected with sink respectively；The liquid outlet of equipment for separating liquid from solid
It is connected respectively with the import of methanol tank with the liquid outlet of drying device, the overflow port of methanol tank passes through pipeline and methanol essence
Distillation unit is connected.
Preferably, the batching kettle is several, several ingredients are arranged in parallel.
Preferably, the hypergravity reaction kettle includes that liquid-inlet, gas feed, the outlet of hypergravity reaction kettle are gentle
Body outlet, being internally provided with for hypergravity reaction kettle is rotary packed bed, and the top of rotary packed bed centre passes through rotary shaft and sets
It is connected in the rotating electric machine of hypergravity reaction kettle hull outside, the end of the liquid-inlet and the end difference of gas feed
It is located at rotary packed bed inside.
Preferably, the equipment for separating liquid from solid is centrifugal filter.
Preferably, flowmeter is equipped between the pressure reducing valve and the gas feed of hypergravity reaction kettle.
A kind of production method of the device using supergravity reactor production oxamides, includes the following steps:
Step 1: the solid oxalic acid dimethyl ester in dimethyl oxalate storage tank is delivered to by solids delivery device after metering
In batching kettle, the methanol in methanol tank is delivered in batching kettle with the first pump after metering, and oxalic acid diformazan is obtained after agitated
Ester methanol solution；The mass ratio of the dimethyl oxalate and methanol is 1: 9~1: 3, and the mixing time in the batching kettle is 1
~30min；The batching kettle is several, several batching kettles are arranged in parallel, and can guarantee that process flow is carried out continuously；
Step 2: dimethyl oxalate methanol solution described in step 1 is delivered to the liquid of hypergravity reaction kettle through the second pump
Body import, ammonia tank enter hypergravity reaction kettle by the gas feed of hypergravity reaction kettle after ammonia by pressure reducing valve decompression
Interior, dimethyl oxalate, ammonia react in hypergravity reaction kettle generates oxamides, and reaction process is using methanol as solvent, reaction life
At solid oxamides and solvent methanol got rid of to the outlet of hypergravity reaction kettle by the packing layer of rotation, it is a small amount of unreacted
Ammonia is emitted into sink by the gas vent and exhaust pipe of hypergravity reaction kettle to be absorbed；It is described in hypergravity reaction kettle
Reaction pressure be 0.1MPa~3MPa, temperature is room temperature, and the mass ratio of dimethyl oxalate and ammonia is 2.37~3.47: 1.
Step 3: oxamides described in step 2 and methanol solid-liquid blend mixture and a small amount of unreacted ammonia pass through weight
Power effect enters equipment for separating liquid from solid, is separated by solid-liquid separation to obtain solid oxamides and liquid methanol, and wherein solid oxamides enters dry
Dry device is dried, and the oxamides finished product after drying enters in oxamides finished product storage tank；Liquid methanol and pass through drying
Liquid methanol after device, which enters in methanol tank, to be recycled；The a small amount of ammonia generated in drying device enters sink interior suction
It receives, is sold outside after ammonia concn reaches a certain concentration as ammonium hydroxide；
Step 4: the reaction process of dimethyl oxalate and ammonia generates methanol, methanol in reaction product using methanol as solvent
The liquid level of storage tank gradually rises, and when methanol capacity is more than the 2/3 of its volume in methanol tank, methanol passes through overflow port and pipeline
Into rectifying in methanol rectifying system, sold outside after rectifying as product.
Under identical conversion ratio, the residence time substantially shortens the present invention, the traditional batch fixed bed reactors residence time
It is 2-6 hours, and the use of reaction when hypergravity reaction kettle is to be carried out continuously；In the identical situation for the treatment of capacity, of the invention is set
Standby size can substantially reduce, while being greatly reduced and this is made, and hypergravity reactor volume is the 1/10- of fixed bed reaction kettle volume
1/5；Have the advantages that can continuous production, small in size, reaction temperature is low low with production cost.
Detailed description of the invention
Fig. 1 is the structural diagram of the present invention.
Fig. 2 is the structural schematic diagram of hypergravity reaction kettle in the present invention.
Specific embodiment
For a clearer understanding of the technical characteristics, objects and effects of the present invention, this hair of Detailed description of the invention is now compareed
Bright specific embodiment, identical label indicates identical component in the various figures.To make simplified form, in each figure only schematically
Ground indicates part relevant to invention, they do not represent its practical structures as product.
As shown in Figure 1, 2, the present invention is a kind of device and production method that oxamides is produced using supergravity reactor, packet
Include dimethyl oxalate storage tank 1, methanol tank 2, ammonia tank 3 and sink 4, dimethyl oxalate storage tank 1 by solids delivery device 5 with
The solids inlet of batching kettle 6 is connected, and the outlet of methanol tank 2 is connected by the first pump 7 with the liquid-inlet of batching kettle 6, ingredient
The outlet of kettle 6 is connected by the second pump 8 with the liquid-inlet 90 of hypergravity reaction kettle 9, and ammonia tank 3 passes through pressure reducing valve 10 and hypergravity
The gas feed 91 of reaction kettle 9 is connected, and the outlet 92 of hypergravity reaction kettle 9 is connected with equipment for separating liquid from solid 11, is separated by solid-liquid separation dress
It sets 11 solid outlets to be connected with drying device 12, the solid outlet of drying device 12 is connected with oxamides finished product storage tank 13, overweight
The gas vent 93 of power reaction kettle 9 and the gas vent of drying device 12 are connected with sink 4 respectively；The liquid of equipment for separating liquid from solid 11
The liquid outlet of body outlet and drying device 12 is connected with the import of methanol tank 2 respectively, and the overflow port of methanol tank 2 passes through pipe
Road is connected with methanol rectifying system 15.The batching kettle 6 is several, several batching kettles 6 are arranged in parallel.Described is overweight
Power reaction kettle 9 includes liquid-inlet 90, gas feed 91, the outlet of hypergravity reaction kettle 9 92 and gas vent 93, and hypergravity is anti-
That answers kettle 9 is internally provided with rotary packed bed 94, and the top among rotary packed bed 94 by rotary shaft 95 and is located at hypergravity
Rotating electric machine 97 outside reaction kettle shell 96 is connected, the end of the liquid-inlet 90 and the end difference of gas feed 91
It is located at rotary packed bed 94 inside.The equipment for separating liquid from solid 11 is centrifugal filter.The pressure reducing valve 10 and super
Flowmeter 14 is equipped between the gas feed 91 of gravity reaction kettle 9.
A kind of production method of the device using supergravity reactor production oxamides, includes the following steps:
Step 1: the solid oxalic acid dimethyl ester in dimethyl oxalate storage tank 1 passes through solids delivery device 5 after metering and conveys
To batching kettle 6, the methanol in methanol tank 2 uses the first pump 7 to be delivered in batching kettle 6 after metering, obtains grass after agitated
Dimethyl phthalate methanol solution；The mass ratio of the dimethyl oxalate and methanol is 1: 9~1: 3, the stirring in the batching kettle 6
Time is 1~30min；The batching kettle 6 is several, several batching kettles 6 are arranged in parallel, and can guarantee that process flow connects
It is continuous to carry out；
Step 2: dimethyl oxalate methanol solution described in step 1 is delivered to hypergravity reaction kettle 9 through the second pump 8
Liquid-inlet 90, ammonia tank 3 are entered super by the decompression of pressure reducing valve 10 by the gas feed 91 of hypergravity reaction kettle 9 after ammonia
In gravity reaction kettle 9, dimethyl oxalate, ammonia react in hypergravity reaction kettle 9 generates oxamides, and reaction process is with methanol
Solvent, the solid oxamides and solvent methanol for reacting generation are got rid of by the packing layer of rotation to the outlet of hypergravity reaction kettle 9
92, a small amount of unreacted ammonia is emitted into sink 4 by the gas vent 93 and exhaust pipe of hypergravity reaction kettle 9 to be absorbed；
The reaction pressure in hypergravity reaction kettle 9 is 0.1MPa~3MPa, and temperature is room temperature, the matter of dimethyl oxalate and ammonia
Amount is than being 2.37~3.47: 1.
Step 3: oxamides described in step 2 and methanol solid-liquid blend mixture and a small amount of unreacted ammonia pass through weight
Power effect enters equipment for separating liquid from solid 11, is separated by solid-liquid separation to obtain solid oxamides and liquid methanol, and wherein solid oxamides enters
Drying device 12 is dried, and the oxamides finished product after drying enters in oxamides finished product storage tank 13；Liquid methanol and logical
Liquid methanol after crossing drying device 12, which enters in methanol tank 2, to be recycled；The a small amount of ammonia generated in drying device 12 into
Enter in sink 4 and absorb, is sold outside after ammonia concn reaches a certain concentration as ammonium hydroxide；
Step 4: the reaction process of dimethyl oxalate and ammonia generates methanol, methanol in reaction product using methanol as solvent
The liquid level of storage tank 2 gradually rises, and when methanol capacity is more than the 2/3 of its volume in methanol tank 2, methanol passes through overflow port and pipe
Road enters rectifying in methanol rectifying system 15, sells outside after rectifying as product.
Applicant's discovery when use for laboratory batch reactor carries out pilot plant test, dimethyl oxalate, ammonia are in methanol
In solvent liquid phase reactor generate oxamides reaction be easy to carry out, but due to product oxamides be solid and cannot and time shift
It removes, is unfavorable for gas-liquid mass transfer, it is easy to occur reacting incomplete phenomenon.Stop can only be increased if it is the conversion ratio for pursuing high
Time.Therefore by hypergravity reaction kettle 9, the internal rotary packed bed hypergravity generated by rotation and shearing force make liquid
Body high degree of dispersion in porous aggregate substantially increases contact area, less turbulence and two alternate phases between gas-liquid two-phase
It to movement velocity, updates phase interface rapidly, to greatly enhance alternate mass transfer, is set reducing equipment energy consumption, reducing
Standby volume, raising yield etc. have the advantages that other mass transfer separation equipments are incomparable.
Below in conjunction with the embodiment of the present invention, the technical solution in the embodiment of the present invention is carried out clearly and completely
Description, it is clear that described embodiment is only a part of the embodiments of the present invention, instead of all the embodiments.Based on this
Embodiment in invention, one of ordinary skilled in the art are obtained all without making creative work
Other embodiments, shall fall within the protection scope of the present invention.
Embodiment 1
A kind of device using supergravity reactor production oxamides, including dimethyl oxalate storage tank 1, methanol tank 2, liquid
Ammonia tank 3 and sink 4, dimethyl oxalate storage tank 1 are connected by solids delivery device 5 with the solids inlet of batching kettle 6, methanol tank
2 outlet is connected by the first pump 7 with the liquid-inlet of batching kettle 6, and the outlet of batching kettle 6 is reacted by the second pump 8 with hypergravity
The liquid-inlet 90 of kettle 9 is connected, and ammonia tank 3 is connected by pressure reducing valve 10 with the gas feed 91 of hypergravity reaction kettle 9, hypergravity
The outlet 92 of reaction kettle 9 is connected with equipment for separating liquid from solid 11, and 11 solid outlet of equipment for separating liquid from solid is connected with drying device 12, does
The solid outlet of dry device 12 is connected with oxamides finished product storage tank 13, the gas vent 93 and drying device of hypergravity reaction kettle 9
12 gas vent is connected with sink 4 respectively；The liquid outlet of equipment for separating liquid from solid 11 and the liquid outlet point of drying device 12
It is not connected with the import of methanol tank 2, the overflow port of methanol tank 2 is connected by pipeline with methanol rectifying system 15.Described
Batching kettle 6 is several, several batching kettles 6 are arranged in parallel.The hypergravity reaction kettle 9 includes liquid-inlet 90, gas
Import 91, the outlet of hypergravity reaction kettle 9 92 and gas vent 93, being internally provided with for hypergravity reaction kettle 9 are rotary packed bed
Top among 94, rotary packed bed 94 passes through rotary shaft 95 and the rotating electric machine 97 being located at outside hypergravity reaction kettle shell 96
It is connected, the end of the liquid-inlet 90 and the end of gas feed 91 are respectively provided at rotary packed bed 94 inside.It is described
Equipment for separating liquid from solid 11 be centrifugal filter.Between the gas feed 91 of the pressure reducing valve 10 and hypergravity reaction kettle 9
Equipped with flowmeter 14.
A kind of production method of the device using supergravity reactor production oxamides, includes the following steps:
Step 1: the solid oxalic acid dimethyl ester in dimethyl oxalate storage tank 1 passes through solids delivery device 5 after metering and conveys
To batching kettle 6, the methanol in methanol tank 2 uses the first pump 7 to be delivered in batching kettle 6 after metering, obtains grass after agitated
Dimethyl phthalate methanol solution；The mass ratio of the dimethyl oxalate and methanol is 1: 9, the mixing time in the batching kettle 6
For 1min；The batching kettle 6 is several, several batching kettles 6 are arranged in parallel, and can guarantee that process flow is carried out continuously；
Step 2: dimethyl oxalate methanol solution described in step 1 is delivered to hypergravity reaction kettle 9 through the second pump 8
Liquid-inlet 90, ammonia tank 3 are entered super by the decompression of pressure reducing valve 10 by the gas feed 91 of hypergravity reaction kettle 9 after ammonia
In gravity reaction kettle 9, dimethyl oxalate, ammonia react in hypergravity reaction kettle 9 generates oxamides, and reaction process is with methanol
Solvent, the solid oxamides and solvent methanol for reacting generation are got rid of by the packing layer of rotation to the outlet of hypergravity reaction kettle 9
92, a small amount of unreacted ammonia is emitted into sink 4 by the gas vent 93 and exhaust pipe of hypergravity reaction kettle 9 to be absorbed；
The reaction pressure in hypergravity reaction kettle 9 is 0.1MPa, and temperature is room temperature, and the mass ratio of dimethyl oxalate and ammonia is
2.37∶1。
Step 3: oxamides described in step 2 and methanol solid-liquid blend mixture and a small amount of unreacted ammonia pass through weight
Power effect enters equipment for separating liquid from solid 11, is separated by solid-liquid separation to obtain solid oxamides and liquid methanol, and wherein solid oxamides enters
Drying device 12 is dried, and the oxamides finished product after drying enters in oxamides finished product storage tank 13；Liquid methanol and logical
Liquid methanol after crossing drying device 12, which enters in methanol tank 2, to be recycled；The a small amount of ammonia generated in drying device 12 into
Enter in sink 4 and absorb, is sold outside after ammonia concn reaches a certain concentration as ammonium hydroxide；
Step 4: the reaction process of dimethyl oxalate and ammonia generates methanol, methanol in reaction product using methanol as solvent
The liquid level of storage tank 2 gradually rises, and when methanol capacity is more than the 2/3 of its volume in methanol tank 2, methanol passes through overflow port and pipe
Road enters rectifying in methanol rectifying system 15, sells outside after rectifying as product.
Embodiment 2
A kind of device using supergravity reactor production oxamides, including dimethyl oxalate storage tank 1, methanol tank 2, liquid
Ammonia tank 3 and sink 4, dimethyl oxalate storage tank 1 are connected by solids delivery device 5 with the solids inlet of batching kettle 6, methanol tank
2 outlet is connected by the first pump 7 with the liquid-inlet of batching kettle 6, and the outlet of batching kettle 6 is reacted by the second pump 8 with hypergravity
The liquid-inlet 90 of kettle 9 is connected, and ammonia tank 3 is connected by pressure reducing valve 10 with the gas feed 91 of hypergravity reaction kettle 9, hypergravity
The outlet 92 of reaction kettle 9 is connected with equipment for separating liquid from solid 11, and 11 solid outlet of equipment for separating liquid from solid is connected with drying device 12, does
The solid outlet of dry device 12 is connected with oxamides finished product storage tank 13, the gas vent 93 and drying device of hypergravity reaction kettle 9
12 gas vent is connected with sink 4 respectively；The liquid outlet of equipment for separating liquid from solid 11 and the liquid outlet point of drying device 12
It is not connected with the import of methanol tank 2, the overflow port of methanol tank 2 is connected by pipeline with methanol rectifying system 15.Described
Batching kettle 6 is several, several batching kettles 6 are arranged in parallel.The hypergravity reaction kettle 9 includes liquid-inlet 90, gas
Import 91, the outlet of hypergravity reaction kettle 9 92 and gas vent 93, being internally provided with for hypergravity reaction kettle 9 are rotary packed bed
Top among 94, rotary packed bed 94 passes through rotary shaft 95 and the rotating electric machine 97 being located at outside hypergravity reaction kettle shell 96
It is connected, the end of the liquid-inlet 90 and the end of gas feed 91 are respectively provided at rotary packed bed 94 inside.It is described
Equipment for separating liquid from solid 11 be centrifugal filter.Between the gas feed 91 of the pressure reducing valve 10 and hypergravity reaction kettle 9
Equipped with flowmeter 14.
A kind of production method of the device using supergravity reactor production oxamides, includes the following steps:
Step 1: the solid oxalic acid dimethyl ester in dimethyl oxalate storage tank 1 passes through solids delivery device 5 after metering and conveys
To batching kettle 6, the methanol in methanol tank 2 uses the first pump 7 to be delivered in batching kettle 6 after metering, obtains grass after agitated
Dimethyl phthalate methanol solution；The mass ratio of the dimethyl oxalate and methanol is 1: 3, the mixing time in the batching kettle 6
For 30min；The batching kettle 6 is several, several batching kettles 6 are arranged in parallel, and can guarantee that process flow is carried out continuously；
Step 2: dimethyl oxalate methanol solution described in step 1 is delivered to hypergravity reaction kettle 9 through the second pump 8
Liquid-inlet 90, ammonia tank 3 are entered super by the decompression of pressure reducing valve 10 by the gas feed 91 of hypergravity reaction kettle 9 after ammonia
In gravity reaction kettle 9, dimethyl oxalate, ammonia react in hypergravity reaction kettle 9 generates oxamides, and reaction process is with methanol
Solvent, the solid oxamides and solvent methanol for reacting generation are got rid of by the packing layer of rotation to the outlet of hypergravity reaction kettle 9
92, a small amount of unreacted ammonia is emitted into sink 4 by the gas vent 93 and exhaust pipe of hypergravity reaction kettle 9 to be absorbed；
The reaction pressure in hypergravity reaction kettle 9 is 3MPa, and temperature is room temperature, and the mass ratio of dimethyl oxalate and ammonia is
3.47∶1。
Step 3: oxamides described in step 2 and methanol solid-liquid blend mixture and a small amount of unreacted ammonia pass through weight
Power effect enters equipment for separating liquid from solid 11, is separated by solid-liquid separation to obtain solid oxamides and liquid methanol, and wherein solid oxamides enters
Drying device 12 is dried, and the oxamides finished product after drying enters in oxamides finished product storage tank 13；Liquid methanol and logical
Liquid methanol after crossing drying device 12, which enters in methanol tank 2, to be recycled；The a small amount of ammonia generated in drying device 12 into
Enter in sink 4 and absorb, is sold outside after ammonia concn reaches a certain concentration as ammonium hydroxide；
Step 4: the reaction process of dimethyl oxalate and ammonia generates methanol, methanol in reaction product using methanol as solvent
The liquid level of storage tank 2 gradually rises, and when methanol capacity is more than the 2/3 of its volume in methanol tank 2, methanol passes through overflow port and pipe
Road enters rectifying in methanol rectifying system 15, sells outside after rectifying as product.
Embodiment 3
A kind of device using supergravity reactor production oxamides, including dimethyl oxalate storage tank 1, methanol tank 2, liquid
Ammonia tank 3 and sink 4, dimethyl oxalate storage tank 1 are connected by solids delivery device 5 with the solids inlet of batching kettle 6, methanol tank
2 outlet is connected by the first pump 7 with the liquid-inlet of batching kettle 6, and the outlet of batching kettle 6 is reacted by the second pump 8 with hypergravity
The liquid-inlet 90 of kettle 9 is connected, and ammonia tank 3 is connected by pressure reducing valve 10 with the gas feed 91 of hypergravity reaction kettle 9, hypergravity
The outlet 92 of reaction kettle 9 is connected with equipment for separating liquid from solid 11, and 11 solid outlet of equipment for separating liquid from solid is connected with drying device 12, does
The solid outlet of dry device 12 is connected with oxamides finished product storage tank 13, the gas vent 93 and drying device of hypergravity reaction kettle 9
12 gas vent is connected with sink 4 respectively；The liquid outlet of equipment for separating liquid from solid 11 and the liquid outlet point of drying device 12
It is not connected with the import of methanol tank 2, the overflow port of methanol tank 2 is connected by pipeline with methanol rectifying system 15.Described
Batching kettle 6 is several, several batching kettles 6 are arranged in parallel.The hypergravity reaction kettle 9 includes liquid-inlet 90, gas
Import 91, the outlet of hypergravity reaction kettle 9 92 and gas vent 93, being internally provided with for hypergravity reaction kettle 9 are rotary packed bed
Top among 94, rotary packed bed 94 passes through rotary shaft 95 and the rotating electric machine 97 being located at outside hypergravity reaction kettle shell 96
It is connected, the end of the liquid-inlet 90 and the end of gas feed 91 are respectively provided at rotary packed bed 94 inside.It is described
Equipment for separating liquid from solid 11 be centrifugal filter.Between the gas feed 91 of the pressure reducing valve 10 and hypergravity reaction kettle 9
Equipped with flowmeter 14.
A kind of production method of the device using supergravity reactor production oxamides, includes the following steps:
Step 1: the solid oxalic acid dimethyl ester in dimethyl oxalate storage tank 1 passes through solids delivery device 5 after metering and conveys
To batching kettle 6, the methanol in methanol tank 2 uses the first pump 7 to be delivered in batching kettle 6 after metering, obtains grass after agitated
Dimethyl phthalate methanol solution；The mass ratio of the dimethyl oxalate and methanol is 1: 6, the mixing time in the batching kettle 6
For 15.5min；The batching kettle 6 be several, several batching kettles 6 are arranged in parallel, can guarantee process flow continuously into
Row；
Step 2: dimethyl oxalate methanol solution described in step 1 is delivered to hypergravity reaction kettle 9 through the second pump 8
Liquid-inlet 90, ammonia tank 3 are entered super by the decompression of pressure reducing valve 10 by the gas feed 91 of hypergravity reaction kettle 9 after ammonia
In gravity reaction kettle 9, dimethyl oxalate, ammonia react in hypergravity reaction kettle 9 generates oxamides, and reaction process is with methanol
Solvent, the solid oxamides and solvent methanol for reacting generation are got rid of by the packing layer of rotation to the outlet of hypergravity reaction kettle 9
92, a small amount of unreacted ammonia is emitted into sink 4 by the gas vent 93 and exhaust pipe of hypergravity reaction kettle 9 to be absorbed；
The reaction pressure in hypergravity reaction kettle 9 is 1.55MPa, and temperature is room temperature, the mass ratio of dimethyl oxalate and ammonia
It is 2.92: 1.
Step 3: oxamides described in step 2 and methanol solid-liquid blend mixture and a small amount of unreacted ammonia pass through weight
Power effect enters equipment for separating liquid from solid 11, is separated by solid-liquid separation to obtain solid oxamides and liquid methanol, and wherein solid oxamides enters
Drying device 12 is dried, and the oxamides finished product after drying enters in oxamides finished product storage tank 13；Liquid methanol and logical
Liquid methanol after crossing drying device 12, which enters in methanol tank 2, to be recycled；The a small amount of ammonia generated in drying device 12 into
Enter in sink 4 and absorb, is sold outside after ammonia concn reaches a certain concentration as ammonium hydroxide；
Step 4: the reaction process of dimethyl oxalate and ammonia generates methanol, methanol in reaction product using methanol as solvent
The liquid level of storage tank 2 gradually rises, and when methanol capacity is more than the 2/3 of its volume in methanol tank 2, methanol passes through overflow port and pipe
Road enters rectifying in methanol rectifying system 15, sells outside after rectifying as product.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " connection ", " phase
Company " etc. shall be understood in a broad sense, for example, it may be being fixedly connected, is integrally connected, may be a detachable connection；It can also be with
It is the connection inside two elements；It can be directly connected, it can also indirectly connected through an intermediary, for the general of this field
For logical technical staff, the specific meanings of the above terms in the present invention can be understood according to specific conditions.It is above specifically
Bright illustrating only for feasible embodiment of the invention, the protection model that they are not intended to limit the invention
It encloses, it is all to should be included in protection of the invention without departing from equivalent implementations, change made by technical spirit of the present invention and transformation
Within the scope of.
Claims (5)
1. a kind of production method of the device using supergravity reactor production oxamides, characterized by the following steps:
Step 1: the solid oxalic acid dimethyl ester in dimethyl oxalate storage tank (1) passes through solids delivery device (5) conveying after metering
In to batching kettle (6), the methanol in methanol tank (2) is delivered in batching kettle (6) with the first pump (7) after metering, agitated
After obtain dimethyl oxalate methanol solution；The mass ratio of the dimethyl oxalate and methanol is 1: 9~1: 3, the batching kettle
(6) mixing time in is 1~30min；The batching kettle (6) is several, several batching kettles (6) are arranged in parallel, energy
Enough guarantee that process flow is carried out continuously；
Step 2: dimethyl oxalate methanol solution described in step 1 is delivered to hypergravity reaction kettle (9) through the second pump (8)
Liquid-inlet (90), ammonia tank (3) passes through hypergravity reaction kettle (9) by pressure reducing valve (10) decompression gas feed after ammonia
(91) enter in hypergravity reaction kettle (9), the reaction in hypergravity reaction kettle (9) of dimethyl oxalate, ammonia generates oxamides, instead
Answer process using methanol as solvent, the solid oxamides and solvent methanol for reacting generation are got rid of by the packing layer of rotation to hypergravity
The outlet (92) of reaction kettle (9), a small amount of unreacted ammonia pass through the gas vent (93) and offgas duct of hypergravity reaction kettle (9)
Line, which is emitted into sink (4), to be absorbed；The reaction pressure in hypergravity reaction kettle (9) is 0.1MPa~3MPa, and temperature is
The mass ratio of room temperature, dimethyl oxalate and ammonia is 2.37~3.47: 1.
Step 3: oxamides described in step 2 and methanol solid-liquid blend mixture and a small amount of unreacted ammonia are made by gravity
With equipment for separating liquid from solid (11) are entered, it is separated by solid-liquid separation to obtain solid oxamides and liquid methanol, wherein solid oxamides enters dry
Dry device (12) is dried, and the oxamides finished product after drying enters in oxamides finished product storage tank (13)；Liquid methanol and
Entered in methanol tank (2) by the liquid methanol after drying device (12) and is recycled；What is generated in drying device (12) lacks
Amount ammonia, which enters in sink (4), to be absorbed, and is sold outside after ammonia concn reaches a certain concentration as ammonium hydroxide；
Step 4: the reaction process of dimethyl oxalate and ammonia generates methanol, methanol tank in reaction product using methanol as solvent
(2) liquid level gradually rises, and when methanol capacity is more than the 2/3 of its volume in methanol tank (2), methanol passes through overflow port and pipe
Road enters rectifying in methanol rectifying system (15), sells outside after rectifying as product；
The described device using supergravity reactor production oxamides include dimethyl oxalate storage tank (1), methanol tank (2),
Ammonia tank (3) and sink (4), dimethyl oxalate storage tank (1) pass through the solids inlet of solids delivery device (5) and batching kettle (6)
It is connected, the outlet of methanol tank (2) is connected by the first pump (7) with the liquid-inlet of batching kettle (6), and batching kettle (6) outlet is logical
Cross second pump (8) be connected with the liquid-inlet (90) of hypergravity reaction kettle (9), ammonia tank (3) pass through pressure reducing valve (10) with it is overweight
The gas feed (91) of power reaction kettle (9) is connected, outlet (92) and equipment for separating liquid from solid (11) phase of hypergravity reaction kettle (9)
Even, equipment for separating liquid from solid (11) solid outlet is connected with drying device (12), the solid outlet and oxamides of drying device (12)
Finished product storage tank (13) is connected, the gas vent of the gas vent (93) of hypergravity reaction kettle (9) and drying device (12) respectively with
Sink (4) is connected；The liquid outlet of the liquid outlet of equipment for separating liquid from solid (11) and drying device (12) respectively with methanol tank
(2) import is connected, and the overflow port of methanol tank (2) is connected by pipeline with methanol rectifying system (15).
2. a kind of production method of device using supergravity reactor production oxamides according to claim 1, special
Sign is: the batching kettle (6) is several, several batching kettles (6) are arranged in parallel.
3. a kind of production method of device using supergravity reactor production oxamides according to claim 1, special
Sign is: the hypergravity reaction kettle (9) include liquid-inlet (90), gas feed (91), hypergravity reaction kettle (9) go out
Mouth (92) and gas vent (93), being internally provided with rotary packed bed (94) for hypergravity reaction kettle (9) are rotary packed bed (94)
Intermediate top is connected by rotary shaft (95) rotating electric machine (97) external with hypergravity reaction kettle shell (96) is located at, described
The end of liquid-inlet (90) and the end of gas feed (91) be respectively provided at the inside of rotary packed bed (94).
4. a kind of production method of device using supergravity reactor production oxamides according to claim 1, special
Sign is: the equipment for separating liquid from solid (11) is centrifugal filter.
5. a kind of production method of device using supergravity reactor production oxamides according to claim 1, special
Sign is: being equipped with flowmeter (14) between the gas feed (91) of the pressure reducing valve (10) and hypergravity reaction kettle (9).
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