CN110003072A - A kind of preparation method of 2- methylaziridine - Google Patents
A kind of preparation method of 2- methylaziridine Download PDFInfo
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- CN110003072A CN110003072A CN201910196848.9A CN201910196848A CN110003072A CN 110003072 A CN110003072 A CN 110003072A CN 201910196848 A CN201910196848 A CN 201910196848A CN 110003072 A CN110003072 A CN 110003072A
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- methylaziridine
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- esterification
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- OZDGMOYKSFPLSE-UHFFFAOYSA-N 2-Methylaziridine Chemical compound CC1CN1 OZDGMOYKSFPLSE-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000004821 distillation Methods 0.000 claims abstract description 60
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 42
- HXKKHQJGJAFBHI-UHFFFAOYSA-N 1-aminopropan-2-ol Chemical compound CC(O)CN HXKKHQJGJAFBHI-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229940102253 isopropanolamine Drugs 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 239000003513 alkali Substances 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 13
- 230000032050 esterification Effects 0.000 claims description 55
- 238000005886 esterification reaction Methods 0.000 claims description 55
- 238000006243 chemical reaction Methods 0.000 claims description 52
- 238000006555 catalytic reaction Methods 0.000 claims description 50
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 12
- 239000012267 brine Substances 0.000 claims description 10
- 238000010992 reflux Methods 0.000 claims description 10
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 229910052763 palladium Inorganic materials 0.000 claims description 9
- 230000018044 dehydration Effects 0.000 claims description 8
- 238000006297 dehydration reaction Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- 239000000470 constituent Substances 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims 2
- 150000001412 amines Chemical class 0.000 claims 1
- 238000010025 steaming Methods 0.000 claims 1
- 238000003786 synthesis reaction Methods 0.000 abstract description 16
- 230000015572 biosynthetic process Effects 0.000 abstract description 14
- 238000000034 method Methods 0.000 abstract description 9
- 239000006227 byproduct Substances 0.000 abstract description 5
- 230000001681 protective effect Effects 0.000 abstract description 5
- 150000002148 esters Chemical class 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 9
- 239000002994 raw material Substances 0.000 description 5
- 238000007599 discharging Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- NOWKCMXCCJGMRR-UHFFFAOYSA-N Aziridine Chemical compound C1CN1 NOWKCMXCCJGMRR-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 239000003183 carcinogenic agent Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- JTJMJGYZQZDUJJ-UHFFFAOYSA-N phencyclidine Chemical compound C1CCCCN1C1(C=2C=CC=CC=2)CCCCC1 JTJMJGYZQZDUJJ-UHFFFAOYSA-N 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000002760 rocket fuel Substances 0.000 description 1
- 235000012773 waffles Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D203/00—Heterocyclic compounds containing three-membered rings with one nitrogen atom as the only ring hetero atom
- C07D203/04—Heterocyclic compounds containing three-membered rings with one nitrogen atom as the only ring hetero atom not condensed with other rings
- C07D203/06—Heterocyclic compounds containing three-membered rings with one nitrogen atom as the only ring hetero atom not condensed with other rings having no double bonds between ring members or between ring members and non-ring members
- C07D203/08—Heterocyclic compounds containing three-membered rings with one nitrogen atom as the only ring hetero atom not condensed with other rings having no double bonds between ring members or between ring members and non-ring members with only hydrogen atoms, hydrocarbon or substituted hydrocarbon radicals, directly attached to the ring nitrogen atom
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the field of chemical synthesis, and in particular to a kind of preparation method of 2- methylaziridine uses isopropanolamine, sulfuric acid and liquid alkaline for Material synthesis 2- methylaziridine, and synthesis condition is mild, is conducive to large-scale industrial production；Furthermore synthesis material is simple, is esterified using sulfuric ester, then is hydrolyzed with liquid alkaline, and distillation purifying process is purified with piece alkali again, and by-product is few, environmentally protective；Just distillation is carried out using normal pressure, then carries out smart distillation with low pressure, obtained 2- methylaziridine purity reaches 99% or more.
Description
Technical field
The invention belongs to the field of chemical synthesis, and in particular to a kind of preparation method of 2- methylaziridine.
Background technique
2- methylaziridine also known as propyleneimine are commonly used for adhesive, curing agent also serves as solid rocket fuel.It defends in the world
The carcinogenic substance inventory edit reference that raw tissue international cancer research institution announces, 2- methylaziridine are clear in 2B class carcinogenic substance
Dan Zhong.
2- methylaziridine is a kind of important medicine intermediate, has a wide range of applications in many fields, has at present
The synthesis technology of many kinds of 2- methylaziridines, but combined coefficient is low, and the by-product of synthesis process is more, to environmental hazard
Greatly.
Summary of the invention
In view of the deficiency of the prior art, the present invention provides combined coefficient height, environmentally protective 2- methyl nitrogen third
The preparation method of pyridine.
To achieve the goals above, present invention employs following technical solutions: a kind of preparation method of 2- methylaziridine,
The following steps are included:
Step 1, with pump by isopropanolamine, sulfuric acid and liquid alkaline 1:(1.2-2.5 in mass ratio): (3.5-4.8) is separately added into
Into the first measuring tank, the second measuring tank and third measuring tank, first measuring tank, the second measuring tank and third measuring tank control
Temperature processed is at 0-4 DEG C；
Isopropanolamine in first measuring tank is transferred completely into esterification catalysis reaction kettle, turn on agitator by step 2,
It will be all slowly added dropwise by sulfuric acid into esterification catalysis reaction kettle in the second measuring tank with 6-8 hours, control esterification catalysis reaction
Temperature in the kettle is at 45-105 DEG C, and then into esterification catalysis reaction kettle, diatomite carried palladium catalyst, control esterification is added in reaction kettle
Hydrolysis temperature in the kettle 135-185 DEG C reaction 3-5 hours；
Wherein for diatomite carried palladium catalyst using acid diatomite as carrier, active constituent is Pd (a) Fe (b) Au (c)
Cu (d) Cl (e) O (f), a, b, c, d, e, f in bracket are the molar ratio of Pd, Fe, Au, Cu, Cl and O respectively；
Step 3 after sulfuric acid is added dropwise, closes the exhaust-valve of esterification catalysis reaction kettle, is then turned on vacuum pump, controls
Esterification catalysis reacting kettle inner pressure controls esterification catalysis reactor temperature at 100-120 DEG C, carries out in 0.035-0.095Mpa
Vacuum concentration dehydration 1-3 hours, esterification catalysis material in reactor cools down after being evaporated, when esterification catalysis reactor temperature
When being down to 20-70 DEG C, the liquid alkaline in third measuring tank is slowly added in esterification catalysis reaction kettle, controls esterification catalysis reaction kettle
15-45 DEG C of interior temperature after reaction 1-3 hours, obtains reaction head product；
The reaction head product that step 3 obtains is fully transferred in just distillation still, then to first distillation still by step 4
Receive that piece alkali is added in kettle, stirring while carries out atmospheric fractions, collects 50-95 DEG C fraction 5-9 hour, distillate at the beginning of obtaining；
Step 5, the first distillate that step 4 is obtained repeat step 4 three times, and it is small to collect 50-95 DEG C of fraction 5-9
When, purifying head product will be obtained；
The purifying head product that step 5 obtains is transferred to smart distillation still, then puts into piece into smart distillation still by step 6
Pressure in smart distillation still is down to 0.03-0.09Mpa vacuum, carries out low-pressure distillation, collects 42-55 DEG C fraction 8-10 hours by alkali,
Obtain 2- methylaziridine.
Preferably, isopropanolamine concentration is not less than 99% in the step 1, and the sulfuric acid is the concentrated sulfuric acid, the concentrated sulfuric acid
Concentration is not less than 98%, and the liquid alkaline is liquid sodium hydroxide, and the liquid alkaline concentration is 32-35%.
Preferably, esterification catalysis reaction kettle is provided with circulating water cooling system, the esterification catalysis reaction in the step 2
Kettle is additionally provided with the first jacket steam heat riser.
Preferably, the ratio of a, b, c and d are 1:(1-2 in the step 2): (0.5-1): (0.2-0.5)
Preferably, the first distillation still in the step 4 is provided with the second jacket steam heat riser and first distillation and reflux is cold
Condenser, the just distillation still receive on kettle or even have just distillation chilled brine condenser.
Preferably, piece alkali is solid NuaO in the step 4, and described alkali purity is not less than 96%, described alkali
Mass ratio with isopropanolamine in step 1 is (0.05-0.1): 1.
Preferably, smart distillation still is provided with third jacket steam heat riser, smart distillation and reflux condensation in the step 6
Device and essence distillation chilled brine condenser.
Preferably, piece alkali is solid NuaO in the step 6, and described alkali purity is not less than 96%, described alkali
Mass ratio with isopropanolamine in step 1 is (0.05-0.1): 1.
Compared with prior art, beneficial effects of the present invention:
What the present invention innovated uses isopropanolamine, sulfuric acid and liquid alkaline for Material synthesis 2- methylaziridine, synthesis condition temperature
Be conducive to large-scale industrial production；Furthermore synthesis material is simple, is esterified using sulfuric ester, then is hydrolyzed with liquid alkaline, distills pure
Change process is purified with piece alkali again, and by-product is few, environmentally protective；Just distillation is carried out using normal pressure, then carries out smart distillation with low pressure, is obtained
To 2- methylaziridine purity reach 99% or more.
Detailed description of the invention
Fig. 1 is synthetic reaction schematic diagram of the invention.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is described in detail, but the present invention can be defined by the claims and
The multitude of different ways of covering is implemented.
Embodiment 1
One, raw material
Two, reaction principle
The present invention is Material synthesis 2- methylaziridine, composition principle such as Fig. 1 institute by isopropanolamine, sulfuric acid and liquid alkaline
Show.
Three, synthesis process
(1) esterification catalysis
Isopropanolamine 100kg, sulfuric acid 133kg and liquid alkaline 385kg are added separately to the first measuring tank, the second metering with pump
In tank and third measuring tank, by the first measuring tank of cooling system, the second measuring tank and third measure control temperature at 4 DEG C.
Isopropanolamine in first measuring tank is transferred completely into esterification catalysis reaction kettle, turn on agitator, by second
Sulfuric acid in measuring tank is added dropwise in esterification catalysis reaction kettle and (opens circulating water in due course), control temperature in the kettle at 100 DEG C,
It is added dropwise 7 hours, is added dropwise, then diatomite carried palladium catalyst Pd (2) Fe (3) is added in reaction kettle into esterification catalysis reaction kettle
Au (2) Cu (1) Cl (4) O (8), control esterification catalysis reactor temperature react 5 hours at 185 DEG C；
Exhaust-valve on kettle, boiled water vacuum pump are closed, while opening the heating of the first jacket steam, carries out vacuum concentration dehydration,
Esterification catalysis reacting kettle inner pressure is controlled in 0.065Mpa, 110 DEG C of temperature in the kettle, carries out vacuum concentration dehydration 2 hours, esterification water
Cool down after material is evaporated in solution reaction kettle, it, will be in third measuring tank when esterification catalysis reactor temperature is down to 50 DEG C
Liquid alkaline is slowly added into reaction kettle.30 DEG C of esterification catalysis reactor temperature of control, after reaction 2 hours, discharging to first distillation still
In.
(2) just distillation, essence distillation
Receive addition solid NuaO 5kg in kettle to first distillation still, opens stirring, while opening the second of just distillation still
Jacket steam heating device, opens first distillation and reflux condenser recirculated water on destilling tower, and opening receives first distiller condenser on kettle
Chilled brine receives 50-95 DEG C of fraction of tower temperature 7 hours, obtains just distillate；First distillate repeats three times just distillation, receives
Collect 50-95 DEG C fraction 7 hours, purifying head product will be obtained；Purifying head product is transferred to smart distillation still, then to smart distillation still
Solid NuaO 5kg is added in interior investment piece alkali, opens vertical type vacuum pump, and essence steams kettle vacuum valve, will be formed in kettle
0.06Mpa vacuum closes vacuum valve on kettle, opens stirring, opens steam valve heating, opens simultaneously smart distiller condenser chilled brine and essence
Distillation and reflux condenser opens pans jacket refrigerating salt water, collects 42-55 DEG C fraction 9 hours, obtains the 2- first of purity 99%
Base aziridine, in terms of isopropanolamine, yield reaches 83%.
As can be seen from the above embodiments, raw material of the present invention are cheap, and react mild, and technical process by-product
It is few, environmentally protective, obtained finished product purity is high, and also combined coefficient is high, is suitable for being mass produced, can be significantly reduced into
Originally it and reduces environmental pollution.
Embodiment 2
One, raw material
| Material name | Specification % | Producer | Quantity kg |
| Isopropanolamine | >=99% | The rich chemical industry that is full of in Shanghai | 100 |
| Sulfuric acid | >=98% | Upper Hainan waffle work | 120 |
| Liquid alkaline | >=32% | Join China in Tianjin and rises chemical industry | 350 |
| Solid NuaO | >=96% | Join China in Tianjin and rises chemical industry | 30 |
Two, reaction principle
The present invention is Material synthesis 2- methylaziridine, composition principle such as Fig. 1 institute by isopropanolamine, sulfuric acid and liquid alkaline
Show.
Two, synthesis process
Three, (1) esterification catalysis
Isopropanolamine 100kg, sulfuric acid 120kg and liquid alkaline 350kg are added separately to the first measuring tank, the second metering with pump
In tank and third measuring tank, by the first measuring tank of cooling system, the second measuring tank and third measure control temperature at 2 DEG C.
Isopropanolamine in first measuring tank is transferred completely into esterification catalysis reaction kettle, turn on agitator, by second
Sulfuric acid in measuring tank is added dropwise in esterification catalysis reaction kettle and (opens circulating water in due course), control temperature in the kettle at 45 DEG C,
It is added dropwise 6 hours, is added dropwise, then diatomite carried palladium catalyst Pd (2) Fe (3) is added in reaction kettle into esterification catalysis reaction kettle
Au (2) Cu (1) Cl (4) O (8), control esterification catalysis reactor temperature react 4 hours at 135 DEG C；
Exhaust-valve on kettle, boiled water vacuum pump are closed, while opening the heating of the first jacket steam, carries out vacuum concentration dehydration,
Esterification catalysis reacting kettle inner pressure is controlled in 0.035Mpa, 100 DEG C of temperature in the kettle, carries out vacuum concentration dehydration 1 hour, esterification water
Cool down after material is evaporated in solution reaction kettle, it, will be in third measuring tank when esterification catalysis reactor temperature is down to 20 DEG C
Liquid alkaline is slowly added into reaction kettle.15 DEG C of esterification catalysis reactor temperature of control, after reaction 1 hour, discharging to first distillation still
In.
(3) just distillation, essence distillation
Receive addition solid NuaO 8kg in kettle to first distillation still, opens stirring, while opening the second of just distillation still
Jacket steam heating device, opens first distillation and reflux condenser recirculated water on destilling tower, and opening receives first distiller condenser on kettle
Chilled brine receives 50-95 DEG C of fraction of tower temperature 5 hours, obtains just distillate；First distillate repeats three times just distillation, receives
Collect 50-95 DEG C fraction 5 hours, purifying head product will be obtained；Purifying head product is transferred to smart distillation still, then to smart distillation still
Solid NuaO 6kg is added in interior investment piece alkali, opens vertical type vacuum pump, and essence steams kettle vacuum valve, will be formed in kettle
0.03Mpa vacuum closes vacuum valve on kettle, opens stirring, opens steam valve heating, opens simultaneously smart distiller condenser chilled brine and essence
Distillation and reflux condenser opens pans jacket refrigerating salt water, collects 42-55 DEG C fraction 8 hours, obtains the 2- first of purity 99%
Base aziridine, in terms of isopropanolamine, yield reaches 81%.
Embodiment 3
One, raw material
Two, reaction principle
The present invention is Material synthesis 2- methylaziridine, composition principle such as Fig. 1 institute by isopropanolamine, sulfuric acid and liquid alkaline
Show.
Four, synthesis process
(1) esterification catalysis
Isopropanolamine 100kg, sulfuric acid 250kg and liquid alkaline 480kg are added separately to the first measuring tank, the second metering with pump
In tank and third measuring tank, by the first measuring tank of cooling system, the second measuring tank and third measure control temperature at 0 DEG C.
Isopropanolamine in first measuring tank is transferred completely into esterification catalysis reaction kettle, turn on agitator, by second
Sulfuric acid in measuring tank is added dropwise in esterification catalysis reaction kettle and (opens circulating water in due course), control temperature in the kettle at 105 DEG C,
It is added dropwise 8 hours, is added dropwise, then diatomite carried palladium catalyst Pd (2) Fe (3) is added in reaction kettle into esterification catalysis reaction kettle
Au (2) Cu (1) Cl (4) O (8), control esterification catalysis reactor temperature react 3 hours at 160 DEG C；
Exhaust-valve on kettle, boiled water vacuum pump are closed, while opening the heating of the first jacket steam, carries out vacuum concentration dehydration,
Esterification catalysis reacting kettle inner pressure is controlled in 0.095Mpa, 120 DEG C of temperature in the kettle, carries out vacuum concentration dehydration 3 hours, esterification water
Cool down after material is evaporated in solution reaction kettle, it, will be in third measuring tank when esterification catalysis reactor temperature is down to 70 DEG C
Liquid alkaline is slowly added into reaction kettle.45 DEG C of esterification catalysis reactor temperature of control, after reaction 3 hours, discharging to first distillation still
In.
(4) just distillation, essence distillation
To first distillation still receive solid NuaO 40kg is added in kettle, open stirring, while the of distillation still at the beginning of opening
Two jacket steam heating devices, open first distillation and reflux condenser recirculated water on destilling tower, and opening receives just distillation condensation on kettle
Device chilled brine receives 50-95 DEG C of fraction of tower temperature 9 hours, obtains just distillate；First distillate repeats three times just distillation,
It collects 50-95 DEG C fraction 9 hours, purifying head product will be obtained；Purifying head product is transferred to smart distillation still, is then distilled to essence
Solid NuaO 40kg is added in investment piece alkali in kettle, opens vertical type vacuum pump, and essence steams kettle vacuum valve, will be formed in kettle
0.09Mpa vacuum closes vacuum valve on kettle, opens stirring, opens steam valve heating, opens simultaneously smart distiller condenser chilled brine and essence
Distillation and reflux condenser opens pans jacket refrigerating salt water, collects 42-55 DEG C fraction 10 hours, obtains the 2- of purity 99%
Methylaziridine, in terms of isopropanolamine, yield reaches 86%.
As can be seen from the above embodiments, raw material of the present invention are cheap, and react mild, and technical process by-product
It is few, environmentally protective, obtained finished product purity is high, and also combined coefficient is high, is suitable for being mass produced, can be significantly reduced into
Originally it and reduces environmental pollution.
The foregoing is merely the preferred embodiments of invention, are not intended to limit the scope of the invention, all to utilize this
It simply modifies or converts made by description of the invention content, be applied directly or indirectly in other relevant technical fields, same
Reason is included within the scope of the present invention.
Claims (8)
1. a kind of preparation method of 2- methylaziridine, which comprises the following steps:
Step 1, with pump by isopropanolamine, sulfuric acid and liquid alkaline 1:(1.2-2.5 in mass ratio): (3.5-4.8) is added separately to
In first measuring tank, the second measuring tank and third measuring tank, first measuring tank, the second measuring tank and the control of third measuring tank
Temperature is at 0-4 DEG C；
Step 2, the isopropanolamine in the first measuring tank is transferred completely into esterification catalysis reaction kettle, and turn on agitator uses 6-
It will be all slowly added dropwise by sulfuric acid into esterification catalysis reaction kettle within 8 hours, controlled in esterification catalysis reaction kettle in second measuring tank
Temperature is at 45-105 DEG C, and then into esterification catalysis reaction kettle, diatomite carried palladium catalyst is added in reaction kettle, controls esterification catalysis
Reactor temperature 135-185 DEG C reaction 3-5 hours；
Wherein for diatomite carried palladium catalyst using acid diatomite as carrier, active constituent is Pd (a) Fe (b) Au (c) Cu (d)
Cl (e) O (f), a, b, c, d, e, f in bracket are the molar ratio of Pd, Fe, Au, Cu, Cl and O respectively；
Step 3 closes the exhaust-valve of esterification catalysis reaction kettle, is then turned on vacuum pump, controls esterification catalysis reacting kettle inner pressure
In 0.035-0.095Mpa, esterification catalysis reactor temperature is controlled at 100-120 DEG C, carries out vacuum concentration dehydration 1-3 hours,
Esterification catalysis material in reactor cools down after being evaporated, when esterification catalysis reactor temperature is down to 20-70 DEG C, by third
Liquid alkaline in measuring tank is slowly added in esterification catalysis reaction kettle, controls 15-45 DEG C of esterification catalysis reactor temperature, reaction
After 1-3 hours, reaction head product is obtained；
The reaction head product that step 3 obtains is fully transferred in just distillation still, then to the receiving of first distillation still by step 4
Piece alkali is added in kettle, stirring while carries out atmospheric fractions, collects 50-95 DEG C fraction 5-9 hour, distillate at the beginning of obtaining；
Step 5, the first distillate that step 4 is obtained repeat step 4 three times, collect 50-95 DEG C fraction 5-9 hours, will
Obtain purifying head product；
The purifying head product that step 5 obtains is transferred to smart distillation still by step 6, and piece alkali is then put into smart distillation still, will
Pressure is down to 0.03-0.09Mpa vacuum in smart distillation still, carries out low-pressure distillation, collects 42-55 DEG C fraction 8-10 hours, obtains
2- methylaziridine.
2. the preparation method of 2- methylaziridine according to claim 1, which is characterized in that isopropanol in the step 1
Amine concentration is not less than 99%, and the sulfuric acid is the concentrated sulfuric acid, and the concentrated sulfuric acid concentration is not less than 98%, and the liquid alkaline is liquid hydroxide
Sodium, the liquid alkaline concentration are 32-35%.
3. the preparation method of 2- methylaziridine according to claim 1, which is characterized in that esterification water in the step 2
Solution reaction kettle is provided with circulating water cooling system, and the esterification catalysis reaction kettle is additionally provided with the first jacket steam heat riser.
4. the preparation method of 2- methylaziridine according to claim 1, which is characterized in that a, b, c in the step 2
Ratio with d is 1:(1-2): (0.5-1): (0.2-0.5).
5. the preparation method of 2- methylaziridine according to claim 1, which is characterized in that the first steaming in the step 4
It evaporates kettle and is provided with the second jacket steam heat riser and first distillation and reflux condenser, the just distillation still receives even to have on kettle
Just distillation chilled brine condenser.
6. the preparation method of 2- methylaziridine according to claim 1, which is characterized in that piece alkali is in the step 4
Solid NuaO, described alkali purity are not less than 96%, and the mass ratio of isopropanolamine is (0.05- in described alkali and step 1
0.1): 1.
7. the preparation method of 2- methylaziridine according to claim 1, which is characterized in that essence distillation in the step 6
Kettle is provided with third jacket steam heat riser, smart distillation and reflux condenser and essence distillation chilled brine condenser.
8. the preparation method of 2- methylaziridine according to claim 1, which is characterized in that piece alkali is in the step 6
Solid NuaO, described alkali purity are not less than 96%, and the mass ratio of isopropanolamine is (0.05- in described alkali and step 1
0.1): 1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112266347A (en) * | 2020-11-13 | 2021-01-26 | 西安近代化学研究所 | Preparation method of high-purity ethylene imine |
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| CN112266347A (en) * | 2020-11-13 | 2021-01-26 | 西安近代化学研究所 | Preparation method of high-purity ethylene imine |
| CN112266347B (en) * | 2020-11-13 | 2022-11-15 | 西安近代化学研究所 | Preparation method of high-purity ethylene imine |
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