CN106432028B - A kind of preparation method and its usage of the 2-Pyrrolidone solution of alkali metal 2-Pyrrolidone salt - Google Patents
A kind of preparation method and its usage of the 2-Pyrrolidone solution of alkali metal 2-Pyrrolidone salt Download PDFInfo
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- CN106432028B CN106432028B CN201610730880.7A CN201610730880A CN106432028B CN 106432028 B CN106432028 B CN 106432028B CN 201610730880 A CN201610730880 A CN 201610730880A CN 106432028 B CN106432028 B CN 106432028B
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- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 229910052783 alkali metal Inorganic materials 0.000 title claims abstract description 69
- -1 alkali metal 2-Pyrrolidone salt Chemical class 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 44
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 40
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 12
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 17
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 17
- 229910052700 potassium Inorganic materials 0.000 claims description 17
- 239000011591 potassium Substances 0.000 claims description 17
- 229910052708 sodium Inorganic materials 0.000 claims description 17
- 239000011734 sodium Substances 0.000 claims description 17
- 238000003860 storage Methods 0.000 claims description 14
- 238000006073 displacement reaction Methods 0.000 claims description 8
- 230000004888 barrier function Effects 0.000 claims description 7
- 239000012295 chemical reaction liquid Substances 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 239000003350 kerosene Substances 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 229910003251 Na K Inorganic materials 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 4
- 239000000956 alloy Substances 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 4
- 229920003023 plastic Polymers 0.000 claims description 4
- 239000004033 plastic Substances 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 7
- 239000012752 auxiliary agent Substances 0.000 abstract description 4
- 238000007086 side reaction Methods 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract 1
- 239000000376 reactant Substances 0.000 abstract 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 7
- 239000001103 potassium chloride Substances 0.000 description 7
- 235000011164 potassium chloride Nutrition 0.000 description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- BTCSSZJGUNDROE-UHFFFAOYSA-N gamma-aminobutyric acid Chemical compound NCCCC(O)=O BTCSSZJGUNDROE-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 5
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 5
- 239000006227 byproduct Substances 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 150000004040 pyrrolidinones Chemical class 0.000 description 4
- 150000003953 γ-lactams Chemical group 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 229960003692 gamma aminobutyric acid Drugs 0.000 description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- PHXKQKZYWQUGLW-UHFFFAOYSA-N 1h-pyrrole;pyrrolidin-2-one Chemical compound C=1C=CNC=1.O=C1CCCN1 PHXKQKZYWQUGLW-UHFFFAOYSA-N 0.000 description 1
- KGIGUEBEKRSTEW-UHFFFAOYSA-N 2-vinylpyridine Chemical compound C=CC1=CC=CC=N1 KGIGUEBEKRSTEW-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 150000001345 alkine derivatives Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 150000003997 cyclic ketones Chemical class 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000002815 homogeneous catalyst Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- GDNULDIPPDQVRH-UHFFFAOYSA-N potassium;pyrrolidin-2-one Chemical class [K].O=C1CCCN1 GDNULDIPPDQVRH-UHFFFAOYSA-N 0.000 description 1
- 150000003239 pyrrolones Chemical class 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D207/18—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member
- C07D207/22—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D207/24—Oxygen or sulfur atoms
- C07D207/26—2-Pyrrolidones
- C07D207/263—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D207/18—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member
- C07D207/22—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D207/24—Oxygen or sulfur atoms
- C07D207/26—2-Pyrrolidones
- C07D207/263—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms
- C07D207/267—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to the ring nitrogen atom
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pyrrole Compounds (AREA)
Abstract
A kind of preparation method and its usage of the 2-Pyrrolidone solution of alkali metal 2-Pyrrolidone salt, belongs to chemical industry method and technology field.The following steps are included: 1) reaction unit nitrogen is replaced；2) 2-Pyrrolidone of sufficient amount is heated into liquid, it is spare；3) by the alkali metal liquid of sufficient amount and 2-Pyrrolidone liquid reactant mixture, the 2-Pyrrolidone solution of alkali metal 2-Pyrrolidone salt is obtained, nitrogen-sealed saves.A kind of preparation method and its usage of the 2-Pyrrolidone solution of above-mentioned alkali metal 2-Pyrrolidone salt, without other solvents or auxiliary agent in preparation process, without handling the second solvent, without catalyst, dispersed without auxiliary agent and is mixed, the lower reaction temperature of a little higher than alkali metal fusing point, extremely low side reaction are simple, economical and safe on a manufacturing scale.
Description
Technical field
The invention belongs to chemical industry method and technology field, specially a kind of 2-Pyrrolidone of alkali metal 2-Pyrrolidone salt is molten
The preparation method and its usage of liquid.
Background technique
Alkali metal 2-Pyrrolidone salt prepares vinylpyridine mainly as catalyst, for 2-Pyrrolidone and acetylene reaction
The catalyst of pyrrolidone.
Patent No.: 200810072060.9, describe the 2-Pyrrolidone and second of the potassium of pyrrolidones containing homogeneous catalyst
The method of alkyne reaction preparing ethylene base pyrrolidones, does not describe the preparation method of pyrrolidones potassium.
2-Pyrrolidone is discussed in " chemical science and technology market " 2004 the 5th phase " synthesis of n-vinyl pyrrolidone " text
Catalyst with acetylene reaction preparing ethylene base pyrrolidones is 2-Pyrrolidone sylvite, and the preparation method of 2-Pyrrolidone sylvite is 2-
Pyrrolidones and potassium hydroxide are dehydrated in the case where vacuum or nitrogen are bubbled to be made, Batch Process.
Patent No.: 200880119517.5, the catalyst for describing 2- pyrrolidones and acetylene reaction is alkali metal pyrrole
Pyrrolidone salt is made by 2- pyrrolidones with alkali metal hydroxide or reaction of alkali metal alkoxide.
Patent No.: 200410061451.2 and 201110354299.7 two patents respectively describe one kind by 2- pyrrole
Pyrrolidone hydrolysis and produces the method for 4-Aminobutanoicacid after being acidified under alkalinity.
The reaction equation of 2-Pyrrolidone and potassium hydroxide is as shown in formula 3 and formula 4:
The reaction product of formula 3 is that 2-Pyrrolidone sylvite is purpose product, and alkalinity is strong, and catalytic activity is good；The reaction of formula 4 produces
Object is 4-Aminobutanoicacid sylvite, by-product, alkaline weak, catalytically inactive.It is generally quickly de- to reduce the method that side reaction occurs
Water, quick separating product.The production quantity of by-product 4-Aminobutanoicacid sylvite is generally 40-50%, can pass through the side of constant-current titration
Method is detected.
In the industrial production, in order to guarantee catalytic activity, 2-Pyrrolidone potassium salts content is improved, increase hydrogen-oxygen is often taken
The method for changing potassium inventory realizes, the increase of by-product when inevitably catalyst being caused to manufacture, 2-Pyrrolidone with
Polymeric by-products when acetylene reaction increase, and yield is low, block reactor, frequently stop production.
It is reacted using alkali metal with 2-Pyrrolidone, prepares 2-Pyrrolidone sylvite catalyst, because the reaction time is short, reaction
Speed is fast, and side reaction is few, and catalytic activity is high, high income, is a selection well.But a large amount of hydrogen can be generated in a short time
Gas, and release a large amount of heat will lead to the high safety requirement in commercial scale, in order to effectively carry out alkali metal dispersion and
The removal of heat, the realization of industrial batch production, which is deposited, to acquire a certain degree of difficulty.
Summary of the invention
For the above-mentioned problems in the prior art, it is an object of the invention to design to provide a kind of alkali metal 2- pyrroles
The technical solution of the preparation method and its usage of the 2-Pyrrolidone solution of alkanone salt can reduce unit reactor body accordingly
Long-pending alkali metal inventory, to control the raising of temperature and the occurrence quantity of hydrogen, can simple microreactor quantity repetition
Increase can realize satisfactory commercial production scale, and production cost is low, and reaction process is safe and reliable.
A kind of preparation method of the 2-Pyrrolidone solution of the alkali metal 2-Pyrrolidone salt, it is characterised in that including
Following steps:
1) by 2-Pyrrolidone feed containers, heater, filter, mixer, microreactor, reaction liquid storage tank, alkali gold
Belong to measuring tank and connection system nitrogen displacement, displacement is to oxygen content less than 0.5%；
2) 2-Pyrrolidone of sufficient amount is fitted into 2-Pyrrolidone feed containers, the temperature control of liquid in feed containers
2-Pyrrolidone is heated to 110-130 DEG C with the heated device of the flow of 80-100ml/min at 28 DEG C -35 DEG C, with pump by system, then
It returns to 2-Pyrrolidone feed containers through filter, mixer, microreactor and is switched to 1.5-2.5 minutes before throwing alkali metal
It reacts in liquid storage tank, so that 2-Pyrrolidone and the reaction solution of alkali metal are sent to reacting in liquid storage tank；
3) alkali metal of sufficient amount is entered in alkali metal measuring tank in the protection down of kerosene, alkali metal amount pot liquid
Temperature control at 105-115 DEG C, the nitrogen-sealed pressure of alkali metal measuring tank is set as 0.35-0.45MPa, then passes through pressure
The alkali metal of melting is extruded to be sent into after mixer is mixed with 2-Pyrrolidone from alkali metal measuring tank bottom and enters microreactor
Reaction, the inlet amount of alkali metal are 0.8-2.2 grams/min, and the liquid after reaction is sent into reaction solution after nitrogen replaces abjection hydrogen
In storage tank, the 2-Pyrrolidone solution of the alkali metal 2-Pyrrolidone salt of 0.1-10% is obtained, nitrogen-sealed saves.
The preparation method of the 2-Pyrrolidone solution of a kind of alkali metal 2-Pyrrolidone salt, it is characterised in that described
Alkali metal be sodium, potassium or Na-K alloy.
The preparation method of the 2-Pyrrolidone solution of a kind of alkali metal 2-Pyrrolidone salt, it is characterised in that described
2-Pyrrolidone, molecular structural formula be formula 1:
Also known as: pyrrolones, penta cyclic ketones of nitrogen, butyrolactam.
The preparation method of the 2-Pyrrolidone solution of a kind of alkali metal 2-Pyrrolidone salt, it is characterised in that described
Alkali metal 2-Pyrrolidone salt, molecular structural formula be formula 2:
M: sodium, potassium, Na-K alloy.
A kind of preparation method of the 2-Pyrrolidone solution of alkali metal 2-Pyrrolidone salt, it is characterised in that step
2) in: 2-Pyrrolidone being heated to 115-125 DEG C with the flow of 85-95ml/min heated device with pump, preferably with pump with 88-
2-Pyrrolidone is heated to 118-120 DEG C by the heated device of the flow of 90ml/min.
A kind of preparation method of the 2-Pyrrolidone solution of alkali metal 2-Pyrrolidone salt, it is characterised in that step
3) in: the nitrogen-sealed pressure of alkali metal measuring tank is set as 0.38-0.44MPa, preferably 0.40-0.42MPa.
A kind of preparation method of the 2-Pyrrolidone solution of alkali metal 2-Pyrrolidone salt, it is characterised in that step
3) in: the inlet amount of alkali metal be 0.9-1.8/min, preferably 1.2-1.5 grams/min.
2-Pyrrolidone solution is for preparing the application in vinyl pyrrolidone with acetylene reaction.
Generated hydrogen can simply be deviate from degasser in reaction.
The microreactor system of this paper is continuous system, and the amount for participating in the material of reaction is gram or milliliter grade range reaction
The channel width of device is generally at 1-10000 μm, preferably 10-1000 μm, more preferable between 50-150 μm.Material is stainless steel,
It can choose the materials such as glass, ceramics, plastics.
The mixing of alkali metal and 2-Pyrrolidone is mixed using microporous barrier, first before material enters reactor
It is introduced into a microporous barrier mixer, the aperture of microporous barrier is generally at 1-1000 μm, and preferably 10-800 μm, more preferable 10-100 μ
Between m.Material is stainless steel, also can choose the materials such as ceramics, plastics.
The temperature of reaction is determined by the melting temperature of alkali metal, 2-Pyrrolidone, the temperature of microreactor system
Ensure that alkali metal, 2-Pyrrolidone have smoothly mobility, ordinary circumstance reaction temperature is lower than 2-Pyrrolidone boiling point
It is good.Reaction temperature general control is at 65-240 DEG C, preferably are as follows: 80-200 DEG C, more preferably 100-150 DEG C.
Reaction heat is taken away by excessive 2-Pyrrolidone, and alkali metal inventory is big, and reaction solution is from starting to be reacted to
Temperature rise at the end of reaction with regard to big, general control reaction temperature rise amplitude be 1-120 DEG C, preferably 1-80 DEG C, more preferably
It is 1-50 DEG C.Also it can choose and remove heat with heat exchanger.
The concentration of alkali metal 2-Pyrrolidone salt is realized by the proportional quantity of control alkali metal and 2-Pyrrolidone, instead
Answer middle 2-Pyrrolidone relative to alkali metal be it is excessive, it is excessive how much situation and reaction solution to be precipitated according to the presence or absence of solution
Temperature rises situation and determines.
Reaction pressure is determined according to mixer, reactor resistance, the factors such as reaction solution temperature rise.
Alkali metal carries out in the case where no mechanical stirring with reacting for 2-Pyrrolidone, reason be microreactor and
The mixed effect of preposition micropore mixer is enough.
A kind of preparation method and its usage of the 2-Pyrrolidone solution of above-mentioned alkali metal 2-Pyrrolidone salt, preparation process
In be not necessarily to catalyst without handling the second solvent without other solvents or auxiliary agent, dispersed without auxiliary agent and mixed, slightly
Higher than the lower reaction temperature of alkali metal fusing point, extremely low side reaction is simple, economical on a manufacturing scale and safety
's.
Specific embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
By 2-Pyrrolidone container, heater, filter, mixer, microreactor, reaction liquid storage tank and connection system nitrogen
Gas displacement, displacement is to oxygen content less than 0.5%.
By the 2-Pyrrolidone of sufficient amount, (fusing point is 24.6 DEG C, and the boiling point under normal pressure is 245 DEG C, density 1.116(25/4
DEG C)) be fitted into feed containers, the temperature of liquid is controlled at 28 DEG C or more in feed containers, it is therefore an objective to be kept at 2-Pyrrolidone
In liquid condition.2-Pyrrolidone is heated to 120 DEG C with the flow of 90ml/min heated device with pump, using filter, is mixed
Clutch, microreactor return to feed storage tank, 2 minutes before throwing metallic sodium, switch in reaction liquid storage tank, so that 2-Pyrrolidone
It send with the reaction solution of sodium to reacting in liquid storage tank.
Sodium measuring tank and sodium feeding line nitrogen are replaced, displacement is to oxygen content less than 0.5%.By the sodium (fusing point of sufficient amount
It is 97.82 DEG C, relative density (H2O) 0.968) enter in sodium measuring tank in the protection down of kerosene, measure the temperature of pot liquid
Control is at 105 DEG C or more, it is therefore an objective to keep metallic sodium in a molten state.The nitrogen-sealed pressure of sodium measuring tank is set as
It is mixed can be measured pot bottom extrusion feeding from sodium by pressure because the sodium of melting is than kerosene weight by 0.4MPa for molten metal sodium
Clutch mixes laggard reactor reaction in a subtle way with 2-Pyrrolidone, and the inlet amount of metallic sodium is 1.0 grams/min, the liquid after reaction
It is sent into reaction liquid storage tank after nitrogen replaces abjection hydrogen, the 2-Pyrrolidone for obtaining about 4.6%2- pyrrolidones sodium salt is molten
Liquid, nitrogen-sealed save.
Embodiment 2
2-Pyrrolidone feeding system replaces sodium with embodiment 1, with potassio.
Potassium measuring tank and potassium feeding line nitrogen are replaced, displacement is to oxygen content less than 0.5%.By the potassium (fusing point of sufficient amount
63.25 DEG C, density 0.86g/cm3) enter in potassium measuring tank in the protection down of kerosene, the temperature for measuring pot liquid is controlled 70
DEG C or more, it is therefore an objective to keep metallic potassium in a molten state.The nitrogen-sealed pressure of potassium measuring tank is set as 0.4MPa, because of melting
Potassium it is slightly heavier than kerosene, molten metal potassium can be measured from potassium by pot bottom by pressure and extruded and be sent into mixer and 2- pyrroles
Alkanone mixes laggard reactor reaction in a subtle way, and the inlet amount of metallic potassium is 0.5 gram/min, and the liquid after reaction is replaced de- through nitrogen
It is sent into after hydrogen in reaction liquid storage tank out, obtains the 2-Pyrrolidone solution of about 1.6%2- pyrrolidones sylvite, nitrogen-sealed is protected
It deposits.
Claims (8)
1. a kind of preparation method of the 2-Pyrrolidone solution of alkali metal 2-Pyrrolidone salt, it is characterised in that including following step
It is rapid:
1) by 2-Pyrrolidone feed containers, heater, filter, mixer, microreactor, reaction liquid storage tank, alkali metal
Measuring tank and connection system nitrogen displacement, displacement is to oxygen content less than 0.5%；
2) 2-Pyrrolidone of sufficient amount is fitted into 2-Pyrrolidone feed containers, the temperature control of liquid exists in feed containers
28 DEG C -35 DEG C, 2-Pyrrolidone is heated to 110-130 DEG C with the flow of 80-100ml/min heated device with pump, using
Filter, mixer, microreactor return to 2-Pyrrolidone feed containers and switch to reaction 1.5-2.5 minutes before throwing alkali metal
In liquid storage tank, so that 2-Pyrrolidone and the reaction solution of alkali metal are sent to reacting in liquid storage tank；
3) alkali metal of sufficient amount is entered in alkali metal measuring tank in the protection down of kerosene, the temperature of alkali metal amount pot liquid
At 105-115 DEG C, the nitrogen-sealed pressure of alkali metal measuring tank is set as 0.35-0.45MPa, then will be melted by pressure for degree control
The alkali metal melted extrudes feeding mixer from alkali metal measuring tank bottom and mixes laggard reactor reaction in a subtle way with 2-Pyrrolidone,
At 65-240 DEG C, the inlet amount of alkali metal is 0.8-2.2 grams/min for reaction temperature control, and the liquid after reaction is replaced de- through nitrogen
It is sent into after hydrogen in reaction liquid storage tank out, obtains the 2-Pyrrolidone solution of the alkali metal 2-Pyrrolidone salt of 0.1-10%, nitrogen
It is sealed；
The microreactor is made of stainless steel, glass, ceramics or plastics, and the channel width of microreactor is 1-10000 μm,
Mixer is stainless steel, microporous barrier mixer made of ceramics or plastics, and the aperture of microporous barrier is 1-1000 μm；
The alkali metal is sodium, potassium or Na-K alloy；
The alkali metal 2-Pyrrolidone salt, molecular structural formula are formula 2:
M: sodium, potassium, Na-K alloy.
2. a kind of preparation method of the 2-Pyrrolidone solution of alkali metal 2-Pyrrolidone salt as described in claim 1, special
Sign is in step 2: 2-Pyrrolidone being heated to 115-125 DEG C with the flow of 85-95ml/min heated device with pump.
3. a kind of preparation method of the 2-Pyrrolidone solution of alkali metal 2-Pyrrolidone salt as described in claim 1, special
Sign is in step 3): the nitrogen-sealed pressure of alkali metal measuring tank is set as 0.38-0.44MPa.
4. a kind of preparation method of the 2-Pyrrolidone solution of alkali metal 2-Pyrrolidone salt as described in claim 1, special
Sign is in step 3): the inlet amount of alkali metal is 0.9-1.8g/min.
5. a kind of preparation method of the 2-Pyrrolidone solution of alkali metal 2-Pyrrolidone salt as described in claim 1, special
Sign is that the channel width of microreactor is 10-1000 μm, and the aperture of mixer microporous barrier is 10-800 μm.
6. a kind of preparation method of the 2-Pyrrolidone solution of alkali metal 2-Pyrrolidone salt as described in claim 1, special
Sign is that the channel width of microreactor is 50-150 μm；The aperture of mixer microporous barrier is 10-100 μm.
7. a kind of preparation method of the 2-Pyrrolidone solution of alkali metal 2-Pyrrolidone salt as described in claim 1, special
Sign is reaction temperature general control at 65-240 DEG C, and the amplitude that control reaction temperature rises is 1-120 DEG C.
8. a kind of preparation method of the 2-Pyrrolidone solution of alkali metal 2-Pyrrolidone salt as described in claim 1, special
Sign is reaction temperature general control at 80-200 DEG C, and the amplitude that control reaction temperature rises is 1-50 DEG C.
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| CN201610730880.7A CN106432028B (en) | 2016-08-26 | 2016-08-26 | A kind of preparation method and its usage of the 2-Pyrrolidone solution of alkali metal 2-Pyrrolidone salt |
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|---|---|---|---|
| CN201610730880.7A CN106432028B (en) | 2016-08-26 | 2016-08-26 | A kind of preparation method and its usage of the 2-Pyrrolidone solution of alkali metal 2-Pyrrolidone salt |
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| CN112574088B (en) * | 2019-09-30 | 2022-11-04 | 中国石油化工股份有限公司 | Method for synthesizing N-vinyl pyrrolidone |
| CN110903229B (en) * | 2019-12-19 | 2021-08-31 | 清华大学 | Synthesis method of N-vinyl pyrrolidone |
| CN111039843A (en) * | 2019-12-19 | 2020-04-21 | 清华大学 | Synthesis process, synthesis system and application of N-vinyl pyrrolidone |
| CN114425239B (en) * | 2020-10-15 | 2023-05-02 | 中国石油化工股份有限公司 | Microchannel permeation gasification device and method for synthesizing pyrrolidone alkali metal salt |
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Denomination of invention: Preparation method and application of 2-pyrrolidone solution of alkali metal 2-pyrrolidone salt Granted publication date: 20191025 Pledgee: Industrial and Commercial Bank of China Limited Quzhou Kecheng sub branch Pledgor: Quzhou Jianhua Nanhang Pharmaceutical Co.,Ltd. Registration number: Y2024330001384 |
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