CN106432028A - Preparation method and application of 2-pyrrolidinone solution of alkali metal 2-pyrrolidinone salt - Google Patents
Preparation method and application of 2-pyrrolidinone solution of alkali metal 2-pyrrolidinone salt Download PDFInfo
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- CN106432028A CN106432028A CN201610730880.7A CN201610730880A CN106432028A CN 106432028 A CN106432028 A CN 106432028A CN 201610730880 A CN201610730880 A CN 201610730880A CN 106432028 A CN106432028 A CN 106432028A
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- pyrrolidone
- alkali metal
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- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 229910052783 alkali metal Inorganic materials 0.000 title claims abstract description 70
- -1 alkali metal 2-pyrrolidinone salt Chemical class 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 41
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 14
- 238000006073 displacement reaction Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000002844 melting Methods 0.000 claims abstract description 4
- 230000008018 melting Effects 0.000 claims abstract description 4
- 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
- 239000000376 reactant 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
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 6
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 6
- 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
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 230000004888 barrier function Effects 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 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
- 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
- 238000011068 loading method Methods 0.000 claims description 3
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 2
- 150000003997 cyclic ketones Chemical class 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 150000003239 pyrrolones Chemical class 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 6
- 238000007086 side reaction Methods 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 4
- 239000006185 dispersion Substances 0.000 abstract description 2
- 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
- 230000000694 effects Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 150000004040 pyrrolidinones Chemical class 0.000 description 4
- 150000003953 γ-lactams Chemical group 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229960003692 gamma aminobutyric acid Drugs 0.000 description 3
- 150000002431 hydrogen Chemical class 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
- 239000012752 auxiliary agent Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000009835 boiling Methods 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
- 238000013019 agitation Methods 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 150000001345 alkine derivatives Chemical class 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000007789 gas Substances 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
- 239000000155 melt Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- GDNULDIPPDQVRH-UHFFFAOYSA-N potassium;pyrrolidin-2-one Chemical class [K].O=C1CCCN1 GDNULDIPPDQVRH-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000000630 rising effect 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
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
The invention provides a preparation method and application of a 2-pyrrolidinone solution of alkali metal 2-pyrrolidinone salt, and belongs to the technical field of chemical methods. The method includes the following steps that firstly, nitrogen displacement is conducted in a reaction device; secondly, an enough amount of 2-pyrrolidinone is heated into liquid for use; thirdly, an enough amount of alkali metal liquid is mixed with and reacts with 2-pyrrolidinone liquid to obtain the 2-pyrrolidinone solution of alkali metal 2-pyrrolidinone salt, and the 2-pyrrolidinone solution is sealed with nitrogen and preserved. In the preparation process, other solvents or auxiliaries are not needed, a second solvent does not need to be processed, catalysts are not needed, the auxiliaries are not needed for dispersion and mixing, reaction temperature is low and slightly higher than the melting point of alkali metal, side reactions are extremely low, and the production scale is simple, economical and safe.
Description
Technical field
The invention belongs to chemical industry method and technology field, the 2-Pyrrolidone of specially a kind of alkali metal 2-Pyrrolidone salt is molten
The preparation method and its usage of liquid.
Background technology
Alkali metal 2-Pyrrolidone salt, mainly as catalyst, prepares vinylpyridine for 2-Pyrrolidone and acetylene reaction
The catalyst of pyrrolidone.
Patent No.：200810072060.9, describe 2-Pyrrolidone and the 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.
《Chemical science and technology market》2004 the 5th phases《The synthesis of NVP》One literary composition discusses 2-Pyrrolidone
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 under vacuum or nitrogen bubble and prepare, Batch Process.
Patent No.：200880119517.5, the catalyst describing 2-pyrrolidones with acetylene reaction is alkali metal pyrrole
Pyrrolidone salt, is prepared with alkali metal hydroxide or reaction of alkali metal alkoxide by 2-pyrrolidones.
Patent No.：Two patents of 200410061451.2 and 201110354299.7 respectively describe a kind of by 2-pyrrole
Pyrrolidone hydrolysis produce the method for 4-Aminobutanoicacid after being acidified under alkalescence.
The reaction equation of 2-Pyrrolidone and potassium hydroxide is as shown in formula 3 and formula 4：
The product of formula 3 be 2-Pyrrolidone sylvite be purpose product, alkalescence is strong, and catalysis activity is good；The product of formula 4 is
4-Aminobutanoicacid sylvite, accessory substance, alkalescence is weak, catalytically inactive.Reduce the way that side reaction occurs and be generally fast dewatering, fast
Speed separates product.The growing amount of accessory substance 4-Aminobutanoicacid sylvite is generally 40-50%, can be entered by the method for constant-current titration
Row detection.
In the industrial production, in order to ensure catalysis activity, improve 2-Pyrrolidone potassium salts content, often take to increase hydrogen-oxygen
Change potassium inventory way realize, the increase of accessory substance when inevitably causing catalyst to manufacture, 2-Pyrrolidone and
Polymeric by-products during acetylene reaction increases, and yield is low, blocks reactor, frequently stops production.
Use alkali metal to react with 2-Pyrrolidone, prepare 2-Pyrrolidone sylvite catalyst, because the reaction time is short, reaction
Speed is fast, and side reaction is few, and catalysis activity is high, and yield is high, is a good selection.But a large amount of hydrogen can be produced at short notice
Gas, and release substantial amounts of heat, will cause the high safety requirements in commercial scale, in order to effectively carry out alkali-metal dispersion and
The removal of heat, the realization that industrial batch produces is deposited and is acquired a certain degree of difficulty.
Content of the invention
For the above-mentioned problems in the prior art, it is an object of the invention to design provides a kind of alkali metal 2-pyrroles
The technical scheme 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, controls the rising of temperature and the generating capacity of hydrogen, can the repetition of simple microreactor quantity
Increasing and just can realizing gratifying commercial production scale, its production cost is low, and course of reaction is safe and reliable.
The preparation method of the 2-Pyrrolidone solution of described a kind of alkali metal 2-Pyrrolidone salt, it is characterised in that include
Following steps：
1）By 2-Pyrrolidone feed containers, heater, filter, blender, microreactor, reactant liquor storage tank, alkali metal
Measuring tank and the displacement of connection system nitrogen, displacement to oxygen content is less than 0.5%；
2）Loading the 2-Pyrrolidone of q.s in 2-Pyrrolidone feed containers, in feed containers, the temperature of liquid controls
28 DEG C-35 DEG C, with the heated device of flow of 80-100ml/min, 2-Pyrrolidone is heated to 110-130 DEG C with pump, then passes through
Filter, blender, microreactor return 2-Pyrrolidone feed containers, 1.5-2.5 minute before throwing alkali metal, switch to reaction
In liquid storage tank so that 2-Pyrrolidone and alkali-metal reactant liquor are delivered in reactant liquor storage tank；
3）The alkali metal of q.s is entered in alkali metal measuring tank at the protection down of kerosene, the temperature of alkali metal amount pot liquid
Degree controls at 105-115 DEG C, and the nitrogen-sealed pressure of alkali metal measuring tank is set as 0.35-0.45MPa, then will be molten by pressure
The alkali metal melting extrudes feeding blender bottom alkali metal measuring tank and mixes laggard reactor reaction in a subtle way with 2-Pyrrolidone,
Alkali-metal inlet amount is 0.8-2.2 gram/min, and reacted liquid sends into reactant liquor storage tank after nitrogen displacement abjection hydrogen
In, obtaining the 2-Pyrrolidone solution of the alkali metal 2-Pyrrolidone salt of 0.1-10%, nitrogen-sealed preserves.
The preparation method of the 2-Pyrrolidone solution of described 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 described a kind of alkali metal 2-Pyrrolidone salt, it is characterised in that described
2-Pyrrolidone, its molecular structural formula is formula 1：
Have another name called：Pyrrolones, nitrogen penta cyclic ketones, butyrolactam.
The preparation method of the 2-Pyrrolidone solution of described a kind of alkali metal 2-Pyrrolidone salt, it is characterised in that described
Alkali metal 2-Pyrrolidone salt, its molecular structural formula is formula 2：
M:Sodium, potassium, Na-K alloy.
The preparation method of the 2-Pyrrolidone solution of described a kind of alkali metal 2-Pyrrolidone salt, it is characterised in that step
2）In：With the heated device of flow of 85-95ml/min, 2-Pyrrolidone is heated to 115-125 DEG C with pump, preferably with pump with 88-
2-Pyrrolidone is heated to 118-120 DEG C by the heated device of flow of 90ml/min.
The preparation method of the 2-Pyrrolidone solution of described a kind 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.
The preparation method of the 2-Pyrrolidone solution of described a kind of alkali metal 2-Pyrrolidone salt, it is characterised in that step
3）In：Alkali-metal inlet amount is 0.9-1.8/min, preferably 1.2-1.5 gram/min.
2-Pyrrolidone solution for preparing the application in vinyl pyrrolidone with acetylene reaction.
In reaction, produced hydrogen simply can be deviate from degasser.
The microreactor system of this paper is continuous system, participates in the amount of material of reaction and is gram or milliliter level scope, reaction
The channel width of device is typically at 1-10000 m, between preferably 10-1000 m, more preferably 50-150 m.Material is stainless steel, also
The materials such as glass, pottery, plastics can be selected.
Alkali metal uses microporous barrier to mix with the mixing of 2-Pyrrolidone, before material enters reactor, first
Be introduced into a microporous barrier blender, the aperture of microporous barrier typically at 1-1000 m, preferably 10-800 m, more preferably 10-100
Between m.Material is stainless steel, it is also possible to select the material such as pottery, plastics.
The temperature of reaction is to be determined by the melt temperature of alkali metal, 2-Pyrrolidone, the temperature of microreactor system
Alkali metal to be guaranteed, 2-Pyrrolidone have mobility smoothly, and ordinary circumstance reaction temperature less than 2-Pyrrolidone boiling point is
Good.Reaction temperature general control, at 65-240 DEG C, is preferably:80-200 DEG C, more preferably 100-150 DEG C.
Reaction heat is to be taken away by excessive 2-Pyrrolidone, and alkali metal inventory is big, and reactant liquor is from starting to be reacted to
Temperature rise at the end of reaction is just big, and the amplitude that general control reaction temperature rises is 1-120 DEG C, preferably 1-80 DEG C, more preferably
For 1-50 DEG C.Also can select to remove heat with heat exchanger.
The concentration of alkali metal 2-Pyrrolidone salt is to be realized by the proportional quantity of control alkali metal and 2-Pyrrolidone, instead
In should, 2-Pyrrolidone be excessive relative to alkali metal, excessive number can be according to the presence or absence precipitation situation of solution and reactant liquor
Temperature rises situation and determines.
Reaction pressure is according to factor determinations such as blender, reactor resistance, reactant liquor temperature rises.
Alkali metal is carried out in the case of not having mechanical agitation with the reaction of 2-Pyrrolidone, reason be microreactor and
The mixed effect of preposition micropore blender is enough.
The preparation method and its usage of the 2-Pyrrolidone solution of above-mentioned a kind of alkali metal 2-Pyrrolidone salt, preparation process
In without other solvent or auxiliary agent, it is not necessary to process the second solvent, it is not necessary to catalyst, it is not necessary to auxiliary agent carries out disperseing and mixing, slightly
It higher than the relatively low reaction temperature of alkali metal fusing point, extremely low side reaction, is simple, economical on a manufacturing scale and safety
's.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
2-Pyrrolidone container, heater, filter, blender, microreactor, reactant liquor storage tank and connection system nitrogen are put
Changing, displacement to oxygen content is less than 0.5%.
By the 2-Pyrrolidone of q.s（Fusing point be the boiling point under 24.6 DEG C, normal pressure be 245 DEG C, density 1.116（25/4
℃））Loading in feed containers, in feed containers, the temperature of liquid controls more than 28 DEG C, it is therefore an objective to keep at 2-Pyrrolidone
In liquid condition.With the heated device of flow of 90ml/min, 2-Pyrrolidone is heated to 120 DEG C with pump, then through filter, mixed
Clutch, microreactor return feed storage tank, are throwing metallic sodium first 2 minutes, are switching in reactant liquor storage tank so that 2-Pyrrolidone
Deliver in reactant liquor storage tank with the reactant liquor of sodium.
Replacing sodium measuring tank and sodium feeding line nitrogen, displacement to oxygen content is less than 0.5%.By the sodium of q.s（Fusing point
It is 97.82 DEG C, relative density (H2O)0.968）Protection down at kerosene enters in sodium measuring tank, the temperature of metering pot liquid
Control is more than 105 DEG C, it is therefore an objective to keep metallic sodium to be in molten condition.The nitrogen-sealed pressure of sodium measuring tank is set as
Melted metallic sodium, because melted sodium is than kerosene weight, can be extruded feeding by pressure mixed bottom sodium measuring tank by 0.4MPa
Clutch mixes laggard reactor reaction in a subtle way with 2-Pyrrolidone, and the inlet amount of metallic sodium is 1.0 grams/min, reacted liquid
Sending in reactant liquor storage tank after nitrogen displacement abjection hydrogen, the 2-Pyrrolidone obtaining about 4.6%2-pyrrolidones sodium salt is molten
Liquid, nitrogen-sealed preserves.
Embodiment 2
2-Pyrrolidone feeding system, with embodiment 1, replaces sodium with potassio.
Replacing potassium measuring tank and potassium feeding line nitrogen, displacement to oxygen content is less than 0.5%.By the potassium of q.s（Fusing point
63.25 DEG C, density 0.86g/cm）Protection down at kerosene enters in potassium measuring tank, and the temperature of metering pot liquid controls 70
More than DEG C, it is therefore an objective to keep metallic potassium to be in molten condition.The nitrogen-sealed pressure of potassium measuring tank is set as 0.4MPa, because melting
Potassium slightly heavier than kerosene, by pressure, melted metallic potassium can be extruded bottom potassium measuring tank feeding blender and 2-pyrroles
The laggard reactor reaction in a subtle way of alkanone mixing, the inlet amount of metallic potassium is 0.5 gram/min, and reacted liquid is de-through nitrogen displacement
Sending in reactant liquor storage tank after going out hydrogen, obtaining the 2-Pyrrolidone solution of about 1.6%2-pyrrolidones sylvite, nitrogen-sealed is protected
Deposit.
Claims (10)
1. the preparation method of the 2-Pyrrolidone solution of an alkali metal 2-Pyrrolidone salt, it is characterised in that include following step
Suddenly：
1）By 2-Pyrrolidone feed containers, heater, filter, blender, microreactor, reactant liquor storage tank, alkali metal
Measuring tank and the displacement of connection system nitrogen, displacement to oxygen content is less than 0.5%；
2）Loading the 2-Pyrrolidone of q.s in 2-Pyrrolidone feed containers, in feed containers, the temperature of liquid controls
28 DEG C-35 DEG C, with the heated device of flow of 80-100ml/min, 2-Pyrrolidone is heated to 110-130 DEG C with pump, then passes through
Filter, blender, microreactor return 2-Pyrrolidone feed containers, 1.5-2.5 minute before throwing alkali metal, switch to reaction
In liquid storage tank so that 2-Pyrrolidone and alkali-metal reactant liquor are delivered in reactant liquor storage tank；
3）The alkali metal of q.s is entered in alkali metal measuring tank at the protection down of kerosene, the temperature of alkali metal amount pot liquid
Degree controls at 105-115 DEG C, and the nitrogen-sealed pressure of alkali metal measuring tank is set as 0.35-0.45MPa, then will be molten by pressure
The alkali metal melting extrudes feeding blender bottom alkali metal measuring tank and mixes laggard reactor reaction in a subtle way with 2-Pyrrolidone,
Alkali-metal inlet amount is 0.8-2.2 gram/min, and reacted liquid sends into reactant liquor storage tank after nitrogen displacement abjection hydrogen
In, obtaining the 2-Pyrrolidone solution of the alkali metal 2-Pyrrolidone salt of 0.1-10%, nitrogen-sealed preserves.
2. the preparation method of the 2-Pyrrolidone solution of a kind of alkali metal 2-Pyrrolidone salt as claimed in claim 1, it is special
Levy and be that described alkali metal is sodium, potassium or Na-K alloy.
3. the preparation method of the 2-Pyrrolidone solution of a kind of alkali metal 2-Pyrrolidone salt as claimed in claim 1, it is special
Levying and being described 2-Pyrrolidone, its molecular structural formula is formula 1：
Have another name called：Pyrrolones, nitrogen penta cyclic ketones, butyrolactam.
4. the preparation method of the 2-Pyrrolidone solution of a kind of alkali metal 2-Pyrrolidone salt as claimed in claim 1, it is special
Levying and being described alkali metal 2-Pyrrolidone salt, its molecular structural formula is formula 2：
M:Sodium, potassium, Na-K alloy.
5. the preparation method of the 2-Pyrrolidone solution of a kind of alkali metal 2-Pyrrolidone salt as claimed in claim 1, it is special
Levy and be step 2）In：With the heated device of flow of 85-95ml/min, 2-Pyrrolidone is heated to 115-125 DEG C with pump, excellent
Select pump, with the heated device of flow of 88-90ml/min, 2-Pyrrolidone is heated to 118-120 DEG C.
6. the preparation method of the 2-Pyrrolidone solution of a kind of alkali metal 2-Pyrrolidone salt as claimed in claim 1, it is special
Levy and be step 3）In：The nitrogen-sealed pressure of alkali metal measuring tank is set as 0.38-0.44MPa, preferably 0.40-0.42MPa.
7. the preparation method of the 2-Pyrrolidone solution of a kind of alkali metal 2-Pyrrolidone salt as claimed in claim 1, it is special
Levy and be step 3）In：Alkali-metal inlet amount is 0.9-1.8/min, preferably 1.2-1.5 gram/min.
8. the preparation method of the 2-Pyrrolidone solution of a kind of alkali metal 2-Pyrrolidone salt as claimed in claim 1, it is special
Levying and being that described microreactor is that stainless steel, glass, pottery or plastics are made, the channel width of microreactor is 1-10000
M, preferably 10-1000 m, between more preferably 50-150 m；Blender is the microporous barrier mixing that stainless steel, pottery or plastics are made
Device, the aperture of microporous barrier is 1-1000 m, preferably 10-800 m, more preferably 10-100 m.
9. the preparation method of the 2-Pyrrolidone solution of a kind of alkali metal 2-Pyrrolidone salt as claimed in claim 1, it is special
Levy and be that reaction temperature general control, at 65-240 DEG C, is preferably:80-200 DEG C, more preferably 100-150 DEG C；Control reaction
The amplitude that temperature rises is 1-120 DEG C, preferably 1-80 DEG C, more preferably 1-50 DEG C.
10. the 2-Pyrrolidone solution preparing such as claim 1 is being used for preparing in vinyl pyrrolidone with acetylene reaction
Application.
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| Application Number | Priority Date | Filing Date | Title |
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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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| CN111039843A (en) * | 2019-12-19 | 2020-04-21 | 清华大学 | Synthetic process, synthetic system and application of N-vinylpyrrolidone |
| CN112574088A (en) * | 2019-09-30 | 2021-03-30 | 中国石油化工股份有限公司 | Method for synthesizing N-vinyl pyrrolidone |
| CN114425239A (en) * | 2020-10-15 | 2022-05-03 | 中国石油化工股份有限公司 | Micro-channel permeation gasification device and method for synthesizing pyrrolidone alkali metal salt |
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| CN111039843A (en) * | 2019-12-19 | 2020-04-21 | 清华大学 | Synthetic process, synthetic system and application of N-vinylpyrrolidone |
| CN114425239A (en) * | 2020-10-15 | 2022-05-03 | 中国石油化工股份有限公司 | Micro-channel 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 |