CN110156632A - A kind of separating and extracting process of malononitrile - Google Patents
A kind of separating and extracting process of malononitrile Download PDFInfo
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- CN110156632A CN110156632A CN201910454545.2A CN201910454545A CN110156632A CN 110156632 A CN110156632 A CN 110156632A CN 201910454545 A CN201910454545 A CN 201910454545A CN 110156632 A CN110156632 A CN 110156632A
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- dichloroethanes
- malononitrile
- water
- solid
- liquid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/20—Preparation of carboxylic acid nitriles by dehydration of carboxylic acid amides
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/32—Separation; Purification; Stabilisation; Use of additives
- C07C253/34—Separation; Purification
Abstract
The invention discloses a kind of separating and extracting process of malononitrile, the following steps are included: using phosphorus oxychloride, cyanoacetamide and dichloroethanes as raw material, addition adsorbent progress elimination reaction, be eliminated solid-liquid mixed liquor, which mainly has dichloroethanes, malononitrile, the calcium chloride solid particle for adsorbing metaphosphoric acid etc.；It adds water and stirs, heats up in dissolution reaction kettle, be added into dissolution reaction kettle and eliminate solid-liquid mixed liquor.Solid-liquid mixed liquor water will be eliminated and dissolve layering, organic layer normal pressure precipitation, vacuum distillation, rectification under vacuum obtain malononitrile fine work.The present invention has simple process easy to operate, and " separation of solid and liquid " is reformed and eliminates opening suction filtration tank using obturator for " Liquid liquid Separation ", prevents the uncontrollable discharge of volatile organic matter, solve environmental issue, it is ensured that safety in production；It is layered using dissolution, worker is not necessarily to slag tap, then throws solid material, and liquid material is through pipeline, the advantages of alleviating the labor intensity of worker, reduce harm to the human body.
Description
Technical field
The invention belongs to chemical production fields, are related to a kind of separating and extracting process of simple and safe malononitrile.
Background technique
At present during preparing malononitrile, terminate in elimination reaction, be eliminated solid-liquid mixed liquor, the elimination solid-liquid
Mixed liquor mainly has dichloroethanes, malononitrile, the calcium chloride solid particle for adsorbing metaphosphoric acid etc..Prior art is using " solid-liquid point
From ", it is filtered by vacuum using backward chemical production equipment " open suction filtration tank ", filtrate goes air-distillation, and recycling design subtracts
Pressure distills to obtain malononitrile crude product, then rectification under vacuum obtains malononitrile finished product；Filter residue is manually dug out from " in open suction filtration tank ", packaging,
Fork truck is sent to phosphoric acid workshop, prepares phosphoric acid byproduct aqueous solution.When blowing is slagged tap, the volatile organic matters such as dichloroethanes, hydrogen chloride,
Uncontrollable discharge.Dichloroethanes is harmful to environment, and the substance is extremely strong to Atmospheric Ozone Layer Depletion power.This production method is to vehicle
Between production bring very big safety and environmental protection hidden danger.Several tons of filter residues need to be dug out closed packet from " open suction filtration tank " daily by worker
Dress is sent to phosphoric acid workshop, then through manually in several tons of filter residue investment reaction kettles, preparing phosphate aqueous solution.Worker operation environment is disliked
It is bad, large labor intensity.Dichloroethanes high poison is suspecious carcinogen, has irritation, endanger the health of worker.
Summary of the invention
It is an object of that present invention to provide a kind of simple process is easy to operate, " separation of solid and liquid " is reformed as " Liquid liquid Separation ", it will
Solid-liquid mixed liquor is eliminated, first dissolves and is layered again, water layer directly prepares the separating and extracting process of the malononitrile of phosphate aqueous solution.
The technical solution adopted by the invention is as follows: a kind of separating and extracting process of malononitrile, it is characterised in that: including following
Step:
A, elimination reaction: using phosphorus oxychloride, cyanoacetamide and dichloroethanes as main material, adsorbent calcium chloride is added and disappears
Except reaction, above-mentioned raw materials are put into elimination reaction kettle, is stirred, is to slowly warm up to 85-90 DEG C, and at 85-90 DEG C, protected
Temperature reaction 4-10 hours, the cyanoacetamide, phosphorus oxychloride, dichloroethanes, calcium chloride usage ratio be by mass cyanogen
Yl acetamide: phosphorus oxychloride: dichloroethanes: calcium chloride=1:1:4:0.12；
B, eliminating terminates, and will eliminate feed liquid and is cooled to 30-40 DEG C, be eliminated solid-liquid mixed liquor, for use；
C, dissolution layering: first add water in dissolution reaction kettle, open stirring, control 20-40 DEG C of water temperature, then will obtain in step b
Solid-liquid mixed liquor is eliminated to be added to the water；The cyanoacetamide, phosphorus oxychloride, dichloroethanes, calcium chloride, water usage ratio press
Quality is calculated as cyanoacetamide: phosphorus oxychloride: dichloroethanes: calcium chloride: water=1:1:4:0.12:0.6 ~ 1.5；
D, frozen cooling is used simultaneously, the material temperature for controlling the dissolution reaction kettle is 20-80 DEG C, it eliminates solid-liquid mixed liquor and adds, after
Continuous control 20-80 DEG C insulation reaction 15-30 minutes, until solid material dissolved clarification；
E, 10-15 minutes are stood, separates lower aqueous layer, collect upper organic layer, water layer is extracted 2-3 times with dichloroethanes, is stood
10-15 minutes, lower aqueous layer is separated, upper organic layer is collected, merges all organic layers, for use, the water layer is that phosphoric acid is water-soluble
Liquid；
F, normal pressure precipitation, vacuum distillation: by the heating of organic layer normal pressure, precipitation to 105 DEG C, then recycling design dichloroethanes subtracts
Pressure distillation, obtains malononitrile crude product；
G, rectification under vacuum: again by malononitrile crude product, heating melts, and carries out rectifying, obtains malononitrile fine work.
A further improvement of the present invention is that: in the step c, water temperature is controlled at 25-35 DEG C.
A further improvement of the present invention is that: the material temperature that reaction kettle is dissolved in the Step d is 25-50 DEG C.
A further improvement of the present invention is that: the cyanoacetamide, phosphorus oxychloride, the use of dichloroethanes, calcium chloride, water
Amount ratio is cyanoacetamide by mass: phosphorus oxychloride: dichloroethanes: calcium chloride: water=1:1:4:0.12:0.8-1.2.
Compared with the prior art, the present invention has the following advantages:
Simple process is easy to operate, and " separation of solid and liquid " is reformed as " Liquid liquid Separation ", will eliminate solid-liquid mixed liquor, and first dissolve and divide again
Layer, water layer are not necessarily to precipitation, directly preparation phosphate aqueous solution；It is effective to control by the control of feed way, water and solution temperature
The hydrolysis of malononitrile processed in acid condition, quality and yield meet the requirement of mass production, optimize technique；Using closed dress
It sets, eliminates backward chemical production equipment " open suction filtration tank ", be not necessarily to vacuum filter, layering, pipe are dissolved in dissolution reaction kettle
Road conveying, stratification temperature is low, prevents volatile organic matter uncontrollable discharge, solves environmental issue, it is ensured that safety in production；Using molten
Solution layering, worker throw solid slag without slagging tap, no longer needing to, and the labour that liquid material can alleviate worker through pipeline is strong
Degree reduces the body harm to human body.
Specific embodiment
Below to be described in further detail by preferred embodiment to present invention process, but protection scope of the present invention
It is not limited thereto.
Embodiment 1
Into elimination reaction kettle, cyanoacetamide 100kg, dichloroethanes 400kg, calcium chloride 12kg and phosphorus oxychloride 100kg are thrown,
Stirring is opened, is to slowly warm up to 85 DEG C, and at 85 DEG C, insulation reaction 10 hours, heat preservation terminated, and was cooled to 30 DEG C, stand-by (letter
Claim: eliminating solid-liquid mixed liquor)；
In dissolution reaction kettle, water 60kg is first added, opens stirring, controls 20 DEG C of water temperature, then into the dissolution reaction kettle, is added
Above-mentioned elimination solid-liquid mixed liquor, while with frozen cooling, the material temperature for controlling the dissolution reaction kettle is 20-25 DEG C, and it is mixed to eliminate solid-liquid
Liquid is closed to add, continue control 20-25 DEG C insulation reaction 30 minutes, until solid material dissolved clarification, stand 10-15 minutes, separate down
Layer water layer, collects upper organic layer；Water layer is extracted 2-3 times with dichloroethanes, is stood 10-15 minutes, is separated lower aqueous layer, is collected
Upper organic layer merges all organic layers, for use；Water layer directly prepares phosphate aqueous solution, sells as byproduct；
Organic layer, to 105 DEG C, then recycling design dichloroethanes is evaporated under reduced pressure, obtain malononitrile crude product for normal pressure heating, precipitation.Again
By malononitrile crude product, heating melts, and carries out rectification under vacuum, obtains malononitrile fine work 68kg, content 99.6%.
Embodiment 2
Into elimination reaction kettle, cyanoacetamide 100kg, dichloroethanes 400kg, calcium chloride 12kg and phosphorus oxychloride 100kg are thrown,
Stirring is opened, is to slowly warm up to 88 DEG C, and at 88 DEG C, insulation reaction 8 hours.Heat preservation terminates, and is cooled to 33 DEG C, stand-by (letter
Claim: eliminating solid-liquid mixed liquor)；
In dissolution reaction kettle, water 80kg is first added, opens stirring, controls 25 DEG C of water temperature, then into the dissolution reaction kettle, is added
Above-mentioned elimination solid-liquid mixed liquor, while with frozen cooling, the material temperature for controlling the dissolution reaction kettle is 27-30 DEG C, and it is mixed to eliminate solid-liquid
Liquid is closed to add, continue control 27-30 DEG C insulation reaction 30 minutes, until solid material dissolved clarification, stand 10-15 minutes, separate down
Layer water layer, collects upper organic layer；Water layer is extracted 2-3 times with dichloroethanes, is stood 10-15 minutes, is separated lower aqueous layer, is collected
Upper organic layer；Merge all organic layers, for use；Water layer directly prepares phosphate aqueous solution, sells as byproduct；
Organic layer, to 105 DEG C, then recycling design dichloroethanes is evaporated under reduced pressure, obtain malononitrile crude product for normal pressure heating, precipitation.Again
By malononitrile crude product, heating melts, and carries out rectification under vacuum, obtains malononitrile fine work 67.9kg, content 99.7%.
Embodiment 3
Into elimination reaction kettle, cyanoacetamide 100kg, dichloroethanes 400kg, calcium chloride 12kg and phosphorus oxychloride 100kg are thrown,
Stirring is opened, is to slowly warm up to 87 DEG C, and at 87 DEG C, insulation reaction 9 hours, heat preservation terminated, and was cooled to 35 DEG C, stand-by (letter
Claim: eliminating solid-liquid mixed liquor)；
In dissolution reaction kettle, water 100kg is first added, opens stirring, controls 37 DEG C of water temperature, then into the dissolution reaction kettle, add
Enter above-mentioned elimination solid-liquid mixed liquor, while with frozen cooling, the material temperature for controlling the dissolution reaction kettle is 41-45 DEG C, eliminates solid-liquid
Mixed liquor adds, continue control 41-45 DEG C insulation reaction 15-30 minute, until solid material dissolved clarification, stand 10-15 minutes, divide
Lower aqueous layer out collects upper organic layer, and water layer is extracted 2-3 times with dichloroethanes, stands 10-15 minutes, separates lower aqueous layer,
Upper organic layer is collected, merges all organic layers, for use；Water layer is phosphate aqueous solution, is sold as byproduct；
Organic layer, normal pressure heating, precipitation are to 105 DEG C, recycling design dichloroethanes.Then it is evaporated under reduced pressure, obtains malononitrile crude product.Again
By malononitrile crude product, heating melts, and carries out rectification under vacuum, obtains malononitrile fine work 67.6kg, content 99.9%.
Embodiment 4
Into elimination reaction bottle kettle, cyanoacetamide 100kg, dichloroethanes 400kg, calcium chloride 12kg and phosphorus oxychloride are thrown
100kg opens stirring, is to slowly warm up to 89 DEG C, and at 89 DEG C, and insulation reaction 7 hours.Heat preservation terminates, and is cooled to 37 DEG C, to
With (referred to as: eliminating solid-liquid mixed liquor).
In dissolution reaction kettle, it is first added 120kg grams, opens stirring, controls 38 DEG C of water temperature, then to the dissolution reaction kettle
In, it is added above-mentioned elimination solid-liquid mixed liquor, while with frozen cooling, the material temperature for controlling the dissolution reaction kettle is 46-50 DEG C, is eliminated
Solid-liquid mixed liquor adds, continue control 46-50 DEG C insulation reaction 15-30 minute, until solid material dissolved clarification, stand 10-15 and divide
Clock separates lower aqueous layer, collects upper organic layer, and water layer is extracted 2-3 times with dichloroethanes, stands 10-15 minutes, separates lower layer
Water layer collects upper organic layer, merges all organic layers, for use；Water layer directly prepares phosphate aqueous solution, goes out as byproduct
It sells；
Organic layer, to 105 DEG C, then recycling design dichloroethanes is evaporated under reduced pressure, obtain malononitrile crude product for normal pressure heating, precipitation.Again
By malononitrile crude product, heating melts, and carries out rectification under vacuum, obtains malononitrile fine work 66.9kg, content >=99.6%.
Embodiment 5
Into elimination reaction bottle kettle, cyanoacetamide 100kg, dichloroethanes 400kg, calcium chloride 12kg and phosphorus oxychloride are thrown
100kg opens stirring, is to slowly warm up to 90 DEG C, and at 90 DEG C, and insulation reaction 4 hours.Heat preservation terminates, and is cooled to 36 DEG C, to
With (referred to as: eliminating solid-liquid mixed liquor)；
In dissolution reaction kettle, water 130kg is first added, opens stirring, controls 39 DEG C of water temperature, then into the dissolution reaction kettle, add
Enter above-mentioned elimination solid-liquid mixed liquor, while with frozen cooling, the material temperature for controlling the dissolution reaction kettle is 51-55 DEG C, eliminates solid-liquid
Mixed liquor adds, continue control 51-55 DEG C insulation reaction 15-30 minute, until solid material dissolved clarification, stand 10-15 minutes, divide
Lower aqueous layer out collects upper organic layer, and water layer is extracted 2-3 times with dichloroethanes, stands 10-15 minutes, separates lower aqueous layer,
Upper organic layer is collected, merges all organic layers, for use；Water layer directly prepares phosphate aqueous solution, sells as byproduct；
Organic layer, to 105 DEG C, then recycling design dichloroethanes is evaporated under reduced pressure, obtain malononitrile crude product for normal pressure heating, precipitation.Again
By malononitrile crude product, heating melts, and carries out rectification under vacuum, obtains 67.5 grams of malononitrile fine work, content 99%.
Embodiment 6
Into elimination reaction bottle, cyanoacetamide 100kg, dichloroethanes 400kg, calcium chloride 12kg and phosphorus oxychloride 100kg are thrown,
Stirring is opened, is to slowly warm up to 86 DEG C, and at 86 DEG C, insulation reaction 7 hours.Heat preservation terminates, and is cooled to 38 DEG C, stand-by (letter
Claim: eliminating solid-liquid mixed liquor)；
In dissolution reaction kettle, water 150kg is first added, opens stirring, controls 40 DEG C of water temperature, then into the dissolution reaction kettle, add
Enter above-mentioned elimination solid-liquid mixed liquor, while with frozen cooling, the material temperature for controlling the dissolution reaction kettle is 56-60 DEG C, eliminates solid-liquid
Mixed liquor adds, continue control 56-60 DEG C insulation reaction 15-30 minute, until solid material dissolved clarification, stand 10-15 minutes, divide
Lower aqueous layer out collects upper organic layer.Water layer is extracted 2-3 times with dichloroethanes, is stood 10-15 minutes, is separated lower aqueous layer,
Collect upper organic layer.Merge all organic layers, for use；Water layer directly prepares phosphate aqueous solution, sells as byproduct；
Organic layer, to 105 DEG C, then recycling design dichloroethanes is evaporated under reduced pressure, obtain malononitrile crude product for normal pressure heating, precipitation.Again
By malononitrile crude product, heating melts, and carries out rectification under vacuum, obtains 66.4 grams of malononitrile fine work, content 99.6%.
Embodiment 7
Into elimination reaction bottle, cyanoacetamide 100kg, dichloroethanes 400kg, calcium chloride 12kg and phosphorus oxychloride 100kg are thrown,
Stirring is opened, is to slowly warm up to 86.5 DEG C, and at 86.5 DEG C, insulation reaction 5 hours.Heat preservation terminates, and is cooled to 39 DEG C, for use
(referred to as: eliminating solid-liquid mixed liquor)；
In dissolution reaction kettle, water 90kg is first added, opens stirring, controls 22 DEG C of water temperature, then into the dissolution reaction kettle, is added
Above-mentioned elimination solid-liquid mixed liquor, while with frozen cooling, the material temperature for controlling the dissolution reaction kettle is 77-80 DEG C, and it is mixed to eliminate solid-liquid
Liquid is closed to add, continue control 77-80 DEG C insulation reaction 15-30 minute, until solid material dissolved clarification, standing 10-15 minutes is separated
Lower aqueous layer collects upper organic layer；Water layer is extracted 2-3 times with dichloroethanes, is stood 10-15 minutes, is separated lower aqueous layer, is received
Collect upper organic layer；Merge all organic layers, for use；Water layer directly prepares phosphate aqueous solution, sells as byproduct；
Organic layer, to 105 DEG C, then recycling design dichloroethanes is evaporated under reduced pressure, obtain malononitrile crude product for normal pressure heating, precipitation.Again
By malononitrile crude product, heating melts, and carries out rectification under vacuum, obtains 69.4 grams of malononitrile fine work, content 99.8%.
Embodiment 8
Into elimination reaction bottle, cyanoacetamide 100kg, dichloroethanes 400kg, calcium chloride 12kg and phosphorus oxychloride 100kg are thrown,
Stirring is opened, is to slowly warm up to 88.5 DEG C, and at 88.5 DEG C, insulation reaction 5 hours.Heat preservation terminates, and is cooled to 39 DEG C, for use
(referred to as: eliminating solid-liquid mixed liquor)；
In dissolution reaction kettle, water 140kg is first added, opens stirring, controls 28 DEG C of water temperature, then into the dissolution reaction kettle, add
Enter above-mentioned elimination solid-liquid mixed liquor, while with frozen cooling, the material temperature for controlling the dissolution reaction kettle is 66-70 DEG C, eliminates solid-liquid
Mixed liquor adds, continue control 66-70 DEG C insulation reaction 15-30 minute, until solid material dissolved clarification, stand 10-15 minutes, divide
Lower aqueous layer out collects upper organic layer.Water layer is extracted 2-3 times with dichloroethanes, is stood 10-15 minutes, is separated lower aqueous layer,
Collect upper organic layer.Merge all organic layers, for use；Water layer directly prepares phosphate aqueous solution, sells as byproduct；
Organic layer, to 105 DEG C, then recycling design dichloroethanes is evaporated under reduced pressure, obtain malononitrile crude product for normal pressure heating, precipitation.Again
By malononitrile crude product, heating melts, and carries out rectification under vacuum, obtains 68.6 grams of malononitrile fine work, content 99.8%.
Present invention process is simple to operation, and " separation of solid and liquid " is reformed as " Liquid liquid Separation ", will eliminate solid-liquid mixed liquor, first
Dissolution is layered again, and water layer is not necessarily to precipitation, directly preparation phosphate aqueous solution；By the control of feed way, water and solution temperature,
The hydrolysis of effective control malononitrile in acid condition, quality and yield meet the requirement of mass production, optimize technique；It adopts
With obturator, backward chemical production equipment " open suction filtration tank " is eliminated, is not necessarily to vacuum filter, is dissolved in dissolution reaction kettle
Layering, pipeline, stratification temperature is low, prevents volatile organic matter uncontrollable discharge, solves environmental issue, it is ensured that safety is raw
It produces；It is layered using dissolution, worker throws solid slag without slagging tap, no longer needing to, and liquid material alleviates worker through pipeline
Labor intensity, reduce to the body harm of human body.
The another statement of applicant, implementation method and apparatus structure of the invention that the present invention is explained by the above embodiments,
But the invention is not limited to above embodiment, that is, do not mean that the present invention must rely on the above method and structure could be real
It applies.It should be clear to those skilled in the art, any improvement in the present invention, to implementation method selected by the present invention etc.
Effect replacement and addition, the selection of concrete mode of step etc., all fall within protection scope of the present invention and scope of disclosure.This
Invention is not limited to the above embodiment, all that all of the object of the invention are realized using structure similar with the present invention and its method
Mode, it is within the scope of the present invention.
Claims (4)
1. a kind of separating and extracting process of malononitrile, it is characterised in that: the following steps are included:
A, elimination reaction: using phosphorus oxychloride, cyanoacetamide and dichloroethanes as main material, adsorbent calcium chloride is added and disappears
Except reaction, above-mentioned raw materials are put into elimination reaction kettle, is stirred, is to slowly warm up to 85-90 DEG C, and at 85-90 DEG C, protected
Temperature reaction 4-10 hours, the cyanoacetamide, phosphorus oxychloride, dichloroethanes, calcium chloride usage ratio be by mass cyanogen
Yl acetamide: phosphorus oxychloride: dichloroethanes: calcium chloride=1:1:4:0.12；
B, eliminating terminates, and will eliminate feed liquid and is cooled to 30-40 DEG C, be eliminated solid-liquid mixed liquor, for use；
C, dissolution layering: first add water in dissolution reaction kettle, open stirring, control 20-40 DEG C of water temperature, then will obtain in step b
Solid-liquid mixed liquor is eliminated to be added to the water；The cyanoacetamide, phosphorus oxychloride, dichloroethanes, calcium chloride, water usage ratio press
Quality is calculated as cyanoacetamide: phosphorus oxychloride: dichloroethanes: calcium chloride: water=1:1:4:0.12:0.6 ~ 1.5；
D, frozen cooling is used simultaneously, the material temperature for controlling the dissolution reaction kettle is 20-80 DEG C, it eliminates solid-liquid mixed liquor and adds, after
Continuous control 20-80 DEG C insulation reaction 15-30 minutes, until solid material dissolved clarification；
E, 10-15 minutes are stood, separates lower aqueous layer, collect upper organic layer, water layer is extracted 2-3 times with dichloroethanes, is stood
10-15 minutes, lower aqueous layer is separated, upper organic layer is collected, merges all organic layers, for use, the water layer is that phosphoric acid is water-soluble
Liquid；
F, normal pressure precipitation, vacuum distillation: by the heating of organic layer normal pressure, precipitation to 105 DEG C, then recycling design dichloroethanes subtracts
Pressure distillation, obtains malononitrile crude product；
G, rectification under vacuum: again by malononitrile crude product, heating melts, and carries out rectifying, obtains malononitrile fine work.
2. a kind of separating and extracting process of malononitrile according to claim 1, it is characterised in that: in the step c, control
Water temperature is at 25-35 DEG C.
3. a kind of separating and extracting process of malononitrile according to claim 1, it is characterised in that: dissolved in the Step d
The material temperature of reaction kettle is 25-50 DEG C.
4. a kind of separating and extracting process of malononitrile according to claim 1, it is characterised in that: the cyanoacetamide,
Phosphorus oxychloride, dichloroethanes, calcium chloride, water usage ratio be by mass cyanoacetamide: phosphorus oxychloride: dichloroethanes:
Calcium chloride: water=1:1:4:0.12:0.8-1.2.
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Cited By (1)
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| CN112679385A (en) * | 2020-12-31 | 2021-04-20 | 河北诚信集团有限公司 | Purification method of malononitrile |
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Application publication date: 20190823 |