CN208883750U - A kind of serialization prepare glycine around pipe reaction device - Google Patents

A kind of serialization prepare glycine around pipe reaction device Download PDF

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Publication number
CN208883750U
CN208883750U CN201821604809.5U CN201821604809U CN208883750U CN 208883750 U CN208883750 U CN 208883750U CN 201821604809 U CN201821604809 U CN 201821604809U CN 208883750 U CN208883750 U CN 208883750U
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China
Prior art keywords
unit
around
reaction device
gas
pipe reaction
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Expired - Fee Related
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CN201821604809.5U
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Chinese (zh)
Inventor
杨仁俊
龚文照
张伟
赫瑞元
赵广
李鑫
韩萌
毋楠
袁秋华
冯志武
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Yangquan Coal Industry Group Co Ltd
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Yangquan Coal Industry Group Co Ltd
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Abstract

The utility model disclose a kind of serialization prepare glycine around pipe reaction device, comprising: the preheating unit for being heated to raw material;Connect with the preheating unit around tube reaction unit, be used to occur synthesis and hydrolysis;With the gas-liquid separation unit being connect around tube reaction unit;With the sequentially connected flash evaporation unit of the gas-liquid separation unit and crystalline element.Pass through device provided by the utility model, hydroxyacetonitrile and ammonia source ammonia source, carbon source, water etc. first pass through after above-mentioned pre-heating system preheated, again through around tube reaction unit successively carried out synthesis and hydrolysis, then distilled, crystallized by gas-liquid separation unit, flash evaporation unit and crystalline element, being separated, dry after obtain high-purity glycine.

Description

A kind of serialization prepare glycine around pipe reaction device
Technical field
The utility model relates to chemical machinery, more particularly to it is a kind of for hydroxyacetonitrile serialization prepare glycine around Pipe reaction device.
Background technique
Glycine is also known as amion acetic acid, chemical formula C2H5NO2, it is a kind of structure amino acid the simplest, is widely applied In fields such as pesticide, food, feed, medicine, organic syntheses.China is maximum glycine production in the world and consumes state, sweet Propylhomoserin market scale is more than 350,000 tons.Currently, the Industrialized processing technique of glycine mainly has Chloroacetic Aminolysis, improved Strecker method (applying special rake method) and direct Hydantion method (direct glycolylurea method), in addition, research report is de- there are also being catalyzed Hydroxide method, biological synthesis process and Radiation Synthesis Method etc..Wherein the first two kind technique is by external (Cha Temu company, the France in the U.S. The West Asia Si Pa company, Japan organic synthesis drug company etc.) monopolization, product towards feed, food, medicine, daily use chemicals and The high-end fields such as fine chemistry industry.It is chloroactic acid method that the country, which prepares glycine prevailing technology, at present, and environmental pollution is serious, and market is competing Fierceness is striven, it is on the verge of being replaced.
There is some disadvantages for several glycine production methods in the prior art.(1) chloroactic acid method: chloroacetic acid ammonolysis process Method is, using methenamine as catalyst, to produce glycine using monoxone and ammonium hydroxide as raw material, is the skill that current China generallys use Art.This process industry time is more early, simple process and not high to equipment requirement, and Technical comparing is mature, and raw material is easy to get, and reacts item Part is mild, but synthesis cost is high, and environmental pollution is serious, and product influences product quality because containing chlorine root and free ammonia, belongs to urgency The backwardness technique that need to be eliminated.(2) traditional special rake method of applying is reacted using formaldehyde, Cymag, ammonium chloride as raw material, is deposited in sulfuric acid In lower alcoholysis, then hydrolyzable generates barium sulfate and glycine together with barium hydroxide.The technique is easy to refine, at low cost, Suitable for large-scale production, but equipment investment is big, and route is longer, and desalination is more complex after reaction, and operating condition is harsher.With chloroethene The shortcomings that sour ammonolysis process equally exists high production cost and environmental pollution is serious.(3) improved to apply special rake method: to improve sweet ammonia Sour quality reduces production cost and reduces environmental pollution, and foreign countries develop the improvement that Cymag or potassium cyanide are substituted with hydrogen cyanide Apply special rake method, react using hydrogen cyanide, formaldehyde, ammonia and carbon dioxide as raw material, reaction solution carries out in tubular reactor.? Glycine is precipitated under low temperature, Recycling Mother Solution uses, and by changing the concentration of by-product in reaction system, makes balance to target product Direction is mobile, to achieve the purpose that improve reaction yield.But the raw material hydrogen cyanide severe toxicity, volatile, Wu Fachang of this method Distance transport, to constrain its popularization and application.(4) direct glycolylurea method: hydroxyacetonitrile is the addition product of hydrogen cyanide and formaldehyde, Its stability is significantly improved compared with hydrogen cyanide and its aqueous solution.Using hydroxyacetonitrile as main material and ammonia source, carbon source (ammonium hydroxide and dioxy Change carbon or ammonium hydrogen carbonate), reaction synthesis glycolylurea under the conditions of good stirring, certain temperature, later in certain temperature, pressure condition Under so that glycolylurea is hydrolyzed to obtain glycine.Direct glycolylurea method is a kind of method of very promising industrially prepared glycine, but current work Batch tank production is only realized in industry, not yet realizes industrial continuous, chemical equation is as follows:
The characteristics of technique is that atom utilization is high, product quality is high, clean and environmental protection, great application prospect.But current work Batch tank production is only realized in industry, there are air-teturning mixed phenomenons using tank reactor, and the reaction time is longer, not yet realize industry Serialization.Therefore, it is necessary to a kind of devices of continuous production glycine.
Utility model content
In order to solve the above-mentioned technical problem, the utility model, which provides, a kind of prepares glycine for hydroxyacetonitrile serialization Around pipe reaction device characterized by comprising
Preheating unit for being heated to raw material;
Connect with the preheating unit around tube reaction unit, be used to occur synthesis and hydrolysis;
With the gas-liquid separation unit being connect around tube reaction unit;
The flash evaporation unit being connect with the gas-liquid separation unit;
The crystalline element being connect with the flash evaporation unit.
Preferably, the preheating unit includes sequentially connected metering pump, preheating and static mixer.
Preferably, it is described around tube reaction unit include sequentially connected first around tubular reactor, second around pipe reaction Device and third are around tubular reactor.
Preferably, described second, exit is provided with the decompression for controlling reaction pressure behind tubular reactor Valve.
Preferably, the gas-liquid separation unit includes gas-liquid separator.
Preferably, the top of the gas-liquid separator is equipped with the first gaseous phase outlet communicated with the entrance of the metering pump.
Preferably, the second gaseous phase outlet being connected with the metering pump intake is provided at the top of the flash evaporation unit.
Preferably, the crystalline element includes the first crystallization kettle and the second crystallization kettle being sequentially connected in series.
Preferably, the top of first crystallization kettle is equipped with and first mother liquid recycle being connected to around pipe reaction unit Mouthful, the top of second crystallization kettle is equipped with the second mother liquid recycle mouth communicated with the flash evaporation unit.
For background technique, in the utility model around pipe reaction device by preheating unit, around tube reaction unit, Gas-liquid separation unit, flash evaporation unit and crystalline element are constituted.Hydroxyacetonitrile and ammonia source ammonia source, carbon source, water etc. first pass through above-mentioned pre- After hot systems are preheated, then through successively carrying out synthesis and hydrolysis around pipe reaction unit, then pass through gas-liquid separation list Member, flash evaporation unit and crystalline element distilled, crystallized, being separated, dry after obtain high-purity glycine.The utility model solves The problem of back-mixing existing for existing tank reactor and length reaction time, also achieves using hydroxyacetonitrile as Material synthesis glycine Continuous production.
Preferably, above-mentioned to be composed in series by three cross-talks around pipe reactor around tube reaction unit, use the mode of temperature-gradient method Combined coefficient is improved, is not only carrying out in tubular reactor synthesis glycolylurea reaction, while also carrying out glycolylurea hydrolysis, this Sample can save reaction solution total residence time, improve reaction efficiency, reduce equipment investment.Compared with direct glycolylurea method, the present invention It realizes and is continuously synthesizing to high-purity glycine by main material of hydroxyacetonitrile, and production process does not generate any waste liquid and can have Effect saves the device space.
Detailed description of the invention
Fig. 1 provides the schematic diagram around pipe reaction device for the utility model.
Specific embodiment
To keep the purpose, technological means and beneficial effect of the application more clear and complete, with reference to the accompanying drawing to the application Specific embodiment be described.Obviously, described embodiment is only some embodiments of the present application, rather than whole Embodiment.Based on the embodiment in the application, those of ordinary skill in the art are obtained without making creative work The all other embodiment obtained, shall fall in the protection scope of this application.
As shown in Figure 1, hydroxyacetonitrile serialization provided by the utility model prepare glycine around pipe reaction device packet Preheating unit is included, the preheating unit includes that sequentially connected metering pump 1 and preheating and static mixer 2, metering pump 1 can be controlled Raw material processed puts into rate, to utilize the speed of feed rate control reaction.The effect of preheater 2 is to be added raw material in advance Heat and be sufficiently mixed, be conducive to reaction progress.
What is connect with the preheating and static mixer 2 is around pipe reaction unit, including sequentially connected first around pipe Formula reactor 3, second, around tubular reactor 5, exports behind pipe reactor 4 around tubular reactor 4 and third described second Place is provided with the pressure reducing valve 6 for controlling reaction pressure.It is to realize temperature each anti-that three sections of effects around tubular reactor, which are arranged, Answer heated up between device in gradient and the synthesis of glycolylurea with separate progress, to further increase combined coefficient, and reduce hydroxyl The decomposition of base acetonitrile and the generation of by-product.Synthesis glycolylurea reaction is not only being carried out in tubular reactor, but also carries out sea Because of hydrolysis, reaction solution total residence time can be saved in this way, improves reaction efficiency, reduce equipment investment.The work of pressure reducing valve 6 Be can make reaction after product steadily enter gas-liquid separation unit.
What is connect with around tube reaction unit is gas-liquid separation unit, including gas-liquid separator 7;With the gas-liquid separation unit Sequentially connected to have flash evaporation unit and crystalline element, the flash evaporation unit includes flash column 8, and the crystalline element includes two strings The first crystallization kettle 9 and the second crystallization kettle 10 of connection.In reaction process, reaction solution successively passes through gas-liquid separator and flash column, returns It receives carbon dioxide and ammonia to utilize as feedstock circulation, ensure that the purity of glycine.
According to the utility model, in the first gas that the entrance that the top of the gas-liquid separator is equipped with the metering pump communicates I is mutually exported, the gas phase being mingled in liquid phase is returned in metering pump 1 by the first gaseous phase outlet I, and carbon dioxide is allowed to repeat to follow Ring utilizes.The top of flash column 8 is equipped with the second gaseous phase outlet II communicated with the entrance of the metering pump, recycling ammonia circulation benefit With.The top of first crystallization kettle 9 is equipped with the first mother liquid recycle mouth III being connected with the three-level around tubular reactor, the second knot The top of brilliant kettle 10 is equipped with the second mother liquor set IV being connected with the flash column.
The utility model, which is utilized, prepares glycine using hydroxyacetonitrile serialization around tubular reactor, based on hydroxyacetonitrile Body raw material forms mixed system with ammonium hydrogen carbonate (or ammonium hydroxide and carbon dioxide), after metering pump enters preheating unit preheating, Thtee-stage shiplock is reacted in tubular reactor, gaseous impurity is removed using gas-liquid separation, flash distillation after reaction, through steaming Evaporate, crystallize, separating, dry after obtain high-purity glycine;The utility model is solved and is returned existing for existing tank reactor The problem for mixing length reaction time, also achieves using hydroxyacetonitrile as the continuous production of Material synthesis glycine.
Due to being composed in series by least three sections around pipe reactor in the utility model around pipe reaction unit, segmentation is used The mode of heating improves combined coefficient, is not only carrying out in tubular reactor synthesis glycolylurea reaction, while also carrying out glycolylurea Hydrolysis can save reaction solution total residence time in this way, improve reaction efficiency, reduce equipment and throw.
The above is only the preferred embodiment of the application, and each embodiment in specification is all made of progressive mode Description, the same or similar parts between the embodiments can be referred to each other, the highlights of each of the examples are with other The difference of embodiment.For system embodiment, since it is substantially similar to the method embodiment, so description Must be fairly simple, the relevent part can refer to the partial explaination of embodiments of method.System embodiment described above is only Schematically, wherein module or the unit as illustrated by the separation member may or may not be it is physically separate , the component shown as module or unit may or may not be physical unit, it can and it is in one place, or Person may be distributed over multiple network units.Some or all of the modules therein can be selected according to the actual needs real The purpose of existing this embodiment scheme.Those of ordinary skill in the art are without creative efforts, it can understand And implement.
Although the application preferred embodiment discloses as above, not the application is made any form of restriction.Although this Application is disclosed above in the preferred embodiment, however is not limited to the application.Anyone skilled in the art, not It is detached under technical scheme ambit, all using the methods and technical content of the disclosure above to technical scheme Make many possible changes and modifications or equivalent example modified to equivalent change.Therefore, all without departing from the application skill The content of art scheme, technical spirit any simple modification made to the above embodiment according to the application and are repaired at equivalent variations Decorations, still fall within technical scheme protection in the range of.

Claims (9)

1. a kind of serialization prepare glycine around pipe reaction device characterized by comprising
Preheating unit for being heated to raw material;
Connect with the preheating unit around tube reaction unit, be used to occur synthesis and hydrolysis;
With the gas-liquid separation unit being connect around tube reaction unit;
The flash evaporation unit being connect with the gas-liquid separation unit;
The crystalline element being connect with the flash evaporation unit.
2. according to claim 1 around pipe reaction device, which is characterized in that the preheating unit includes sequentially connected Metering pump, preheating and static mixer.
3. according to claim 2 around pipe reaction device, which is characterized in that described around tube reaction unit includes successively connecting First connect is around tubular reactor, second around tubular reactor and third around tubular reactor.
4. according to claim 3 around pipe reaction device, which is characterized in that described second after tubular reactor Face exit is provided with the pressure reducing valve for controlling reaction pressure.
5. according to claim 4 around pipe reaction device, which is characterized in that the gas-liquid separation unit includes gas-liquid point From device.
6. according to claim 5 around pipe reaction device, which is characterized in that the top of the gas-liquid separator be equipped with The first gaseous phase outlet that the entrance of the metering pump communicates.
7. according to claim 6 around pipe reaction device, which is characterized in that the flash evaporation unit top is provided with and institute State the second gaseous phase outlet that metering pump intake is connected.
8. according to claim 7 around pipe reaction device, which is characterized in that the crystalline element includes being sequentially connected in series First crystallization kettle and the second crystallization kettle.
9. according to claim 8 around pipe reaction device, which is characterized in that the top of first crystallization kettle be equipped with The top of the first mother liquid recycle mouth around the connection of pipe reaction unit, second crystallization kettle is equipped with and the flash evaporation unit The the second mother liquid recycle mouth communicated.
CN201821604809.5U 2018-09-29 2018-09-29 A kind of serialization prepare glycine around pipe reaction device Expired - Fee Related CN208883750U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110563596A (en) * 2019-09-16 2019-12-13 山东泰和水处理科技股份有限公司 preparation method of dicarboxymethylamino acid salt
CN110698357A (en) * 2019-10-08 2020-01-17 阳泉煤业(集团)有限责任公司 Method for continuously preparing glycine from hydroxyacetonitrile by using microchannel reactor

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110563596A (en) * 2019-09-16 2019-12-13 山东泰和水处理科技股份有限公司 preparation method of dicarboxymethylamino acid salt
CN110563596B (en) * 2019-09-16 2022-07-26 山东泰和水处理科技股份有限公司 Preparation method of dicarboxymethylamino acid salt
CN110698357A (en) * 2019-10-08 2020-01-17 阳泉煤业(集团)有限责任公司 Method for continuously preparing glycine from hydroxyacetonitrile by using microchannel reactor

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