CN204034675U - A kind of serialization ultralow temperature reaction unit - Google Patents

A kind of serialization ultralow temperature reaction unit Download PDF

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Publication number
CN204034675U
CN204034675U CN201420483542.4U CN201420483542U CN204034675U CN 204034675 U CN204034675 U CN 204034675U CN 201420483542 U CN201420483542 U CN 201420483542U CN 204034675 U CN204034675 U CN 204034675U
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China
Prior art keywords
tubulation
kettle
charging aperture
low head
reaction unit
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn - After Issue
Application number
CN201420483542.4U
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Chinese (zh)
Inventor
陈辉
张朋可
杨振强
杨瑞娜
孙敏青
屈凤波
蒋卫鹏
张银龙
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Institute of Chemistry Henan Academy of Sciences Co Ltd
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Institute of Chemistry Henan Academy of Sciences Co Ltd
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Priority to CN201420483542.4U priority Critical patent/CN204034675U/en
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Publication of CN204034675U publication Critical patent/CN204034675U/en
Withdrawn - After Issue legal-status Critical Current
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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The utility model discloses a kind of serialization ultralow temperature reaction unit, belong to field of chemical equipment.This reaction unit comprises low head and kettle.Its feature is: upper cover is provided with man-hole opening, mirror mouth, noble gas protective conduit, charging aperture, is provided with static column plate in charging aperture pipeline, and charging aperture pipe end is connected with distributing device.Kettle is made up of tubulation, external jacket, thermo detector, and tubulation is vertically arranged in parallel, isometric with kettle, and the upper orifice of every root tubulation is corresponding with the circular hole that upper cover base plate distributes to be connected, and lower nozzle is corresponding with the circular hole on low head base plate to be connected.Fill solid catalyst or solid reaction raw material or solid inert filler in tubulation, bottom tubulation, install screen pack additional; Be full of liquid nitrogen between tubulation, thermo detector is positioned at the outer side of kettle, and one end is connected with tubulation; Vacuum jacket layer is provided with outside kettle.Low head is provided with mirror mouth, Pressure gauge, noble gas blowback pipeline, discharging opening.The utility model structure is simple, and consume energy low, reaction yield is high, steady quality, is particularly suitable for the ultralow temperature reaction industry such as organic phosphine class, boric acid class and applies.

Description

A kind of serialization ultralow temperature reaction unit
Technical field
The utility model belongs to field of chemical equipment, relates to a kind of reaction unit, particularly relates to a kind of serialization ultralow temperature reaction unit.
Background technology
Organic phosphine class, boric acid compound are the important intermediates of a class in pharmacy, electronic chemical product, catalyst field, and most of reaction needed is reacted under the condition of ultralow temperature of-80 DEG C.At present, the low-temp reaction still that the 500L of employing band stirs more is in the industrial production produced, and the structure of reactor is: add coil pipe in still, passes into liquid nitrogen and lowers the temperature; Still outer jacketed is vacuum state in chuck.Due in course of reaction, air-teturning mixed phenomenon is serious, and temperature in the kettle is once higher than reaction temperature, and side reaction aggravates, and causes target product yield to reduce.In course of reaction, the temperature of charge near coil pipe is extremely low, and the temperature of charge away from coil pipe is higher, and cooling-down effect is poor.All need cleaning reaction owing to producing at every turn, again feed intake, drop to-80 DEG C from normal temperature repeatedly to reactor, production efficiency is low, and energy waste is extremely serious, and cost of labor remains high.For meeting industrial production demand, be badly in need of at present improving it.
Summary of the invention
Not enough for prior art, it is simple that the utility model object is to provide a kind of structure, consumes energy low, simple to operate, steady quality, operating efficiency is high, be particularly suitable for ultra low temperature state under continuous prodution organic phosphine class, boric acid series products device.
For realizing the purpose of this utility model, concrete technical scheme is as follows:
This reaction unit comprises low head and kettle.Its feature is: upper cover has man-hole opening, mirror mouth, noble gas import, charging aperture, is provided with static column plate in charging aperture pipeline, and charging aperture pipe end is connected with distributing device.Different liquid charging stocks enters pipeline by charging aperture, the static column plate in charging aperture pipeline mixes, by being delivered continuously in reactor after distributing device.Kettle is made up of tubulation, external jacket, thermo detector, and tubulation is vertically arranged in parallel, isometric with kettle, and the upper orifice of every root tubulation is corresponding with the circular hole that upper cover base plate distributes to be connected, and lower nozzle is corresponding with the circular hole on low head base plate to be connected.Fill solid catalyst or solid reaction raw material or solid inert filler in every root tubulation, bottom tubulation, install screen pack additional; Be full of liquid nitrogen between tubulation, thermo detector is positioned at the outer side of kettle, and one end is connected with tubulation outer wall; Be provided with vacuum jacket layer outside kettle, play protection heat-blocking action.Low head is provided with mirror mouth, Pressure gauge, inert gas outlet, discharging opening.Upper low head is with bolts with kettle respectively.
Described distributing device adopts gondola water faucet structure with holes, is evenly distributed in by liquid charging stock in reactor tube side.Thermo detector upper, middle and lower are uniformly distributed in the outer side of kettle, as point for measuring temperature observing and controlling temperature in the kettle at any time.
The utility model device innovative point and principle are: reaction raw materials is by charging aperture pipeline Homogeneous phase mixing, carried by gondola water faucet distributing device and flow into tubulation, load solid catalyst or solid material or solid inert filler in tubulation, liquid nitrogen is full of between tubulation outer wall, circulation is imported and exported by liquid nitrogen, reaction temperature can be regulated well, maintain low-temperature condition, under low-temperature condition, liquid charging stock at the uniform velocity down contacts with solid catalyst in tubulation or solid material in flow process in tubulation, gradual reaction in tubulation tube side, reacted material enters subsequent processing by discharging opening.
The invention has the beneficial effects as follows: adopt tubular structure in still, different material mixes in charging aperture, can continuity periodic duty, cold media uses the liquid nitrogen of-198 DEG C, and under tubulation is in protection of liquid nitrogen state, heat transfer efficiency is high, consumes energy extremely low; Fill solid catalyst or solid material or solid inert filler in tubulation, augmenting response contact area, because material is without air-teturning mixed phenomenon, avoids side reaction aggravate, and main reaction can be carried out preferably, thus the production yield that acquisition is higher.Organic phosphine class, boric acid series products is produced, steady quality, high, the applicable industrial application of operating efficiency under ultra low temperature state.
Accompanying drawing explanation
Fig. 1 is the utility model structural representation.
Detailed description of the invention
For being described in detail to the utility model better, by reference to the accompanying drawings, give an actual example as follows:
Embodiment 1
The utility model comprises upper cover 16, low head 17 and kettle 18.Its feature is: upper cover 16 is provided with mirror mouth 4, man-hole opening 5, inert gas import 6 and charging aperture 1, is provided with static column plate 2 in charging aperture 1 pipeline, and charging aperture 1 pipe end is connected with distributing device 3.Different liquid charging stocks enters pipeline by charging aperture 1, the static column plate 2 in charging aperture 1 pipeline mixes, by being delivered continuously in reactor after distributing device 3.Kettle 18 is made up of tubulation 10, external jacket 8, thermo detector 7, tubulation 10 is vertically arranged in parallel, isometric with kettle 18, the upper orifice of every root tubulation 10 is corresponding with the circular hole that upper cover 16 base plate distributes to be connected, and lower nozzle is corresponding with the circular hole on low head 17 base plate to be connected.Fill solid catalyst or solid reaction raw material or solid inert filler 9 in every root tubulation 10, bottom tubulation 10, install 325 order screen packs additional; Liquid nitrogen is passed into by liquid nitrogen import 11, and liquid nitrogen outlet 12 is discharged, and makes to be full of liquid nitrogen between tubulation 10.Thermo detector 7 is positioned at the outer side of kettle 18, and one end is connected with tubulation 10 outer wall; Be provided with vacuum jacket layer 8 outside kettle 18, play protection heat-blocking action.Low head 17 is provided with mirror mouth 4, material flow can be observed through state and Pressure gauge 14, inert gas outlet 13, discharging opening 15.Upper low head 16,17 is with bolts with kettle 18 respectively.
Described distributing device 3 adopts gondola water faucet structure with holes, is evenly distributed in by liquid charging stock in reactor tube side.Thermo detector 7 upper, middle and lower are uniformly distributed in the outer side of kettle 18, as point for measuring temperature observing and controlling temperature in the kettle at any time.
Application examples 1
During actual production tri-butyl phosphine, catalyst 9 has been pre-charged with in tubulation 10, inert gas is passed into by inert gas charging aperture 6, by air emptying in tubulation 10, liquid nitrogen is passed into by liquid nitrogen import 11, temperature in reactor tubulation 10 is down to-80 DEG C, methyl tertiary butyl ether(MTBE), tertiary butyl chloride is transported to charging aperture 1 by different pipelines according to the speed of 30Kg/h, static column plate 2 mixes, evenly spray through distributing device 3, flow in tubulation 10, contact with the catalyst 9 be distributed in tubulation, gradual reaction in flowing, reacted liquid product flow goes out tubulation 10, enter in low head 17, next process is entered by discharging opening 15.

Claims (3)

1. a serialization ultralow temperature reaction unit, comprises low head and kettle, and its feature is: upper cover is provided with man-hole opening, mirror mouth, noble gas import, charging aperture, is provided with static column plate in charging aperture pipeline, and charging aperture pipe end is connected with distributing device; Kettle is made up of tubulation, external jacket, thermo detector, and tubulation is vertically arranged in parallel, isometric with kettle, and the upper orifice of every root tubulation is corresponding with the circular hole that upper cover base plate distributes to be connected, and lower nozzle is corresponding with the circular hole on low head base plate to be connected; Fill solid catalyst or solid reaction raw material or solid inert filler in every root tubulation, bottom tubulation, install screen pack additional; Liquid nitrogen is full of between tubulation; Thermo detector is positioned at the outer side of kettle, and one end is connected with tubulation outer wall; Vacuum jacket layer is provided with outside kettle; Low head is provided with mirror mouth, Pressure gauge, inert gas outlet, discharging opening; Upper low head is with bolts with kettle respectively.
2. serialization ultralow temperature reaction unit as claimed in claim 1, its feature is: described distributing device adopts gondola water faucet structure with holes.
3. serialization ultralow temperature reaction unit as claimed in claim 1 or 2, its feature is: described thermo detector upper, middle and lower are uniformly distributed in the outer side of kettle.
CN201420483542.4U 2014-08-26 2014-08-26 A kind of serialization ultralow temperature reaction unit Withdrawn - After Issue CN204034675U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201420483542.4U CN204034675U (en) 2014-08-26 2014-08-26 A kind of serialization ultralow temperature reaction unit

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201420483542.4U CN204034675U (en) 2014-08-26 2014-08-26 A kind of serialization ultralow temperature reaction unit

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CN204034675U true CN204034675U (en) 2014-12-24

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104162388A (en) * 2014-08-26 2014-11-26 河南省科学院化学研究所有限公司 Continuous ultralow temperature reaction device
CN107388042A (en) * 2017-08-14 2017-11-24 上海航天设备制造总厂 Liquid nitrogen sustainable supply device and method for ultralow temperature cutting

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104162388A (en) * 2014-08-26 2014-11-26 河南省科学院化学研究所有限公司 Continuous ultralow temperature reaction device
CN104162388B (en) * 2014-08-26 2016-05-11 河南省科学院化学研究所有限公司 A kind of serialization ultralow temperature reaction unit
CN107388042A (en) * 2017-08-14 2017-11-24 上海航天设备制造总厂 Liquid nitrogen sustainable supply device and method for ultralow temperature cutting

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C14 Grant of patent or utility model
GR01 Patent grant
AV01 Patent right actively abandoned

Granted publication date: 20141224

Effective date of abandoning: 20160511

C25 Abandonment of patent right or utility model to avoid double patenting