CN102357351A - Direct reflux reaction apparatus for high pressure reaction materials used for production of ethanolamine - Google Patents

Direct reflux reaction apparatus for high pressure reaction materials used for production of ethanolamine Download PDF

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CN102357351A
CN102357351A CN2011102110394A CN201110211039A CN102357351A CN 102357351 A CN102357351 A CN 102357351A CN 2011102110394 A CN2011102110394 A CN 2011102110394A CN 201110211039 A CN201110211039 A CN 201110211039A CN 102357351 A CN102357351 A CN 102357351A
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section
tubular reactor
high pressure
reactor
returning charge
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CN102357351B (en
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谢争兵
尹述柏
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HUBEI XIANLIN CHEMICAL INDUSTRY Co Ltd
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HUBEI XIANLIN CHEMICAL INDUSTRY Co Ltd
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Abstract

The invention provides a direct reflux reaction apparatus for high pressure reaction materials used for production of ethanolamine. The apparatus has multiple sections of tubular reactors, every two adjacent sections directly communicate with each other and connect to form an integral body, the front end of each section of tubular reactor is provided with a feed inlet and a mixer, the rear end of each section of tubular reactor is provided with an extraction opening, the first section of tubular reactor is provided with two mixers, and a material returning opening is provided between the two mixers; the extraction opening of every section of tubular reactor is connected with a feed inlet of a material returning pump through a valve and a material returning pipe, the material returning pipe of the material returning pump discharges materials through two pipelines, one of the pipelines is connected with the material returning opening of the first section of tubular reactor through a valve, and the other one of the pipelines is connected with the extraction opening of the second section of tubular reactor through a valve. The apparatus provided in the invention has the following advantages: utilization efficiency of reaction materials is high; production process flow for ethanolamine can be simplified; energy consumption for separating products used as returning materials is saved; process flow is easy to control and operate; utilization amount of the products of monoethanolamine and diethanolamine used as returning materials is reduced.

Description

The direct back flow reaction device of monoethanolamine reaction under high pressure material
Technical field
The present invention relates to a kind of production of monoethanolamine, especially relate to the direct back flow reaction device of a kind of monoethanolamine reaction under high pressure material.
Background technology
In the production of liquid ammonia process for caustic soda purification monoethanolamine; Be to guarantee safety, the relative oxirane of liquefied ammonia is excessive greatly, generally all surpasses 10 in the mol ratio (being that ammonia alkane compares) of liquefied ammonia and the oxirane of charging place; Ammonia alkane is higher than more, and the shared ratio of the monoethanolamine in the product is just big more.The problem of bringing thus is: in final product structure, the ratio of monoethanolamine (MEA), diethanol amine (DEA), triethanolamine (TEA) is not suitable for the market demand.And will adjust the product mix, just need to reduce ammonia alkane ratio.Improved way is to adopt the multisection type reactor, all establishes the oxirane feed points at every section, and the ammonia alkane ratio that makes every section reactor is all greater than 10, but the ammonia alkane of whole reactor has reached the purpose of in the part scope, adjusting the product mix than having reduced with this.In order to adjust the product mix in a wider context, need monoethanolamine product, diethanol amine product Returning reactor be continued and reacting ethylene oxide.In the process of from reaction mass, isolating very high monoethanolamine product of purity and diethanol amine product, need through a series of separation equipment, the reaction mass utilization ratio is low like this, expend more steam, recirculated cooling water etc.Be necessary to seek a kind of simple, energy-conservation solution for this reason, realize the purpose of product restructuring.
Summary of the invention
The present invention provides a kind of monoethanolamine reaction under high pressure material direct back flow reaction device.It is high mainly to solve existing multisection type reactor energy consumption, and the reaction mass utilization ratio is low, can't adjust technical problems such as monoethanolamine in the final discharging, diethanol amine, triethanolamine proportion of composing.
The present invention mainly is able to solve the problems of the technologies described above through following technical proposals: the direct back flow reaction device of a kind of monoethanolamine reaction under high pressure material; Has the multistage tubular reactor; Directly communicate and fuse between adjacent each section, every section tubular reactor front end is provided with charging aperture, blender, and end is provided with extracts mouth out; Wherein first section tubular reactor has former and later two blenders, is provided with the returning charge mouth between two blenders; Extraction mouth on each section tubular reactor is connected with the charging aperture of returning charge pump through valve, refeed line; The discharge nozzle of returning charge pump is divided into two-way output; Wherein one tunnel process valve is connected with first section tubular reactor returning charge mouth, and another road is connected with the extraction mouth of second section tubular reactor through valve.
As preferably, said refeed line is provided with external jacket outward, logical cooling water in the external jacket, and the external jacket temperature is controlled at 60~95 ℃.
As preferably, the returning charge mouth in said first section tubular reactor is near the back blender.
As preferably, said pipe reaction actuator temperature is controlled at 80~150 ℃, and reactor pressure is controlled at 6.0~11.0Mpa.
As preferably, said direct reflux has four sections tubular reactors.
As preferably, said returning charge pump is selected the high pressure resistant pump of stationary seal for use.
Apparatus of the present invention reaction mass utilization ratio is high, can simplify the technological process of production of monoethanolamine, practices thrift the separating energy consumption as the product of returning charge, and technological process is easy to control operation.Reduce simultaneously and adopt monoethanolamine, diethanol amine product as the needed consumption of returning charge.Use this device; Can change monoethanolamine, diethanol amine, triethanolamine proportion of composing in the final discharging of monoethanolamine reactor; On purpose transfer the proportion of big diethanol amine or triethanolamine; Can accomplish does not have monoethanolamine in the final product structure, or does not have diethanol amine, with meeting the market requirement.
Description of drawings
Fig. 1 is a kind of structural representation of the present invention.
The specific embodiment
Pass through the specific embodiment below, and combine accompanying drawing, do further bright specifically technical scheme of the present invention.
Fig. 1 is a kind of structural representation of the present invention.Can know that by Fig. 1 the direct back flow reaction device of monoethanolamine reaction under high pressure material has four sections tubular reactors 5,6,7,8.Directly communicate and fuse between adjacent each section, every section tubular reactor front end is provided with charging aperture, blender, and end is provided with extracts mouth out, and wherein the 4th section tubular reactor 8 is connected with reaction ager 9.
First section tubular reactor has 3,4, two blender close proximity of two blenders, two blenders 3, is provided with returning charge mouth 2 between 4, and the layout of returning charge mouth 2 is as far as possible near the back blender.Liquefied ammonia, water, oxirane converge with returning charge earlier in preceding mixer mixing then, so that rapidly at back mixer mixing, raising reaction efficiency.Temperature of reactor is controlled at 80~150 ℃, and pressure is controlled at 6.0~11.0Mpa.
Extraction mouth on each section tubular reactor is connected with the charging aperture of returning charge pump 1 through valve 10, refeed line 12; Returning charge pump 1 is selected the high pressure resistant pump of stationary seal for use; Can adopt displacement pump, centrifugal pump etc.; Preferred high voltage bearing centrifugal pump, further preferable mask electric pump or magnetic force driven centrifugal pump adopt frequency control to regulate flow.Be arranged with external jacket 11 outside the refeed line 12, logical cooling water in the external jacket 11, temperature is controlled at 60~95 ℃.The discharge nozzle of returning charge pump 1 is divided into two-way output, and wherein one tunnel process valve 10 is connected with the returning charge mouth 2 of first section tubular reactor 5, and another road is connected with the extraction mouth 52 of first section tubular reactor 6 through valve 10.The charging aperture 61 of extracting mouthful 52 and second sections reactors 6 out near blender, is actually the returning charge inlet of second section reactor 6 at a distance of nearer.
Use this device to produce the concrete case of product:
(1) injects ammonia 2800kg/h, water 185kg/h and oxirane 800kg/h from first section reactor, 5 charging apertures 51; Second section reactor 6 charging apertures 61 injection ring oxidative ethane 750kg/h, the 3rd section reactor 7 charging apertures 71 injection ring oxidative ethane 700kg/h, the 4th section reactor 8 charging apertures 81 injection ring oxidative ethane 600kg/h; Every section ammonia alkane ratio is greater than 10; Total ammonia alkane is than 2.5, and temperature of reactor is controlled at 5 ℃, and reactor pressure is controlled at 6.5Mpa; Extract mouthful 52 extraction mixed material 200kg/h out from first section reactor 5, returning charge pipeline 12 is not lowered the temperature, and temperature is 95 ℃, injects returning charge mouth 2 reactions of first section reactor 5 through returning charge pump 1.After reaction finished, the products obtained therefrom structure was MEA: DEA: TEA ≈ 17: 33: 50.
(2) inject ammonia 2800kg/h, water 185kg/h and oxirane 850kg/h from first section reactor, 5 charging apertures 51; Second section reactor 6 charging apertures, 61 injection ring oxidative ethane 800kg/h and DEA 500kg/h; The 3rd section reactor 7 charging apertures 71 injection ring oxidative ethane 800kg/h and DEA500~700kg/h, the 4th section reactor 8 charging apertures 81 injection ring oxidative ethane 600kg/h, every section ammonia alkane ratio is greater than 10; Temperature of reactor is controlled at 90~100 ℃, and reactor pressure is controlled at 6.0~6.5Mpa; Extract mouthful 62 extraction mixed material 300kg/h out from second section reactor 6, material air-teturning temperature is controlled at 75 ℃, injects returning charge mouth 2 reactions of first section reactor 5 through the returning charge pump.After reaction finished, the products obtained therefrom structure is MEA: DEA: TEA ≈ 25: 0: 75 did not finally have the diethanol amine product.
(3) inject ammonia 2800kg/h, water 185kg/h, MEA 600kg/h from first section reactor, 5 charging apertures 51; And oxirane 850kg/h, second section reactor 6 charging apertures 61 injection ring oxidative ethane 800kg/h, the 3rd section reactor 7 charging apertures 71 injection ring oxidative ethane 800kg/h; The 4th section reactor 8 charging apertures 81 injection ring oxidative ethane 600kg/h; Every section ammonia alkane ratio is greater than 10, and temperature of reactor is controlled at 95 ℃, and reactor pressure is controlled at 6.5Mpa; Extract mouthful 62 extraction mixed material 500kg/h out from second section reactor 6; Material air-teturning temperature is controlled at 70 ℃; Inject the extraction mouth 52 of first section reactor 5 through the returning charge pump and (extract mouth 52 out near second section reactor 6; Through by-pass valve control, extract the returning charge mouth that mouth 52 can be used as second section reactor 6 out), and then get into second section reactor, 6 blender internal reactions.After reaction finished, the products obtained therefrom structure was MEA: DEA: TEA ≈ 10: 40: 50.
(4) inject ammonia 2800kg/h, water 185kg/h, MEA 700kg/h from first section reactor, 5 charging apertures 51; And oxirane 850kg/h, second section reactor 6 charging apertures 61 injection ring oxidative ethane 800kg/h, the 3rd section reactor 7 charging apertures 71 injection ring oxidative ethane 800kg/h; The 4th section reactor 8 charging apertures 81 injection ring oxidative ethane 600kg/h; Every section ammonia alkane ratio is greater than 10, and temperature of reactor is controlled at 95 ℃, and reactor pressure is controlled at 6.5Mpa; Extract mouthful 52 extraction mixed material 500kg/h out from first section reactor 5, material air-teturning temperature is controlled at 70 ℃, injects returning charge mouth 2 reactions of first section reactor 5 through the returning charge pump.After reaction finished, the products obtained therefrom structure was MEA: DEA: TEA ≈ 10: 30: 60
(5) inject ammonia 2800kg/h, water 185kg/h, MEA 700kg/h from first section reactor, 5 charging apertures 51; And oxirane 850kg/h, second section reactor 6 charging apertures, 61 injection ring oxidative ethane 800kg/h and DEA 900kg/h, the 3rd section reactor 7 charging apertures 71 injection ring oxidative ethane 800kg/h; The 4th section reactor 8 charging apertures 81 injection ring oxidative ethane 600kg/h; Every section ammonia alkane ratio is greater than 10, and temperature of reactor is controlled at 95 ℃, and reactor pressure is controlled at 6.5Mpa; Extract mouthful 52 extraction mixed material 600kg/h out from first section reactor 5, material air-teturning temperature is controlled at 70 ℃, injects returning charge mouth 2 reactions of first section reactor 5 through the returning charge pump.After reaction finished, products obtained therefrom finally had only triethanolamine.

Claims (6)

1. direct back flow reaction device of monoethanolamine reaction under high pressure material; Has the multistage tubular reactor; Directly communicate and fuse between adjacent each section, it is characterized in that every section tubular reactor front end is provided with charging aperture, blender, end is provided with extracts mouth out; Wherein first section tubular reactor has former and later two blenders, is provided with the returning charge mouth between two blenders; Extraction mouth on each section tubular reactor is connected with the charging aperture of returning charge pump through valve, refeed line; The discharge nozzle of returning charge pump is divided into two-way output; Wherein one tunnel process valve is connected with first section tubular reactor returning charge mouth, and another road is connected with the extraction mouth of second section tubular reactor through valve.
2. the direct back flow reaction device of a kind of monoethanolamine reaction under high pressure material according to claim 1 is characterized in that said refeed line is provided with external jacket outward, logical cooling water in the external jacket, and the external jacket temperature is controlled at 60~95 ℃.
3. the direct back flow reaction device of a kind of monoethanolamine reaction under high pressure material according to claim 1, it is characterized in that in said first section tubular reactor the returning charge mouth near the back blender.
4. the direct back flow reaction device of a kind of monoethanolamine reaction under high pressure material according to claim 1 is characterized in that said pipe reaction actuator temperature is controlled at 80~150 ℃, and reactor pressure is controlled at 6.0~11.0Mpa.
5. the direct back flow reaction device of a kind of monoethanolamine reaction under high pressure material according to claim 1 is characterized in that said direct reflux has four sections tubular reactors.
6. the direct back flow reaction device of a kind of monoethanolamine reaction under high pressure material according to claim 1 is characterized in that said returning charge pump selects the high pressure resistant pump of stationary seal for use.
CN201110211039.4A 2011-07-27 2011-07-27 Direct reflux reaction apparatus for high pressure reaction materials used for production of ethanolamine Active CN102357351B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101148412A (en) * 2007-09-29 2008-03-26 吴兆立 Multi-point charging EO technique for ethanolamine production
CN101613289A (en) * 2009-05-12 2009-12-30 嘉兴金燕化工有限公司 The abbreviated system that thanomin is produced
CN102126966A (en) * 2010-12-22 2011-07-20 浙江建德建业有机化工有限公司 Method for synthesizing N,N-diethyl ethanolamine

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101148412A (en) * 2007-09-29 2008-03-26 吴兆立 Multi-point charging EO technique for ethanolamine production
CN101613289A (en) * 2009-05-12 2009-12-30 嘉兴金燕化工有限公司 The abbreviated system that thanomin is produced
CN102126966A (en) * 2010-12-22 2011-07-20 浙江建德建业有机化工有限公司 Method for synthesizing N,N-diethyl ethanolamine

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Denomination of invention: Ethanolamine high pressure reaction material direct reflux reaction device

Effective date of registration: 20220125

Granted publication date: 20140723

Pledgee: Bank of China Limited Xiantao branch

Pledgor: HUBEI XIANLIN CHEMICAL CO.,LTD.

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