CN204097373U - The continuous reacting device of synthesis 3-amino-1,2-PD - Google Patents
The continuous reacting device of synthesis 3-amino-1,2-PD Download PDFInfo
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- CN204097373U CN204097373U CN201420439893.5U CN201420439893U CN204097373U CN 204097373 U CN204097373 U CN 204097373U CN 201420439893 U CN201420439893 U CN 201420439893U CN 204097373 U CN204097373 U CN 204097373U
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- 230000015572 biosynthetic process Effects 0.000 title description 3
- 238000003786 synthesis reaction Methods 0.000 title description 3
- 238000006243 chemical reaction Methods 0.000 claims abstract description 49
- 238000002156 mixing Methods 0.000 claims abstract description 25
- 238000010521 absorption reaction Methods 0.000 claims abstract description 21
- 239000006200 vaporizer Substances 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 13
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 12
- 238000002425 crystallisation Methods 0.000 claims abstract description 12
- 230000018044 dehydration Effects 0.000 claims abstract description 10
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 10
- 230000009615 deamination Effects 0.000 claims abstract description 8
- 238000006481 deamination reaction Methods 0.000 claims abstract description 8
- 230000008025 crystallization Effects 0.000 claims abstract description 7
- DNIAPMSPPWPWGF-UHFFFAOYSA-N propylene glycol Substances CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims abstract description 7
- KLSJWNVTNUYHDU-UHFFFAOYSA-N Amitrole Chemical compound NC1=NC=NN1 KLSJWNVTNUYHDU-UHFFFAOYSA-N 0.000 claims abstract description 6
- 230000000694 effects Effects 0.000 claims abstract description 6
- 230000003139 buffering effect Effects 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 239000011552 falling film Substances 0.000 claims abstract description 4
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 229910021529 ammonia Inorganic materials 0.000 description 11
- 229960004063 propylene glycol Drugs 0.000 description 9
- 238000000034 method Methods 0.000 description 7
- 208000005156 Dehydration Diseases 0.000 description 6
- 238000001704 evaporation Methods 0.000 description 6
- 230000008020 evaporation Effects 0.000 description 6
- 239000011541 reaction mixture Substances 0.000 description 5
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 235000011121 sodium hydroxide Nutrition 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 3
- 238000010612 desalination reaction Methods 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000005192 partition Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000007086 side reaction Methods 0.000 description 3
- MQDLKAADJTYKRH-UHFFFAOYSA-N 1-aminopropane-1,2,3-triol Chemical compound NC(O)C(O)CO MQDLKAADJTYKRH-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 241000216843 Ursus arctos horribilis Species 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000009969 flowable effect Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- RNIPBGMVTAUWNH-UHFFFAOYSA-N [F].[I] Chemical compound [F].[I] RNIPBGMVTAUWNH-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 238000005915 ammonolysis reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000002872 contrast media Substances 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- NBQNWMBBSKPBAY-UHFFFAOYSA-N iodixanol Chemical compound IC=1C(C(=O)NCC(O)CO)=C(I)C(C(=O)NCC(O)CO)=C(I)C=1N(C(=O)C)CC(O)CN(C(C)=O)C1=C(I)C(C(=O)NCC(O)CO)=C(I)C(C(=O)NCC(O)CO)=C1I NBQNWMBBSKPBAY-UHFFFAOYSA-N 0.000 description 1
- NTHXOOBQLCIOLC-UHFFFAOYSA-N iohexol Chemical compound OCC(O)CN(C(=O)C)C1=C(I)C(C(=O)NCC(O)CO)=C(I)C(C(=O)NCC(O)CO)=C1I NTHXOOBQLCIOLC-UHFFFAOYSA-N 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model discloses one to be used for synthesizing 3-amino-1, the continuous reacting device of 2-propylene glycol, described continuous reacting device comprises mixing tank, Multistage tower-type reactor, vaporizer, crystallization kettle, condenser, absorption tower and recycle pump, described Multistage tower-type reactor is the tower reactor of band inner member, its progression is 2-10 level, described vaporizer is three grades of falling-film evaporators, described mixing tank is connected with one end of Multistage tower-type reactor, the other end of Multistage tower-type reactor is connected with vaporizer, the effect of vaporizer is deamination dehydration, its gas phase be evaporated enters absorption tower by coupled condenser, material through deamination dehydration enters the crystallization kettle crystallisation by cooling be connected with vaporizer, absorption tower is furnished with tourie and recycle pump, in order to store ammoniacal liquor and circular buffering.The continuous device that the utility model provides is simple, workable, and production capacity is large, and reaction yield is high.
Description
Technical field
The utility model relates to a kind of continuous reacting device being used for synthesizing 3-amino-1,2-PD.
Background technology
3-amino-1,2-PD, molecular formula C
3h
9nO
2, CAS NO:616-30-8, boiling point 264-265 DEG C, amino-glycerol is medicine intermediate, mainly the X-CT contrast medium Schering AG) (i.e. Omnipaque) of water-soluble, non-ionic type, iodine fluorine alcohol, the synthesis material of Visipaque 320.Its operational path is by 3-chlorine-1,2-propylene glycol-> 3-amino-1,2-PD, and the aqueous solution generation ammonolysis reaction of 3-chlorine-1,2-propylene glycol and ammonia or ammonia is obtained 3-amino-1,2-PD aqueous solution and ammonium chloride.Again by dehydration desalination, thick steaming and rectifying obtain highly purified 3-amino-1,2-PD.A lot of by product can be produced, as diamines and triamine in ammonia solution preocess.Reduce side reaction as far as possible, improve the key that product purity is this technique.
CN 201516344 U, discloses a kind of tank reactor to realize the device of this reaction process, and this is a kind of more conventional reaction unit.All the time it is low to there is efficiency in single kettle device production material, and output is little, complex operation etc. problem.CN 101250115A discloses a kind of 3-amino-1, the continuous production method of 2-propylene glycol, by 3-chlorine-1,2-propylene glycol and ammoniacal liquor first through mixing tank premix, then react through a segment pipe reactor, temperature of reaction is 60-100 DEG C, pressure is 3-6Ma, and the time is 6-12 minute, obtains 3-amino-1, the mixing solutions of 2-propylene glycol and ammoniacal liquor, then obtains finished product after purifying.The method yield can reach 70%.The method relative productivity is comparatively large, but temperature is high, and pressure is high, and side reaction is many, and yield is low.
Utility model content
For prior art Problems existing, the invention provides a kind of continuous reacting device synthesizing 3-amino-1,2-PD.Concrete technical scheme is as follows:
Described continuous reacting device comprises mixing tank, Multistage tower-type reactor, vaporizer, crystallization kettle, condenser, absorption tower and recycle pump, described Multistage tower-type reactor is the tower reactor of band inner member, its progression is 2-10 level, described vaporizer is three grades of falling-film evaporators, described mixing tank is connected with one end of Multistage tower-type reactor, the other end of Multistage tower-type reactor is connected with vaporizer, the effect of vaporizer is deamination dehydration, its gas phase be evaporated enters absorption tower by coupled condenser, material through deamination dehydration enters the crystallization kettle crystallisation by cooling be connected with vaporizer, absorption tower is furnished with tourie and recycle pump, in order to store ammoniacal liquor and circular buffering.
Tower reactor utilizes the relative merits of in chemical reactor two primitive reaction devices and multistage CSTR reactor and piston flow reactor to combine design.Mainly consider economy and the operability of the chemical reaction industrial implementation of large reaction volume.Horizontal sliding flow reactor needs higher flow velocity to improve Reynolds number, and multistage CSTR reactor then exists larger back-mixing; In the application, Multistage tower-type reactor adopts in band and purchases the structure of part, possesses the feature of complete mixing flow and piston flow reactor, and can effective distribute fluids flowable state, and adjusts flow-pattern, and increase empir-ical formulation mass transfer effect, reduces longitudinal back-mixing degree.
In the present invention, preferably, described inner member is the structure that traverse baffle is alternate with orifice plate, and distance between plates is 1-5 times of reaction tower diameter.
More preferably, described traverse baffle is circular baffling screen, and diameter is identical with reaction tower internal diameter, the wide 80-90mm of grizzly bar, and grizzly bar is spaced apart 40-60mm; Described orifice plate is circular sieve plate, and sieve diameter is 8-12mm circular hole, and center of circle spacing is 16-24mm, evenly arranges, and is fastened by bolts on tower wall, and be convenient to dismounting and maintenance, be bolted on reaction tower tower wall, 3-5 portion installed by each reaction tower.
In the present invention, preferably, described internal partition spacing is 2.5 times of reaction tower diameter.
In the present invention, preferably, the progression of described Multistage tower-type reactor is 2-5 level.
In the present invention, preferably, the annexation of described Multistage tower-type reactor is in parallel or series connection, is more preferably series connection.
In the present invention, preferably, the diameter of described tower reactor is 0.6-0.8m, and tower height is 13-15m.
Preferably, in described continuous reacting device, for staged reactor, first material will be pumped it in mixing tank by fresh feed pump, the upper end of mixing tank is connected with first order reaction tower top, the bottom of first order reaction tower is connected with the bottom of second order reaction tower, and second order reaction column overhead and the bottom of third order reaction tower link, then the bottom of third order reaction tower links with the bottom of fourth-order reaction tower, and fourth-order reaction column overhead and the bottom of Pyatyi reaction tower link, recycling cross like this connects and composes Multistage tower-type reactor, last step reaction tower top is connected with the top of one-level vaporizer.
Beneficial effect: use the Multistage tower-type reactor of band inner member to realize high-level efficiency continuous prodution, tower reactor both ensure that enough reaction volumes, achieve again the successive reaction of similar horizontal sliding streaming, and tower reactor has optimum investment and productivity ratio under equivalent responses pressure and the residence time, installation and maintenance is more laborsaving, very convenient in production capacity adjustment, can adapt to the variation of larger load, 5 grades of towers realize 3 times of production capacities and regulate.Effect is very good in actual applications, and the three grade falling-film evaporators ease in use accordingly at subsequent processing stage evaporate deamination and dehydration.Single unit system is fairly simple, workable, and production capacity is very large.
Accompanying drawing explanation
The continuous reacting device structure brief introduction figure that Fig. 1: 3-amino-1,2-PD is used, the progression of reactor is 2 grades.
In figure: 1-3-chloro-1, 2-propylene glycol fresh feed pump, 2-3-chloro-1, 2-propylene glycol storage tank, 3-mixing tank, 4-first order reaction tower, 5-second order reaction tower, 6-liquid caustic soda storage tank, 7-liquid caustic soda fresh feed pump, 8-level vaporizer, 9-level condenser, 10-ammoniacal liquor fresh feed pump, 11-first order absorption tank, 12-first order absorption recycle pump, 13-first grade absorption tower, 14-secondary evaporimeter, 15-secondary transfering material pump, 16-secondary condenser, 17-secondary tourie, 18-secondary absorbent recirculation pump, 19-two-level absorption tower, 20-tri-grades of vaporizers, 21-crystallization kettle, 22-whizzer, 23-whizzer geosyncline, 24-mother liquor produces pump, 25-tri-grades of condensers, 26-water rushes vacuum pump, 27-tri-grades of touries.
Embodiment
Below in conjunction with accompanying drawing, explanation is further explained to the utility model.
First the present invention provides a kind of process unit of continuous prodution amino-glycerol, and this is a kind of Multistage tower-type reaction unit, obtains the device of 3-amino-1,2-PD for 3-chlorine-1,2-propylene glycol and ammoniacal liquor successive reaction.Multi-stage column reactor generally can have 2-10 level, preferred 2-5 stage reactor.Multistage tower-type reactor adopts the structure of band internal partition, and strengthening mass transfer and heat transfer, possess the feature of complete mixing flow and piston flow reactor, and can effective distribute fluids flowable state, and adjust flow-pattern, increase empir-ical formulation mass transfer effect, reduce longitudinal back-mixing degree.
Tower reactor utilizes the relative merits of in chemical reactor two primitive reaction devices and multistage CSTR reactor and piston flow reactor to combine design.Mainly consider economy and the operability of the chemical reaction industrial implementation of large reaction volume.Horizontal sliding flow reactor needs higher flow velocity to improve Reynolds number, then there is larger back-mixing in multistage CSTR reactor, the application solves this problem by the tower reactor installing internal partition additional, as long as use secondary diameter 0.6 meter, the reaction tower of high 13 meters just can realize 500 tons/year of production capacities, 1000 tons/year of production capacities can be realized at level Four tower, can adjust easily as required.The above reaction tower device of secondary, increases tower level and can increase production capacity, can parallel connection can connect, consider from control angle, and series connection stability is better than parallel connection.Reaction mass is with the reaction tower of inner member after mixing tank, and inner member is the structure that traverse baffle is alternate with orifice plate, and distance between plates is 1-5 times of tower diameter, superior distance 2.5 times, improves flow velocity and strengthening parallel mixing, reduces inter-stage back-mixing degree simultaneously.
The feature of this reaction unit is that parallel mixing is effective, side reaction is few, can realize DCS automatic control, and specific works process is: for secondary tower reactor, as shown in Figure 1, reaction mass is transported to according to proportioning from 3 material pots by 3 fresh feed pumps by device charging needs position.Use fresh feed pump 1 from storage tank 2 by chloro-for 3-1, 2-propylene glycol is pumped in mixing tank 3, fresh feed pump 10 is used to be pumped into by ammoniacal liquor in mixing tank 3, 3-chloro-1, reaction tower is entered after 2-propylene glycol and ammoniacal liquor mixing, just start to react in mixing process, and enter first reaction tower and second reaction tower continuation reaction successively, fresh feed pump 7 is used by liquid caustic soda from liquid caustic soda storage tank pump to the second reaction tower when reaction mixture enters second reaction tower, the reaction mixture material reacted completely through the second reaction tower enters one-level vaporizer 8 from the part of second order reaction tower near top and is evaporated from reaction mixture by the ammonia that major part is superfluous, the ammonia gone out through one-level evaporator evaporation is by first-stage condenser 9, first grade absorption tower 13 and first order absorption tank 11 condensation also fully recycling, because ammonia surplus is more, first order absorption can not reclaim completely, also need through secondary, three grades of evaporations are evaporated as far as possible and are reclaimed superfluous ammonia, reaction mixture after one-level evaporator evaporation then enters secondary evaporimeter 14 and continues deamination dehydration, after secondary evaporimeter evaporation, the ammonia of remainder enters two-level absorption tower 19 by secondary condenser 16 condensation and is recovered to secondary tourie 17 and recycles, simultaneously, ammoniacal liquor in secondary tourie enters first order absorption tank and then recycle through secondary transfering material pump 15, equally, reaction mixture through dual evaporation enters third evaporator 20 and rushes vacuum pump 26 and three grades of condensers 25 and three grades of tourie 27 decompression dehydrations by water, be exactly mainly 3-amino-1 from third evaporator material out, 2-propylene glycol and salt, water mixture, the material removed after most of water contains a lot of precipitation salt, this material just enters crystallization kettle 21 crystallisation by cooling, and filter desalination by whizzer 22, crude product after desalination obtains qualified 3-amino-1 through refining, 2-propylene glycol product.Be exactly briefly that the ammonia be evaporated, by entering first grade absorption tower 13 after first-stage condenser 9 condensation, fully absorbs by the gas phase that ammonia goes out through one-level evaporator evaporation; The direct condensation of the ammonia water mixture that secondary evaporimeter steams obtains ammonia soln, and the ammonia do not absorbed completely enters absorption tower, the second stage and absorbs, and an absorbent recirculation pump and tourie are joined in each absorption tower, is used for storing ammoniacal liquor and circular buffering.
The above; be only the utility model preferably embodiment; but protection domain of the present utility model is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the utility model discloses; be equal to according to the technical solution of the utility model and utility model design thereof and replace or change, all should be encompassed within protection domain of the present utility model.
Claims (7)
1. one kind is used for synthesizing 3-amino-1, the continuous reacting device of 2-propylene glycol, it is characterized in that, described continuous reacting device comprises mixing tank, Multistage tower-type reactor, vaporizer, crystallization kettle, condenser, absorption tower and recycle pump, described Multistage tower-type reactor is the tower reactor of band inner member, its progression is 2-10 level, described vaporizer is three grades of falling-film evaporators, described mixing tank is connected with one end of Multistage tower-type reactor, the other end of Multistage tower-type reactor is connected with vaporizer, the effect of vaporizer is deamination dehydration, its gas phase be evaporated enters absorption tower by coupled condenser, material through deamination dehydration enters the crystallization kettle crystallisation by cooling be connected with vaporizer, absorption tower is furnished with tourie and recycle pump, in order to store ammoniacal liquor and circular buffering.
2. continuous reacting device according to claim 1, is characterized in that, described inner member is the structure that traverse baffle is alternate with orifice plate, and distance between plates is 1-5 times of reaction tower diameter.
3. continuous reacting device according to claim 2, is characterized in that, described traverse baffle is circular baffling screen, and described orifice plate is circular sieve plate, is bolted on reaction tower tower wall, and 3-5 portion installed by each reaction tower.
4. continuous reacting device according to claim 2, it is characterized in that, described inner member spacing is 2.5 times of reaction tower diameter.
5. continuous reacting device according to claim 1, is characterized in that, the progression of described Multistage tower-type reactor is 2-5 level.
6. continuous reacting device according to claim 1, is characterized in that, the annexation of described Multistage tower-type reactor is in parallel or series connection.
7. continuous reacting device according to claim 1, is characterized in that, the diameter of described tower reactor is 0.6-0.8m, and tower height is 13-15m.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420439893.5U CN204097373U (en) | 2014-08-06 | 2014-08-06 | The continuous reacting device of synthesis 3-amino-1,2-PD |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201420439893.5U CN204097373U (en) | 2014-08-06 | 2014-08-06 | The continuous reacting device of synthesis 3-amino-1,2-PD |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104130140A (en) * | 2014-08-06 | 2014-11-05 | 内蒙古圣氏化学有限公司 | Method for synthetizing 3-amino-1, 2-propylene glycol by using continuous reaction device |
| CN110922363A (en) * | 2019-12-28 | 2020-03-27 | 新华制药（寿光）有限公司 | Continuous production process of violuric acid |
| CN111116523A (en) * | 2019-12-30 | 2020-05-08 | 浙江新和成股份有限公司 | System and process for producing α -chloro- α -acetyl-gamma-butyrolactone |
-
2014
- 2014-08-06 CN CN201420439893.5U patent/CN204097373U/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104130140A (en) * | 2014-08-06 | 2014-11-05 | 内蒙古圣氏化学有限公司 | Method for synthetizing 3-amino-1, 2-propylene glycol by using continuous reaction device |
| CN104130140B (en) * | 2014-08-06 | 2016-04-13 | 内蒙古圣氏化学有限公司 | By the method for continuous reacting device synthesis 3-amino-1,2-PD |
| CN110922363A (en) * | 2019-12-28 | 2020-03-27 | 新华制药（寿光）有限公司 | Continuous production process of violuric acid |
| CN111116523A (en) * | 2019-12-30 | 2020-05-08 | 浙江新和成股份有限公司 | System and process for producing α -chloro- α -acetyl-gamma-butyrolactone |
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Address after: The Inner Mongolia Autonomous Region Alashanzuoqi of Alashan Alashan Economic Development Zone Town WuSitai Patentee after: INNER MONGOLIA SAINTCHEM CHEMICALS CO.,LTD. Address before: The Inner Mongolia Autonomous Region Alashanzuoqi of Alashan Alashan Economic Development Zone Patentee before: INNER MONGOLIA SAINTCHEM CHEMICALS Co.,Ltd. |
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Denomination of utility model: Continuous reactor for synthesis of 3-amino-1,2-propanediol Effective date of registration: 20210324 Granted publication date: 20150114 Pledgee: Bank of China Limited BAYANHOT branch Pledgor: INNER MONGOLIA SAINTCHEM CHEMICALS Co.,Ltd. Registration number: Y2021150000028 |
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Denomination of utility model: Continuous reactor for synthesis of 3-amino-1,2-propanediol Effective date of registration: 20220526 Granted publication date: 20150114 Pledgee: Bank of China Limited BAYANHOT branch Pledgor: INNER MONGOLIA SAINTCHEM CHEMICALS CO.,LTD. Registration number: Y2022150000044 |
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