CN205328901U - Device of dichloroacetic acid selectivity dechlorination - Google Patents
Device of dichloroacetic acid selectivity dechlorination Download PDFInfo
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- CN205328901U CN205328901U CN201620080103.8U CN201620080103U CN205328901U CN 205328901 U CN205328901 U CN 205328901U CN 201620080103 U CN201620080103 U CN 201620080103U CN 205328901 U CN205328901 U CN 205328901U
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Abstract
The utility model discloses a device of dichloroacetic acid selectivity dechlorination, including raw material liquid storage tank, N2 storage tank, H2 storage tank, gas -liquid mixer, initial response ware, second reactor, vapour and liquid separator, absorption tower and distillation column, raw material liquid storage tank, N2 storage tank and H2 storage tank all are connected with gas -liquid mixer's pan feeding mouth, gas -liquid mixer's discharge gate is connected with the feed inlet of initial response ware and second reactor respectively, the discharge gate of initial response ware is connected with the feed inlet of vapour and liquid separator and second reactor respectively, the discharge gate of second reactor is connected with vapour and liquid separator's feed inlet, vapour and liquid separator's discharge gate is connected with the feed inlet on absorption tower and the feed inlet of distillation column respectively, the discharge gate and the hydrochloric acid collection tank on absorption tower are connected, the discharge gate and a monoxone collection tank of distillation column are connected. The utility model discloses simple structure, reasonable in design, easy operation, hydrogenation is efficient.
Description
Technical field
This utility model relates to a kind of dechlorination apparatus, especially relates to the device of a kind of dichloroacetic acid selectivity dechlorination。
Background technology
Monoxone is mainly used in the conventional Insecticides (tech) & Herbicides (tech) of synthesis kind more than 20 and plant growth regulation;Secondly it is mainly used in producing the medicine such as vitamins, hormone in pharmaceuticals industry;It is mainly used in synthesizing activity dyestuff at fuel industry;It addition, monoxone is also important organic synthesis intermediate, can be used for preparing the fine chemicals such as malonic acid, Cyanoacetyl-Cyacetazid, malonate。At present, chloroacetic acid prepares mainly by acetic acid carries out chlorination, has sulfur method and acetic anhydride method。Compared with sulfur method, the consumption of acetic anhydride method acetic acid in course of reaction and chlorine is all smaller, and the quality of by-product hydrochloric acid is also higher, and the growing amount of dichloroacetic acid is fewer (3~5%)。But whether sulfur method or acetic anhydride method, can generate chlorinated secondary product dichloroacetic acid even trichloroacetic acid in course of reaction。
Dichloroacetic acid is harmful so that the chloroacetic acid that chlorination obtains cannot use in food additive, medicine and cosmetics, not only contaminated environment, and reduces the competitiveness of product。It is thus desirable to obtain a kind of substantially pure monochloroacetic acid, or the chloroacetic acid containing minute quantity dichloroacetic acid, this this work of by-product dichloroacetic acid allowing for how effectively removing in chlorizate becomes the focus of research。Due to chloroacetic acid and dichloroacetic acid boiling point very close to so that cannot realize by distilling the dichloroacetic acid separating and removing in chloroacetic acid in the industry。Generally by carrying out selective catalytic hydrogenation dechlorination reaction in fixed bed system in present engineering, dichloroacetic acid is taken off a chlorine and obtains chloroacetic acid。Compared to traditional technique, its system is simple, cost reduces, realizes the dechlorination of dichloroacetic acid。But, the device of this existing technique often problem arises in that when actual motion: the concentration requirement of dichloroacetic acid is higher, once beyond claimed range, hydrogenation efficiency significantly reduces, and selectivity reduces, deterioration in quality。
Therefore, nowadays lack a kind of simple in construction, reasonable in design, simple to operate, hydrogenation efficiency is high, suitable in the device of dichloroacetic acid selective hydrogenation dechlorination。
Utility model content
Technical problem to be solved in the utility model is in that for above-mentioned deficiency of the prior art, it is provided that the device of a kind of dichloroacetic acid selectivity dechlorination。This apparatus structure is simple, reasonable in design, simple to operate, hydrogenation efficiency is high, suitable in dichloroacetic acid selective hydrogenation dechlorination。
For solving above-mentioned technical problem, the technical solution adopted in the utility model is: the device of a kind of dichloroacetic acid selectivity dechlorination, it is characterised in that: include material liquid storage tank, N2Storage tank, H2Storage tank, air and liquid mixer, reactor, gas-liquid separator, absorption tower and distillation column, described reactor includes the first reactor and the second reactor, the discharging opening of described material liquid storage tank, N2The gas outlet of storage tank and H2The gas outlet of storage tank is connected with the feeding mouth of air and liquid mixer each through pipeline, the discharging opening of described air and liquid mixer is connected with the charging aperture of the charging aperture of the first reactor and the second reactor respectively by pipeline, the discharging opening of described first reactor is connected with the charging aperture of the charging aperture of gas-liquid separator and the second reactor respectively by pipeline, the discharging opening of described second reactor is connected with the charging aperture of gas-liquid separator by pipeline, the discharging opening of described gas-liquid separator includes liquid material outlet and gas material outlet, the outlet of described gas material is connected with the charging aperture on absorption tower by pipeline, the discharging opening on described absorption tower is connected with hydrochloric acid collecting tank by pipeline, the outlet of described liquid material is connected with the charging aperture of distillation column by pipeline, the discharging opening of described distillation column is connected with chloroacetic acid collecting tank by pipeline。
The device of above-mentioned a kind of dichloroacetic acid selectivity dechlorination, it is characterised in that: it is connected to magnetic force driving pump also by pipeline between discharging opening and the feeding mouth of air and liquid mixer of described material liquid storage tank。
The device of above-mentioned a kind of dichloroacetic acid selectivity dechlorination, it is characterised in that: described first reactor and the second reactor are the hydrogenation tower being filled with catalyst。
The device of above-mentioned a kind of dichloroacetic acid selectivity dechlorination, it is characterised in that: the internal diameter of described hydrogenation tower is 0.8m~1.0m, and the height of described hydrogenation tower is 6m~8m, and described catalyst is palladium carbon catalyst。
The device of above-mentioned a kind of dichloroacetic acid selectivity dechlorination, it is characterised in that: on the pipeline between described magnetic force driving pump and the feeding mouth of air and liquid mixer, N2On pipeline between gas outlet and the feeding mouth of air and liquid mixer of storage tank, H2On pipeline between gas outlet and the feeding mouth of air and liquid mixer of storage tank, on pipeline between discharging opening and the charging aperture of the first reactor of air and liquid mixer, on pipeline between discharging opening and the charging aperture of the second reactor of air and liquid mixer, on pipeline between discharging opening and the charging aperture of gas-liquid separator of the first reactor, on pipeline between discharging opening and the charging aperture of gas-liquid separator of the second reactor, on pipeline between discharging opening and the charging aperture of the second reactor of the first reactor, on pipeline between gas material outlet and the charging aperture on absorption tower, on pipeline between discharging opening and the hydrochloric acid collecting tank on absorption tower, on pipeline between liquid material outlet and the charging aperture of distillation column, and the pipeline between the discharging opening of distillation column and chloroacetic acid collecting tank is provided with valve。
The device of above-mentioned a kind of dichloroacetic acid selectivity dechlorination, it is characterised in that: all it is wound with electric-heating belt outside described pipeline。
This utility model compared with prior art has the advantage that
1, this utility model simple in construction, novel in design reasonable, it is achieved convenient, practical, result of use is good, it is simple to promote。
2, this utility model have developed a kind of device suitable in dichloroacetic acid selective hydrogenation dechlorination, and this apparatus structure is simple, reasonable in design, simple to operate, it is adaptable to dichloroacetic acid selective hydrogenation dechlorination, and hydrogenation efficiency is high。
3, this utility model efficiently solves in traditional dichloroacetic acid selectivity dechlorination process, and equipment is complicated, automaticity is low, treatment effeciency is low, the problem that ingredient requirement is high。
4, all pipelines in this utility model adopt electric-heating belt to be wound around, and install simple, safe and reliable, easy to maintenance, have good pipe insulation and antifreezing effect。It is the chlorated liquid of severe corrosive due to what carry in the pipeline of dichloroacetic acid selective hydrogenation dechlorination apparatus, store, and the temperature of steam tracing easily fluctuates, easily cause local material overheated, tubing local corrosion seriously can be caused to penetrate, affect normal operation to produce, so processing for the preferred electric tracing of pipeline。
5, this utility model can avoid when regulating manually of complexity, it is only necessary to control piper and valve can realize the parallel/serial of two reactors and arbitrarily convert, simple to operate, and treatment effeciency is high, practical。
6, the parallel/serial of two reactors of this utility model is arranged, and is possible not only to improve hydrogenation effect, it may also be used for overhaul of the equipments switching reactor, when can also be used for expanding the scale of production parallel connection produce。
Below by drawings and Examples, the technical solution of the utility model is described in further detail。
Accompanying drawing explanation
Fig. 1 is structural representation of the present utility model。
Description of reference numerals:
1 material liquid storage tank;2 N2Storage tank;3 H2Storage tank;
4 air and liquid mixers;5-1 the first reactor;5-2 the second reactor;
6 gas-liquid separators;7 absorption towers;8 distillation column;
9 hydrochloric acid collecting tanks;10 chloroacetic acid collecting tanks;11 magnetic force driving pumps;
12 valves。
Detailed description of the invention
As it is shown in figure 1, the device of this utility model dichloroacetic acid selectivity dechlorination includes material liquid storage tank 1, N2Storage tank 2, H2Storage tank 3, air and liquid mixer 4, reactor, gas-liquid separator 6, absorption tower 7 and distillation column 8, described reactor includes the first reactor 5-1 and the second reactor 5-2, the discharging opening of described material liquid storage tank 1, N2The gas outlet of storage tank 2 and H2The gas outlet of storage tank 3 is connected each through the feeding mouth of pipeline with air and liquid mixer 4, the discharging opening of described air and liquid mixer 4 is connected with the charging aperture of the charging aperture of the first reactor 5-1 and the second reactor 5-2 respectively by pipeline, the discharging opening of described first reactor 5-1 is connected with the charging aperture of the charging aperture of gas-liquid separator 6 and the second reactor 5-2 respectively by pipeline, the discharging opening of described second reactor 5-2 is connected with the charging aperture of gas-liquid separator 6 by pipeline, the discharging opening of described gas-liquid separator 6 includes liquid material outlet and gas material outlet, the outlet of described gas material is connected by the charging aperture of pipeline with absorption tower 7, the discharging opening on described absorption tower 7 is connected with hydrochloric acid collecting tank 9 by pipeline, the outlet of described liquid material is connected by the charging aperture of pipeline with distillation column 8, the discharging opening of described distillation column 8 is connected with chloroacetic acid collecting tank 10 by pipeline。
As it is shown in figure 1, be connected to magnetic force driving pump 11 also by pipeline between the discharging opening of described material liquid storage tank 1 and the feeding mouth of air and liquid mixer 4。
In the present embodiment, described first reactor 5-1 and the second reactor 5-2 is the hydrogenation tower being filled with catalyst。Preferably, the internal diameter of described hydrogenation tower is 0.8m~1.0m, and the height of described hydrogenation tower is 6m~8m, and described catalyst is palladium carbon catalyst。
As it is shown in figure 1, on pipeline between described magnetic force driving pump 11 and the feeding mouth of air and liquid mixer 4, N2On pipeline between gas outlet and the feeding mouth of air and liquid mixer 4 of storage tank 2, H2On pipeline between gas outlet and the feeding mouth of air and liquid mixer 4 of storage tank 3, on pipeline between discharging opening and the charging aperture of the first reactor 5-1 of air and liquid mixer 4, on pipeline between discharging opening and the charging aperture of the second reactor 5-2 of air and liquid mixer 4, on pipeline between discharging opening and the charging aperture of gas-liquid separator 6 of the first reactor 5-1, on pipeline between discharging opening and the charging aperture of gas-liquid separator 6 of the second reactor 5-2, on pipeline between discharging opening and the charging aperture of the second reactor 5-2 of the first reactor 5-1, on pipeline between gas material outlet and the charging aperture on absorption tower 7, on pipeline between discharging opening and the hydrochloric acid collecting tank 9 on absorption tower 7, on pipeline between liquid material outlet and the charging aperture of distillation column 8, and the pipeline between the discharging opening of distillation column 8 and chloroacetic acid collecting tank 10 is provided with valve 12。
In the present embodiment, described pipeline is outer, and (that is: the pipeline between discharging opening and the feeding mouth of air and liquid mixer 4 of material liquid storage tank 1 is outer, N2Pipeline between gas outlet and the feeding mouth of air and liquid mixer 4 of storage tank 2 is outer, H2Outside pipeline between gas outlet and the feeding mouth of air and liquid mixer 4 of storage tank 3, outside pipeline between discharging opening and the charging aperture of the first reactor 5-1 of air and liquid mixer 4, outside pipeline between discharging opening and the charging aperture of the second reactor 5-2 of air and liquid mixer 4, outside pipeline between discharging opening and the charging aperture of gas-liquid separator 6 of the first reactor 5-1, outside pipeline between discharging opening and the charging aperture of gas-liquid separator 6 of the second reactor 5-2, outside pipeline between discharging opening and the charging aperture of the second reactor 5-2 of the first reactor 5-1, outside pipeline between gas material outlet and the charging aperture on absorption tower 7, outside pipeline between discharging opening and the hydrochloric acid collecting tank 9 on absorption tower 7, pipeline outside pipeline between liquid material outlet and the charging aperture of distillation column 8 and between discharging opening and the chloroacetic acid collecting tank 10 of distillation column 8 is outer) all it is wound with electric-heating belt。
In conjunction with Fig. 1, this utility model realizes the method for dichloroacetic acid selectivity dechlorination and comprises the steps:
1st step, adds the mixed type chlorated liquid containing dichloroacetic acid, chloroacetic acid and acetic acid obtained through chloridization process in material liquid storage tank 1 as material liquid;
In actually used process, adopt steam-heated mode that material liquid storage tank 1 is heated, make the heating material in material liquid storage tank 1 to design temperature and be incubated;
2nd step, squeezes in air and liquid mixer 4 by the material liquid of heating and thermal insulation by magnetic force driving pump 11, mixes with hydrogen and nitrogen;
3rd step, enters in reactor and carries out selective hydrogenation dechlorination reaction, make the dichloroacetic acid in material liquid be converted into chloroacetic acid;In selective hydrogenation dechlorination reaction process, by regulating the valve on pipeline, it is possible to make two reactors realize used in parallel, series connection and use, or when reactor be maintenance, Out of order, another reactor is used alone;
4th step, reacted product enters in gas-liquid separator 6 and carries out gas-liquid separation, liquid product enters in distillation column 8 and carries out product purification, finally in chloroacetic acid collecting tank 10, obtain chloroacetic acid (target product), gas-phase product enters the absorption carrying out hydrogen chloride in absorption tower 7, finally obtaining hydrochloric acid (by-product) in hydrochloric acid collecting tank 9, after absorption tower 7 absorbs, remaining hydrogen is delivered to the emptying of Factory Building overhead。
In sum, this utility model have developed a kind of device suitable in dichloroacetic acid selective hydrogenation dechlorination, and this device efficiently solves equipment complexity in traditional dichloroacetic acid selectivity dechlorination process, automaticity is low, treatment effeciency is low, the problem that ingredient requirement is high。In this utility model, the parallel/serial of two reactors is arranged, and is possible not only to improve hydrogenation effect, it may also be used for overhaul of the equipments switching reactor, when can also be used for expanding the scale of production parallel connection produce。This utility model simple in construction, reasonable in design, simple to operate, it is adaptable to dichloroacetic acid selective hydrogenation dechlorination, hydrogenation efficiency is high。
The above; it it is only preferred embodiment of the present utility model; not this utility model is imposed any restrictions; every any simple modification, change and equivalent structure change above example made according to this utility model technical spirit, all still falls within the protection domain of technical solutions of the utility model。
Claims (6)
1. the device of a dichloroacetic acid selectivity dechlorination, it is characterised in that: include material liquid storage tank (1), N2Storage tank (2), H2Storage tank (3), air and liquid mixer (4), reactor, gas-liquid separator (6), absorption tower (7) and distillation column (8), described reactor includes the first reactor (5-1) and the second reactor (5-2), the discharging opening of described material liquid storage tank (1), N2The gas outlet of storage tank (2) and H2The gas outlet of storage tank (3) is connected each through the feeding mouth of pipeline with air and liquid mixer (4), the discharging opening of described air and liquid mixer (4) is connected with the charging aperture of the charging aperture of the first reactor (5-1) and the second reactor (5-2) respectively by pipeline, the discharging opening of described first reactor (5-1) is connected with the charging aperture of the charging aperture of gas-liquid separator (6) and the second reactor (5-2) respectively by pipeline, the discharging opening of described second reactor (5-2) is connected with the charging aperture of gas-liquid separator (6) by pipeline, the discharging opening of described gas-liquid separator (6) includes liquid material outlet and gas material outlet, the outlet of described gas material is connected by the charging aperture of pipeline with absorption tower (7), the discharging opening on described absorption tower (7) is connected with hydrochloric acid collecting tank (9) by pipeline, the outlet of described liquid material is connected by the charging aperture of pipeline with distillation column (8), the discharging opening of described distillation column (8) is connected with chloroacetic acid collecting tank (10) by pipeline。
2. the device of a kind of dichloroacetic acid selectivity dechlorination according to claim 1, it is characterised in that: it is connected to magnetic force driving pump (11) also by pipeline between discharging opening and the feeding mouth of air and liquid mixer (4) of described material liquid storage tank (1)。
3. the device of a kind of dichloroacetic acid selectivity dechlorination according to claim 1, it is characterised in that: described first reactor (5-1) and the second reactor (5-2) are the hydrogenation tower being filled with catalyst。
4. the device of a kind of dichloroacetic acid selectivity dechlorination according to claim 3, it is characterised in that: the internal diameter of described hydrogenation tower is 0.8m~1.0m, and the height of described hydrogenation tower is 6m~8m, and described catalyst is palladium carbon catalyst。
5. the device of a kind of dichloroacetic acid selectivity dechlorination according to claim 2, it is characterised in that: on the pipeline between the feeding mouth of described magnetic force driving pump (11) and air and liquid mixer (4), N2On pipeline between gas outlet and the feeding mouth of air and liquid mixer (4) of storage tank (2), H2On pipeline between gas outlet and the feeding mouth of air and liquid mixer (4) of storage tank (3), on pipeline between discharging opening and the charging aperture of the first reactor (5-1) of air and liquid mixer (4), on pipeline between discharging opening and the charging aperture of the second reactor (5-2) of air and liquid mixer (4), on pipeline between discharging opening and the charging aperture of gas-liquid separator (6) of the first reactor (5-1), on pipeline between discharging opening and the charging aperture of gas-liquid separator (6) of the second reactor (5-2), on pipeline between discharging opening and the charging aperture of the second reactor (5-2) of the first reactor (5-1), on pipeline between gas material outlet and the charging aperture of absorption tower (7), on pipeline between discharging opening and the hydrochloric acid collecting tank (9) on absorption tower (7), on pipeline between liquid material outlet and the charging aperture of distillation column (8), and the pipeline between the discharging opening of distillation column (8) and chloroacetic acid collecting tank (10) is provided with valve (12)。
6. the device of a kind of dichloroacetic acid selectivity dechlorination according to claim 1, it is characterised in that: all it is wound with electric-heating belt outside described pipeline。
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110314618A (en) * | 2019-08-14 | 2019-10-11 | 凯莱英医药集团(天津)股份有限公司 | Sectional integral type solid catalysis continuous reaction apparatus and continuous reaction system |
WO2021026821A1 (en) * | 2019-08-14 | 2021-02-18 | 凯莱英医药集团(天津)股份有限公司 | Segmentable integrated solid catalytic continuous reaction apparatus and continuous reaction system |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110314618A (en) * | 2019-08-14 | 2019-10-11 | 凯莱英医药集团(天津)股份有限公司 | Sectional integral type solid catalysis continuous reaction apparatus and continuous reaction system |
WO2021026821A1 (en) * | 2019-08-14 | 2021-02-18 | 凯莱英医药集团(天津)股份有限公司 | Segmentable integrated solid catalytic continuous reaction apparatus and continuous reaction system |
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