CN102516062B - Hydrolysis outer circulation heat exchange process and device for friedel-crafts reaction liquid for synthesis of ibuprofen - Google Patents
Hydrolysis outer circulation heat exchange process and device for friedel-crafts reaction liquid for synthesis of ibuprofen Download PDFInfo
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- 238000005727 Friedel-Crafts reaction Methods 0.000 title claims abstract description 74
- 239000012295 chemical reaction liquid Substances 0.000 title claims abstract description 72
- 238000000034 method Methods 0.000 title claims abstract description 61
- 230000007062 hydrolysis Effects 0.000 title claims abstract description 27
- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 27
- HEFNNWSXXWATRW-UHFFFAOYSA-N Ibuprofen Chemical compound CC(C)CC1=CC=C(C(C)C(O)=O)C=C1 HEFNNWSXXWATRW-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229960001680 ibuprofen Drugs 0.000 title claims abstract description 19
- 230000015572 biosynthetic process Effects 0.000 title abstract 2
- 238000003786 synthesis reaction Methods 0.000 title abstract 2
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 230000003301 hydrolyzing effect Effects 0.000 claims description 106
- 238000000354 decomposition reaction Methods 0.000 claims description 76
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 51
- 230000002631 hypothermal effect Effects 0.000 claims description 51
- 239000011780 sodium chloride Substances 0.000 claims description 51
- 238000001816 cooling Methods 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 4
- 230000007797 corrosion Effects 0.000 abstract description 8
- 238000005260 corrosion Methods 0.000 abstract description 8
- 238000012423 maintenance Methods 0.000 abstract description 5
- 239000012530 fluid Substances 0.000 description 11
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 230000002950 deficient Effects 0.000 description 3
- 238000007086 side reaction Methods 0.000 description 3
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 description 2
- WETWJCDKMRHUPV-UHFFFAOYSA-N acetyl chloride Chemical compound CC(Cl)=O WETWJCDKMRHUPV-UHFFFAOYSA-N 0.000 description 2
- 239000012346 acetyl chloride Substances 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 230000000202 analgesic effect Effects 0.000 description 2
- 230000001754 anti-pyretic effect Effects 0.000 description 2
- 239000002221 antipyretic Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000004886 process control Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- WRJZDDJYWWJLIS-UHFFFAOYSA-N 4-methyl-1-phenylpentan-1-one Chemical compound CC(C)CCC(=O)C1=CC=CC=C1 WRJZDDJYWWJLIS-UHFFFAOYSA-N 0.000 description 1
- 238000003476 Darzens condensation reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- KXUHSQYYJYAXGZ-UHFFFAOYSA-N isobutylbenzene Chemical compound CC(C)CC1=CC=CC=C1 KXUHSQYYJYAXGZ-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000000041 non-steroidal anti-inflammatory agent Substances 0.000 description 1
- 229940021182 non-steroidal anti-inflammatory drug Drugs 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000002923 oximes Chemical class 0.000 description 1
- VODRWDBLLGYRJT-UHFFFAOYSA-N propan-2-yl 2-chloroacetate Chemical compound CC(C)OC(=O)CCl VODRWDBLLGYRJT-UHFFFAOYSA-N 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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Abstract
The invention relates to a hydrolysis outer circulation heat exchange process and a hydrolysis outer circulation heat exchange device for a friedel-crafts reaction liquid for synthesis of ibuprofen. In the process, the temperature in the hydrolysis process of the friedel-crafts reaction liquid is controlled by an outer circulation heat exchange process, so the friedel-crafts reaction liquid can be hydrolyzed smoothly, the reaction temperature in the hydrolysis process can be controlled stably, the heat transfer efficiency can be improved, maintenance cost of equipment is reduced, and the problem of unqualified product caused by corrosion and leakage can be avoided.
Description
Technical field
The invention belongs to pharmaceutical technology field, be specifically related to synthetic Friedel-Crafts reaction liquid hydrolysis external circulation heat exchanging technique and the device used of a kind of Ibuprofen BP/EP.
Background technology
Ibuprofen BP/EP is one of current antipyretic and analgesic three large pillar products, first synthetic in 1964 by Nicholson, and in the later stage eighties 20th century, the appearance of carboxylated method and 1,2-transposition method technique significantly improves its industrial scale.Because Ibuprofen BP/EP is a kind of non-steroid antiinflammatory drug, there is the curative effects such as stronger anti-inflammatory analgesic, antipyretic, rheumatism, and toxicity is low, is developed rapidly in recent years.Although there are various new Ibuprofen BP/EP production technique, but due to the restriction of the conditions such as yield, equipment, the three wastes, safety, in domestic industry, produce Ibuprofen BP/EP at present and mainly adopt glycidic ester method, that is: Isobuytel Benzene and Acetyl Chloride 98Min. make isobutyl acetophenone through Friedel-Crafts reaction, then carry out Darzens condensation with isopropyl chloracetate, through basic hydrolysis, acid neutralization, decarboxylic reaction, make isobutyl-benzene propionic aldehyde again, then through oxidation or the hydrolysis of one-tenth oxime, make Ibuprofen BP/EP.In this technological process, the temperature control of the hydrolytic process of Friedel-Crafts reaction liquid is comparatively crucial.
Existing Friedel-Crafts reaction process is: sherwood oil, aluminum chloride are joined in retort according to certain ratio, by mixing control temperature, be no more than 5 ℃, under the condition of overtemperature not, add the Isobuytel Benzene of metering, then add the Acetyl Chloride 98Min. of desired number, continue to stir and react within 4 hours, to make Friedel-Crafts reaction liquid.
The hydrolytic process of Friedel-Crafts reaction liquid is: in hydrolytic decomposition pot, configure the hydrochloric acid of pH=3, by Friedel-Crafts reaction liquid being transported in hydrolytic decomposition pot intermittently, be hydrolyzed about 3 hours keeping in tank in the situation that temperature being no more than 15 ℃.After hydrolysis, enter subsequent processing and wash.Because excess Temperature can cause the generation of side reaction, therefore the hydrolysis of Friedel-Crafts reaction liquid need to complete under cold condition, but temperature is too low, easily produces crystallization, causes line clogging.The control condition of industrial hydrolytic process is: adopt the heat exchange mode of inner coil pipe, coil pipe is titanium material, passes into hypothermic saline in coil pipe; 35 cubes ms/h of hypothermic saline consumptions, hydrolysis time is about 3 hours, and hypothermic saline inflow temperature is-17 ℃, and leaving water temperature(LWT) is-12 ℃.During current industrial Friedel-Crafts reaction liquid hydrolysis, can there is following problem: what adopt due to the hydrolytic decomposition pot of Friedel-Crafts reaction liquid is that inner coil pipe interchanger carries out heat exchange, Friedel-Crafts reaction liquid heat exchanger has very strong corrodibility, often occur that built-in titanium coil pipe part damages because of corrosion, Friedel-Crafts reaction liquid is mixed with hypothermic saline, thereby polluted the hypothermic saline of whole factory, make Friedel-Crafts reaction liquid also be polluted, quality product is defective simultaneously.On the other hand, the titanium pipe that interchanger adopts involves great expense, and maintenance cost is very high, and frequent replacing meeting causes very large economical load to workshop, makes production cost high, has reduced economic benefit.From heat transfer angle, the heat transfer efficiency of the heat exchange mode of built-in titanium coil pipe is lower, has limited the raising of hydrolytic process throughput.
Summary of the invention
The present invention has overcome the deficiencies in the prior art, Ibuprofen BP/EP has been proposed synthetic with Friedel-Crafts reaction liquid hydrolysis external circulation heat exchanging technique and device, described technical process adopts the temperature in outer circulation type heat-exchanging process control Friedel-Crafts reaction liquid hydrolytic process, realize Friedel-Crafts reaction liquid and complete smoothly hydrolytic process, stablize the temperature of reaction of controlled hydrolysis process, improve heat transfer efficiency, reduce the maintenance cost of equipment, avoid corrosion to reveal the underproof problem of product causing.
Technical scheme of the present invention is: a kind of Ibuprofen BP/EP is synthetic with Friedel-Crafts reaction liquid hydrolysis external circulation heat exchanger, comprise central control unit, hydrolytic decomposition pot, interchanger combination, recycle pump, on the top of described hydrolytic decomposition pot, be provided with control device and feed entrance, the inside of described hydrolytic decomposition pot is provided with whipping appts, the bottom of described hydrolytic decomposition pot is provided with reaction solution outlet, described central control unit is connected with control device by signal wire, described central control unit is connected with recycle pump with interchanger combination respectively by signal wire, the reaction solution outlet of described hydrolytic decomposition pot is connected with recycle pump by pipeline, described heat exchanger package is combined into two interchanger that are cascaded by pipeline, described interchanger combination is connected with recycle pump by pipeline, the reaction solution entrance of described hydrolytic decomposition pot is connected with interchanger combination by pipeline.
Interchanger combination is provided with heat exchanger entrance sensor assembly and heat exchanger exit sensor assembly, and described interchanger is the corrosion-resistant materials such as graphite or tetrafluoroethylene, and its form is shell and tube heat exchanger.
In the bottom sides of described hydrolytic decomposition pot, be provided with hydrolytic decomposition pot sensor assembly.
A kind of Ibuprofen BP/EP is synthetic utilizes hydrolytic decomposition pot, interchanger, recycle pump equipment to be hydrolyzed by Friedel-Crafts reaction liquid hydrolysis external circulation heat exchanging technique, and concrete hydrolysis process flow process is:
1) hydrochloric acid that configures pH=3 in hydrolytic decomposition pot is as hydrolyzed solution;
2) open imported valve and the outlet valve of the hypothermic saline (cold general facilities) of interchanger;
3) start the be hydrolyzed cooling of liquid of recycle pump, the inlet temperature of hypothermic saline is-17 ℃～-5 ℃, and the temperature out of hypothermic saline is-12 ℃～0 ℃;
4) Friedel-Crafts reaction liquid is transported in hydrolytic decomposition pot continuously, under the control of Controlling System, keeps in tank 0～10 ℃ of temperature;
5) repeating step 4, is hydrolyzed 1～3 hour;
6) close recycle pump, close hypothermic saline imported valve and the outlet valve of interchanger, be hydrolyzed completely, complete liquid and enter subsequent processing and wash.
For the 4th step, Friedel-Crafts reaction liquid adopts continuously feeding mode, avoids intermittent feeding to cause in reacting liquid temperature fluctuation and hydrolytic decomposition pot local temperature of charge too high.
For the 5th step, keeping the inlet temperature of hypothermic saline is-17 ℃～-5 ℃, and the temperature out of hypothermic saline is-12 ℃～0 ℃, and flow is 5 tons/hour～70 tons/hour.
For the 5th step, after the outer circulation of interchanger composition is cooling, the temperature that turns back to hydrolytic decomposition pot is controlled at 5 ℃～10 ℃, and the outer circulation amount of Friedel-Crafts reaction liquid is 10 tons/hour～90 tons/hour.
For the 6th step, to the processing power of Friedel-Crafts reaction liquid, be 0.5 ton/hour～5 tons/hour, the operating time is 1 hour～4 hours.
Principle of the present invention is:
The hydrolysis of Friedel-Crafts reaction liquid is a thermopositive reaction, in hydrolytic process, liberated heat shifts out reaction system by external circulation heat exchanging device E01 and E02, by controlling the flow of hypothermic saline and the feed rate of Friedel-Crafts reaction liquid, the temperature in control Friedel-Crafts reaction liquid hydrolytic process is in the scope of defined.The flow of water at low temperature and temperature in have very significantly impact to the operation of technological process, in use, if the flow of hypothermic saline increases, the temperature out of hydrolyzed solution reduces, be easy to cause the ctystallizing point lower than hydrolyzed solution, thereby cause interchanger to stop up; If the flow of hypothermic saline reduces, the temperature out of hydrolyzed solution increases, and is easy to can not cause the cooling task of hydrolytic decomposition pot, and the interior fluid temperature of hydrolytic decomposition pot is raise, and side reaction increases, thereby causes quality product defective.In like manner, also there is so impact in the temperature in of hypothermic saline.So the flow of hypothermic saline and temperature in should obtain strict control, the present invention controls automatically to the temperature out of hydrolyzed solution, makes the fluid temperature in hydrolytic decomposition pot in hydrolytic process be stabilized in required scope.Thereby reacting liquid temperature fluctuation and issuable local temperature is too high improves the quality of products in the hydrolytic decomposition pot simultaneously producing for fear of intermittent feeding, the present invention adopts continuously feeding mode that Friedel-Crafts reaction liquid is transported in hydrolytic decomposition pot.Accurate for reaching temperature control, the object of raising heat transfer efficiency, interchanger is selected the materials such as anti-low temperature, corrosion resistant graphite and tetrafluoroethylene.
The present invention has following beneficial effect:
1) technical process of the present invention adopts the temperature in outer circulation type heat-exchanging process control Friedel-Crafts reaction liquid hydrolytic process, realize Friedel-Crafts reaction liquid and complete smoothly hydrolytic process, stablize the temperature of reaction of controlled hydrolysis process, improve heat transfer efficiency, the maintenance cost of reduction equipment, avoids corrosion to reveal the underproof problem of product causing.
2) the present invention can steady running, there will not be corrosion to reveal the very high problem of cost that the product causing is defective or the frequent maintenance of equipment causes.
3) the present invention reduces the needed operating time when processing identical Friedel-Crafts reaction liquid, and efficiency improves.
4) Friedel-Crafts reaction liquid of the present invention adopts continuously feeding mode, avoids intermittent feeding to cause in reacting liquid temperature fluctuation and hydrolytic decomposition pot local temperature of charge too high, has reduced the generation of side reaction, is conducive to improve the purity of product.
Accompanying drawing explanation
Accompanying drawing is structural representation of the present invention.
In figure, 1, central control unit; 2, interchanger combination; 3, recycle pump; 4, heat exchanger exit sensor assembly; 5, hydrolytic decomposition pot; 6, control device; 7, whipping appts; 8, hydrolytic decomposition pot sensor assembly; 9, feed entrance; 10, reaction solution outlet; 11, reaction solution entrance; 12, heat exchanger entrance sensor assembly.
Embodiment
A kind of Ibuprofen BP/EP is synthetic with Friedel-Crafts reaction liquid hydrolysis external circulation heat exchanger, comprise central control unit 1, hydrolytic decomposition pot 5, interchanger combination 2, recycle pump 3, on the top of described hydrolytic decomposition pot 5, be provided with control device 6 and feed entrance 9, the inside of described hydrolytic decomposition pot 5 is provided with whipping appts 7, the bottom of described hydrolytic decomposition pot 5 is provided with reaction solution outlet 10, described central control unit 1 is connected with control device 6 by signal wire, described central control unit 1 is connected with recycle pump 3 with interchanger combination 2 respectively by signal wire, the reaction solution outlet 10 of described hydrolytic decomposition pot 5 is connected with recycle pump 3 by pipeline, two interchanger of described interchanger combination 2 for being cascaded by pipeline, described interchanger combination 2 is connected with recycle pump 3 by pipeline, the reaction solution entrance 11 of described hydrolytic decomposition pot 5 is connected with interchanger combination 2 by pipeline.Interchanger combination 2 is provided with heat exchanger entrance sensor assembly 12 and heat exchanger exit sensor assembly 4, and described interchanger is the corrosion-resistant materials such as graphite or tetrafluoroethylene, and its form is shell and tube heat exchanger.In the bottom sides of described hydrolytic decomposition pot 5, be provided with hydrolytic decomposition pot sensor assembly 8.Central control unit 1 is connected with interchanger combination 2 by signal wire, the control device 6 of hydrolytic decomposition pot 5 is connected by mechanical mechanism with whipping appts 7, central control unit 1 can be controlled the control device of hydrolytic decomposition pot 5, and central control unit 1 can be controlled recycle pump 3 and interchanger combination 2 by signal wire.Heat exchanger exit sensor assembly 4 comprises pressure transmitter, temperature sensor and flow sensor.Hydrolytic decomposition pot sensor assembly 8 comprises pressure transmitter, temperature sensor and flow sensor.Heat exchanger entrance sensor assembly 12 comprises pressure transmitter, temperature sensor and flow sensor.
First in hydrolytic decomposition pot, add a certain amount of hydrolyzed solution, then start recycle pump hydrolyzed solution is carried out to circulating cooling by external heat exchanger, the heat-eliminating medium of interchanger is hypothermic saline.After hydrolyzed solution in hydrolytic decomposition pot is cooled to 0 ℃～10 ℃ scopes, opens Friedel-Crafts reaction liquid feed valve and carry out continuously feeding.By controlling the flow of hypothermic saline and the input speed of Friedel-Crafts reaction liquid, make the temperature-stable of hydrolytic decomposition pot in whole hydrolytic process at 0 ℃～10 ℃.
Below embodiment of the present invention:
Embodiment 1: first add the hydrolyzed solution of 1.5 tons in hydrolytic decomposition pot, then start recycle pump hydrolyzed solution is carried out to circulating cooling by external heat exchanger, the flow of circulation fluid is 45 tons/hour.The heat-eliminating medium of interchanger is hypothermic saline, and the temperature in of hypothermic saline is-17 ℃, and temperature out is-12 ℃, and flow is 20 tons/hour.Hydrolyzed solution in hydrolytic decomposition pot is cooled to after 5 ℃, opens Friedel-Crafts reaction liquid feed valve and carries out continuously feeding.By controlling the flow of hypothermic saline and the input speed of Friedel-Crafts reaction liquid, make the temperature-stable of hydrolytic decomposition pot in whole hydrolytic process at 0 ℃～10 ℃.Whole hydrolytic process completed in 2 hours, and the total amount of handled Friedel-Crafts reaction liquid is 2 tons.Device steady running, the problems such as corrosion-free, leakage, obstruction occur.
Embodiment 2: first add the hydrolyzed solution of 3 tons in hydrolytic decomposition pot, then start recycle pump hydrolyzed solution is carried out to circulating cooling by external heat exchanger, the flow of circulation fluid is 55 tons/hour.The heat-eliminating medium of interchanger is hypothermic saline, and the temperature in of hypothermic saline is-12 ℃, and temperature out is-6 ℃, and flow is 20 tons/hour.Hydrolyzed solution in hydrolytic decomposition pot is cooled to after 8 ℃, opens Friedel-Crafts reaction liquid feed valve and carries out continuously feeding.By controlling the flow of hypothermic saline and the input speed of Friedel-Crafts reaction liquid, make the temperature-stable of hydrolytic decomposition pot in whole hydrolytic process at 0 ℃～10 ℃.Whole hydrolytic process completed in 3 hours, and the total amount of handled Friedel-Crafts reaction liquid is 4 tons.Device steady running, the problems such as corrosion-free, leakage, obstruction occur.
Embodiment 3: first add the hydrolyzed solution of 0.5 ton in hydrolytic decomposition pot, then start recycle pump hydrolyzed solution is carried out to circulating cooling by external heat exchanger, the flow of circulation fluid is 30 tons/hour.The heat-eliminating medium of interchanger is hypothermic saline, and the temperature in of hypothermic saline is-10 ℃, and temperature out is-5 ℃, and flow is 12 tons/hour.Hydrolyzed solution in hydrolytic decomposition pot is cooled to after 2 ℃, opens Friedel-Crafts reaction liquid feed valve and carries out continuously feeding.By controlling the flow of hypothermic saline and the input speed of Friedel-Crafts reaction liquid, make the temperature-stable of hydrolytic decomposition pot in whole hydrolytic process at 0 ℃～10 ℃.Whole hydrolytic process completed in 1 hour, and the total amount of handled Friedel-Crafts reaction liquid is 0.7 ton.Device steady running, the problems such as corrosion-free, leakage, obstruction occur.
Embodiment 4: first add the hydrolyzed solution of 1 ton in hydrolytic decomposition pot, then start recycle pump hydrolyzed solution is carried out to circulating cooling by external heat exchanger, the flow of circulation fluid is 55 tons/hour.The heat-eliminating medium of interchanger is hypothermic saline, and the temperature in of hypothermic saline is-10 ℃, and temperature out is-5 ℃, and flow is 20 tons/hour.Hydrolyzed solution in hydrolytic decomposition pot is cooled to after 0 ℃, opens Friedel-Crafts reaction liquid feed valve and carries out continuously feeding.By controlling the flow of hypothermic saline and the input speed of Friedel-Crafts reaction liquid, make the temperature-stable of hydrolytic decomposition pot in whole hydrolytic process at 0 ℃～10 ℃.Whole hydrolytic process completed in 1.5 hours, and the total amount of handled Friedel-Crafts reaction liquid is 1.3 tons.Device steady running, the problems such as corrosion-free, leakage, obstruction occur.
Embodiment 5: first add the hydrolyzed solution of 2.0 tons in hydrolytic decomposition pot, then start recycle pump hydrolyzed solution is carried out to circulating cooling by external heat exchanger, the flow of circulation fluid is 45 tons/hour.The heat-eliminating medium of interchanger is hypothermic saline, and the temperature in of hypothermic saline is-17 ℃, and temperature out is-12 ℃, and flow is 30 tons/hour.Hydrolyzed solution in hydrolytic decomposition pot is cooled to after 6 ℃, opens Friedel-Crafts reaction liquid feed valve and carries out continuously feeding.By controlling the flow of hypothermic saline and the input speed of Friedel-Crafts reaction liquid, make the temperature-stable of hydrolytic decomposition pot in whole hydrolytic process at 0 ℃～10 ℃.Whole hydrolytic process completed in 2 hours, and the total amount of handled Friedel-Crafts reaction liquid is 2.7 tons.Device steady running, the problems such as corrosion-free, leakage, obstruction occur.
Embodiment 6: first add the hydrolyzed solution of 2.5 tons in hydrolytic decomposition pot, then start recycle pump hydrolyzed solution is carried out to circulating cooling by external heat exchanger, the flow of circulation fluid is 30 tons/hour.The heat-eliminating medium of interchanger is hypothermic saline, and the temperature in of hypothermic saline is-10 ℃, and temperature out is-5 ℃, and flow is 20 tons/hour.Hydrolyzed solution in hydrolytic decomposition pot is cooled to after 5 ℃, opens Friedel-Crafts reaction liquid feed valve and carries out continuously feeding.By controlling the flow of hypothermic saline and the input speed of Friedel-Crafts reaction liquid, make the temperature-stable of hydrolytic decomposition pot in whole hydrolytic process at 0 ℃～10 ℃.Whole hydrolytic process completed in 3.5 hours, and the total amount of handled Friedel-Crafts reaction liquid is 3.3 tons.Device steady running, the problems such as corrosion-free, leakage, obstruction occur.
Embodiment 7: first add the hydrolyzed solution of 3.8 tons in hydrolytic decomposition pot, then start recycle pump hydrolyzed solution is carried out to circulating cooling by external heat exchanger, the flow of circulation fluid is 65 tons/hour.The heat-eliminating medium of interchanger is hypothermic saline, and the temperature in of hypothermic saline is-9 ℃, and temperature out is-4 ℃, and flow is 40 tons/hour.Hydrolyzed solution in hydrolytic decomposition pot is cooled to after 4 ℃, opens Friedel-Crafts reaction liquid feed valve and carries out continuously feeding.By controlling the flow of hypothermic saline and the input speed of Friedel-Crafts reaction liquid, make the temperature-stable of hydrolytic decomposition pot in whole hydrolytic process at 0 ℃～10 ℃.Whole hydrolytic process completed in 2.5 hours, and the total amount of handled Friedel-Crafts reaction liquid is 5 tons.Device steady running, the problems such as corrosion-free, leakage, obstruction occur.
Embodiment 8: first add the hydrolyzed solution of 4.5 tons in hydrolytic decomposition pot, then start recycle pump hydrolyzed solution is carried out to circulating cooling by external heat exchanger, the flow of circulation fluid is 70 tons/hour.The heat-eliminating medium of interchanger is hypothermic saline, and the temperature in of hypothermic saline is-17 ℃, and temperature out is-12 ℃, and flow is 60 tons/hour.Hydrolyzed solution in hydrolytic decomposition pot is cooled to after 1 ℃, opens Friedel-Crafts reaction liquid feed valve and carries out continuously feeding.By controlling the flow of hypothermic saline and the input speed of Friedel-Crafts reaction liquid, make the temperature-stable of hydrolytic decomposition pot in whole hydrolytic process at 0 ℃～10 ℃.Whole hydrolytic process completed in 2 hours, and the total amount of handled Friedel-Crafts reaction liquid is 6 tons.Device steady running, the problems such as corrosion-free, leakage, obstruction occur.
Embodiment 9: first add the hydrolyzed solution of 6.0 tons in hydrolytic decomposition pot, then start recycle pump hydrolyzed solution is carried out to circulating cooling by external heat exchanger, the flow of circulation fluid is 45 tons/hour.The heat-eliminating medium of interchanger is hypothermic saline, and the temperature in of hypothermic saline is-15 ℃, and temperature out is-10 ℃, and flow is 60 tons/hour.Hydrolyzed solution in hydrolytic decomposition pot is cooled to after 0 ℃, opens Friedel-Crafts reaction liquid feed valve and carries out continuously feeding.By controlling the flow of hypothermic saline and the input speed of Friedel-Crafts reaction liquid, make the temperature-stable of hydrolytic decomposition pot in whole hydrolytic process at 0 ℃～10 ℃.Whole hydrolytic process completed in 3 hours, and the total amount of handled Friedel-Crafts reaction liquid is 8 tons.Device steady running, the problems such as corrosion-free, leakage, obstruction occur.
Claims (5)
1. an Ibuprofen BP/EP is synthetic with Friedel-Crafts reaction liquid hydrolysis external circulation heat exchanger, it is characterized in that: comprise central control unit, hydrolytic decomposition pot, interchanger combination, recycle pump, on the top of described hydrolytic decomposition pot, be provided with control device and feed entrance, the inside of described hydrolytic decomposition pot is provided with whipping appts, the bottom of described hydrolytic decomposition pot is provided with reaction solution outlet, described central control unit is connected with control device by signal wire, described central control unit is connected with recycle pump with interchanger combination respectively by signal wire, the reaction solution outlet of described hydrolytic decomposition pot is connected with recycle pump by pipeline, described heat exchanger package is combined into two interchanger that are cascaded by pipeline, described interchanger combination is connected with recycle pump by pipeline, the reaction solution entrance of described hydrolytic decomposition pot is connected with interchanger combination by pipeline,
Wherein interchanger combination is provided with heat exchanger entrance sensor assembly and heat exchanger exit sensor assembly, and described interchanger is shell and tube heat exchanger, and its material is graphite or tetrafluoroethylene;
And be provided with hydrolytic decomposition pot sensor assembly in the bottom sides of described hydrolytic decomposition pot.
2. right to use requires described in 1 that Ibuprofen BP/EP is synthetic carries out the synthetic technique that is hydrolyzed external circulation heat exchanging with Friedel-Crafts reaction liquid of Ibuprofen BP/EP with Friedel-Crafts reaction liquid hydrolysis external circulation heat exchanger, and the hydrolysis process flow process of this technique is:
1) hydrochloric acid that configures pH=3 in hydrolytic decomposition pot is as hydrolyzed solution;
2) open imported valve and the outlet valve of the hypothermic saline of interchanger;
3) start the be hydrolyzed cooling of liquid of recycle pump, the inlet temperature of hypothermic saline is-17 ℃～-5 ℃, and the temperature out of hypothermic saline is-12 ℃～0 ℃;
4) Friedel-Crafts reaction liquid is transported in hydrolytic decomposition pot continuously, under the control of Controlling System, keeps in tank 0～10 ℃ of temperature;
5) repeating step 4, is hydrolyzed 1～3 hour;
6) close recycle pump, close hypothermic saline imported valve and the outlet valve of interchanger, be hydrolyzed complete.
3. Ibuprofen BP/EP according to claim 2 is synthetic by Friedel-Crafts reaction liquid hydrolysis external circulation heat exchanging technique, it is characterized in that: for the 5th step, keeping the inlet temperature of hypothermic saline is-17 ℃～-5 ℃, and the temperature out of hypothermic saline is-12 ℃～0 ℃, and flow is 5～70 tons/hour.
4. Ibuprofen BP/EP according to claim 2 is synthetic by Friedel-Crafts reaction liquid hydrolysis external circulation heat exchanging technique, it is characterized in that: for the 5th step, beyond Friedel-Crafts reaction liquid, Recycle design is after interchanger is cooling, the temperature that turns back to hydrolytic decomposition pot is controlled at 5 ℃～10 ℃, and outer circulation amount is 10 tons/hour～90 tons/hour.
5. Ibuprofen BP/EP according to claim 2 is synthetic by Friedel-Crafts reaction liquid hydrolysis external circulation heat exchanging technique, it is characterized in that: for the 6th step, to the processing power of Friedel-Crafts reaction liquid, be 0.5 ton/hour～5 tons/hour, the operating time is 1 hour～4 hours.
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| CN101456808A (en) * | 2009-01-06 | 2009-06-17 | 长沙理工大学 | Method for preparing ibuprofen |
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