CN103880622B - A kind of brufen process units and technique - Google Patents
A kind of brufen process units and technique Download PDFInfo
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- CN103880622B CN103880622B CN201210552749.8A CN201210552749A CN103880622B CN 103880622 B CN103880622 B CN 103880622B CN 201210552749 A CN201210552749 A CN 201210552749A CN 103880622 B CN103880622 B CN 103880622B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/45—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by condensation
- C07C45/46—Friedel-Crafts reactions
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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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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to device and technique that a kind of brufen produces.For current brufen produce present in problem, develop a kind of external circulation process technology of high efficient heat exchanging in brufen produces, the material after Friedel-Crafts reaction is enable to carry out effectively hydrolyzing, improve purity and the yield of intermediate, and reduce in hydrolytic process the corrosion to equipment, thus reduce production cost.The technical process of the present invention is as follows: Friedel-Crafts reaction terminates, material puts into Fu Ke hydrolytic decomposition pot from Friedel-Crafts reaction tank, by adjusting the aperture of blowing regulation valve, control the reaction temperature in Fu Ke hydrolytic decomposition pot, hydrolysis liquid in Fu Ke hydrolytic decomposition pot throws outer circulation condenser into by dnockout pump, goes out the aperture of water regulating valve at external control hydrolysising reacting temperature by controlling chilled water inlet regulating valve and chilled water.After hydrolysis completes, material enters chlorine ketone water washing tank, and reclaims solvent therein by chlorine ketone recycling can.
Description
Technical field
The invention belongs to chemical field, particularly to a kind of brufen process units and technique.
Background technology
Friedel-Crafts reaction is the first step reaction during brufen produces, mainly by isobutylbenzene with chloro-propanoyl chloride is at alchlor
Catalysis under the chemical reaction that carries out, it is chlorine ketone that reaction produces thing, contain excessive chloro-propanoyl chloride and alchlor simultaneously, because of
This second step needs to hydrolyze by alchlor and chloro-propanoyl chloride.Friedel-Crafts reaction is it is generally required to strict temperature control, because warm
Spending height and can cause the generation of accessory substance, temperature is too low, causes reaction not exclusively, and easily produces crystallization and block pipeline.Existing
During having technique Friedel-Crafts reaction liquid to be hydrolyzed, use during in hydrolytic decomposition pot, built-in titanium coil heat exchanger is hydrolyzed
Temperature controls, and this technique exists following defect: 1, due to the severe corrosive of reactant liquor, the row of reactant liquor heat exchanger often occur
The corrosion of pipe, makes material mix with chilled brine, thus pollutes the chilled brine of whole factory, makes Friedel-Crafts reaction simultaneously
Liquid is also polluted;2, the titanium tube heat exchanger somewhat expensive used, frequent replacing can cause the biggest burden to workshop;3, adopt
The total heat transfer efficiency carrying out heat exchange with built-in titanium coil pipe is relatively low, limits production capacity;4, batch (-type) blowing, material exists continuously
Heat up cooling process, cause quality of material poor, impurity content height, intermediate yield is low.Therefore, needing exploitation one badly can
Solve the problems referred to above and realize the technology of high efficient heat exchanging in brufen produces.
Summary of the invention
The present invention is aiming at problem present in the production of above-mentioned brufen, and exploitation is a kind of efficiently changes in brufen produces
The external circulation process technology of heat, enables the material after Friedel-Crafts reaction to carry out effectively hydrolyzing, improves purity and the yield of intermediate,
And reduce in hydrolytic process the corrosion to equipment, thus reduce production cost.
A kind of brufen process units, Friedel-Crafts reaction tank connects Fu Ke hydrolytic decomposition pot, Fu Ke hydrolytic decomposition pot and outer circulation condenser
Connecting into peripheral passage, be connected dnockout pump between Fu Ke hydrolytic decomposition pot with outer circulation condenser, Fu Ke hydrolytic decomposition pot is also connected with chlorine ketone water
Cleaning of evaporator, chlorine ketone hydrolytic decomposition pot is connected with chlorine ketone recycling can;Blowing regulation valve is set between Friedel-Crafts reaction tank and Fu Ke hydrolytic decomposition pot, follows outward
The import and export of ring condenser is provided with chilled water inlet regulating valve and chilled water goes out water regulating valve.
Temperature indicator is had, it is achieved the temperature measuring of hydrolysis liquid and reality in Fu Ke hydrolytic decomposition pot on described Fu Ke hydrolytic decomposition pot
Time display.
Described Fu Ke hydrolytic decomposition pot is provided with agitating device, makes Friedel-Crafts reaction liquid can be sufficiently mixed uniformly.
Described outer circulation condenser is composed in series by two heat exchangers, preferably graphite or teflon heat exchanger.
A kind of brufen production technology, Friedel-Crafts reaction liquid is hydrolyzed and uses outer circulation type heat-exchanging process, and process is as follows: Fu
Gram reaction terminates, and material puts into Fu Ke hydrolytic decomposition pot from Friedel-Crafts reaction tank, by adjusting the aperture of blowing regulation valve, controls Fu Keshui
Solving the reaction temperature in tank, the hydrolysis liquid in Fu Ke hydrolytic decomposition pot throws outer circulation condenser into by dnockout pump, by controlling
Chilled water inlet regulating valve and chilled water go out the aperture of water regulating valve at external control hydrolysising reacting temperature.
Before described Friedel-Crafts reaction liquid enters Fu Ke hydrolytic decomposition pot, hydrolyzate temperature in Fu Ke hydrolytic decomposition pot is controlled at 8~10 DEG C.
Reaction temperature in described Fu Ke hydrolytic decomposition pot is 12~18 DEG C.
It is 15m by blowing governor valve control Friedel-Crafts reaction liquid dispensing speed3/h。
Being chosen as of runner in cycle condenser outside: the hydrolysis liquid flowed out in Fu Ke hydrolytic decomposition pot walks tube side, flow velocity
For 36.5t/h;Chilled brine walks shell side, and flow velocity is 43t/h.
In tube side, hydrolysis liquid temp is 12~18 DEG C.
In shell side, chilled water inlet temperature is-5 DEG C, and chilled water outlet temperature is 0 DEG C, i.e. the chilled water Inlet and outlet water temperature difference is constant
It it is 5 DEG C.
After hydrolysis completes, material enters chlorine ketone water washing tank, and reclaims solvent therein by chlorine ketone recycling can.
The design principle of present invention process is as follows:
1, in Fu Ke hydrolytic decomposition pot and the determination of hydrolysising reacting temperature in outer circulation condenser tube side:
As described in the background art, existing technique all completes the temperature to hydrolysis by built-in heat exchanger and controls, and does not has
There is the report utilizing outer loop.It has been investigated that after the main cause causing outer loop effectively not carry out is Friedel-Crafts reaction
Hydrolysis liquid crystallize at a certain temperature, thus block the tubulation of heat exchanger, cause heat exchange cannot be carried out.The most accurate
Measure the crystallization temperature of hydrolysis liquid, be by one of key point of outer loop design of heat exchanger.
Test method: Friedel-Crafts reaction drop entering temperature after in hydrolyzate and rises rapidly, after stopping dropping, temperature is down to 12
About DEG C, reduce rate of addition and continue dropping and maintain about 15 DEG C;During dropping, engender what profit was layered
Phenomenon, upper strata occurs that troubled liquor, lower floor are crocus oily, stands upon reaction completion, upper strata limpid yellowish lower floor
It it is then obvious crocus oily.
By hydrolysis liquid as in chilled brine, in flask, reacting liquid temperature is gradually lowered with external environment condition, in temperature
During less than 12 DEG C, liquid surface occurs crystallizing covering on a small quantity, when 11 DEG C bottom be with outside yellow oily liquid and crystallize out existing, be less than
Bottom when 9 DEG C, oily liquids fully charge becomes solid.
Freezing hydrolysis liquid is taken out, is placed in the middle of the environment of about 15 DEG C, it was observed that the bottom crystal when 8.7 DEG C
Periphery start thawing oily occur, more than 10 DEG C after a large amount of yellow oil occur, all melt to solid when 12.5 DEG C.
When temperature is more than 18 DEG C, side reaction occurs, and produces part accessory substance.
According to above-mentioned experimental result, the crystalline temperature of hydrolysis liquid is 12 DEG C, in order to effective precaution of hydrolysis reactant liquor exists
Heat exchanger intercrystalline causes heat exchanger to block, and the tube wall temperature that hydrolysis liquid contacts with heat exchanger should be tied more than hydrolyzate
Brilliant point 12 DEG C, and less than 15 DEG C, it is therefore desirable to heat exchanger strictly designs, and uses 2 40 graphite or polytetrafluoroethylene (PTFE)
Heat exchanger is used in series.
2, chilled water temperature and the determination of flow
Through multiple authentication, it is respectively adopted the deep cooling salt solution of-17 DEG C and the general salt solution of-5 DEG C as chilled water, according to along pipe
Temperature Distribution on sub-radial direction, and the temperature of hydrolysis liquid side is higher than crystalline temperature 12 DEG C and less than 18 DEG C, thus
Heat exchange can be made to be smoothed out.For the first time in process of the test, use the hypothermic saline of-17 DEG C, according to along pipe radial direction
Temperature Distribution, the temperature of hydrolysis liquid side is easily reduced below crystalline temperature, thus causes hydrolysis liquid at pipe
Inner side crystallization, and then blocking tube side.For the second time in process of the test, use the hypothermic saline of-5 DEG C, according to along pipe radial direction
On Temperature Distribution, the temperature of hydrolysis liquid side can control more than crystalline temperature, so that heat exchange is smoothed out.Simultaneously
The operation of technical process is had by the flow of chilled water and inlet temperature obviously to be affected.If chilled brine temperature mistake
Low, then the temperature of hydrolysis liquid side is easily reduced below crystalline temperature, and then blocking tube side;If circulating water flow mistake
Greatly, according to diabatic process principle, hydrolysis liquid outlet temperature reduces, still results in Crystallization Plugging.Chilled water according to regulation
With the heat exchanger of inlet temperature design, in use, if the flow of chilled water increases, then the outlet temperature of hydrolysis liquid
Degree reduces, it is easy to causes the crystalline temperature less than hydrolysis liquid, thus causes heat exchanger to block;If the flow of chilled water subtracts
Few, then the outlet temperature of hydrolysis liquid increases, it is easy to causes the cooling task not finishing hydrolytic decomposition pot, thus causes product matter
Measure defective.In like manner, the inlet temperature of chilled water there is also so impact.
So, the flow of chilled water and inlet temperature should obtain strict control, the therefore outlet to hydrolysis liquid
Temperature is automatically controlled, and controls chilled water inlet temperature and is-5 DEG C, and chilled water outlet temperature is 0 DEG C, i.e. chilled water turnover
Water temperature difference is constant is 5 DEG C, and hydrolysis liquid temp is 12~18 DEG C, and Friedel-Crafts reaction liquid dispensing speed is 15m3/h.According to Fu Ke
Temperature in hydrolytic decomposition pot controls other each parameter, and chilled water Inlet and outlet water valve is automatically adjusted.
The heat exchange of outer loop process calculates:
According to result of the test, if a batch materials completed hydrolytic process in 3 hours, then the thermic load of hydrolytic process is:
Wherein: Q exchanger heat load, W
WcThe mass flow of chilled water, kg/h
CpcThe specific heat capacity of-chilled water, kJ/kg DEG C
t1Chilled water inlet temperature, DEG C
t2-chilled water outlet temperature, DEG C
According to knowhow, in reactor, the temperature of hydrolysis liquid not can exceed that 18 DEG C, therefore T1 < 18 in below equation
DEG C, simultaneously in order to prevent the crystallization of material, the temperature of charge at heat exchanger exit have to be larger than 12 DEG C, i.e. T2 in figure > 12 DEG C.If
During meter calculates, it is stipulated that T1=17 DEG C, T2=13 DEG C, then the internal circulating load of hydrolysis liquid outer circulation is at least:
Wherein: Q exchanger heat load, W
WhThe mass flow of hydrolysis liquid, kg/s
CphThe specific heat capacity of hydrolysis liquid, kJ/kg DEG C
T1 hydrolysis liquid inlet temperature, DEG C
T2 hydrolysis liquid outlet temperature, DEG C
According to result of the test, the inlet temperature of chilled water is-5 DEG C, it is stipulated that outlet temperature is 0 DEG C, then the consumption of chilled water
For:
Heat exchanger simulation calculates:
According to the feature of hydrolysation process, the hydrolysis liquid of external circulation heat exchanging technique walks tube side, and chilled brine walks shell
Journey is more reasonable.
Using the heat exchanger of polytetrafluoroethylene (PTFE), the heat exchange to technical process is simulated calculating, and the major requirement of design is
Under conditions of ensureing the out temperature of hydrolysis liquid, it is ensured that the tube wall temperature contacted with hydrolysis liquid phase is more than 12 DEG C.
Result of calculation is as follows:
Table 1 outer circulation condenser parameters result of calculation
After using above-mentioned outer circulation condenser, can calculate and be distributed as along the thermal resistance on pipe radial direction:
Table 2 outer circulation condenser thermal resistance is distributed
Project | Thermal resistance percentage |
Shell side | 8.89% |
Tube wall | 83.35% |
Tube side | 7.76% |
According to thermal resistance distribution and then to calculate outer circulation condenser tube internal wall as follows with tube wall temperature:
Table 3 outer circulation condenser tube internal and external temperature
Project | Entrance | Outlet |
Hot fluid temperature | 17℃ | 13℃ |
Cooling fluid temperature | -5℃ | 0℃ |
Inside pipe wall temperature | 15.3℃ | 12.0℃ |
Tube wall temperature | -3.04℃ | 1.16℃ |
By adjusting further and analyzing, the tube wall temperature contacted with hydrolysis liquid phase is all higher than 12.0 DEG C, will not lead
Cause hydrolysis liquid, at pipe intercrystalline, meets technological requirement.
The hydrolysis external circulation process of the present invention, has removed the titanium coil pipe in hydrolytic decomposition pot, adds 1 circulation fluorine and moulds pump (general
Hydrolysis liquid squeezes into outer circulation condenser from Fu Ke hydrolytic decomposition pot) and 2 40m2Graphite or teflon heat exchanger series connection make
With, at a constant temperature, by the precise controlling to dispensing speed, make material consistent react, chilled water uses more just
Suitable general salt solution replaces deep cooling salt solution, is monitored the temperature of charge of turnover condenser, is automatically adjusted dispensing speed and turnover
Salt solution valve opening, it is ensured that condenser inner wall can the most quick and complete reaction do not tied by material.The project implementation process
In, in order to obtain the heat exchange of stability and high efficiency, the key issue that emphasis solves has:
(1) being sufficiently mixed of hydrolysis liquid in Fu Ke hydrolytic decomposition pot.
(2) temperature test of hydrolysis liquid and display in real time in Fu Ke hydrolytic decomposition pot.
(3) material of heat exchanger, specifications design.
Chilled water out temperature and the automatic precision control problem of flow.
The invention has the beneficial effects as follows:
(1) breach Friedel-Crafts reaction product hydrolysis in tradition brufen production process and can only pass through built-in heat exchanger control
The limitation of temperature, develops a kind of brand-new efficient external circulation heat exchanging technique.
(2) this process heat transfer efficiency is high, temperature control is effective, it is possible to promoting hydrolysis complete, the intermediate product of generation is pure
Degree is high, yield is high.
(3) alleviate the corrosion of hydrolysis liquid heat exchanger, it is to avoid the Friedel-Crafts reaction liquid caused because of equipment corrosion and
The mutual pollution of chilled water, reduces production cost.
(4) it is suitable for large-scale production.
Accompanying drawing explanation
Friedel-Crafts reaction liquid during Fig. 1 brufen of the present invention produces hydrolyzes external circulating device figure
1. Friedel-Crafts reaction tank, 2. Fu Ke hydrolytic decomposition pot, 3. dnockout pump, 4. outer circulation condenser a, 5. outer circulation condenser b, 6.
Chlorine ketone water washing tank, 7. chlorine ketone recycling can, 8. blowing regulation valve, 9. temperature indicator, 10. chilled water inlet regulating valve,Chilled water
Go out water regulating valve.
Detailed description of the invention
Below in conjunction with the accompanying drawings and the present invention is further described by specific embodiment, but be not intended to the present invention.
Use connected mode as shown in Figure 1: 2. 1. Friedel-Crafts reaction tank connect Fu Ke hydrolytic decomposition pot, and Fu Ke hydrolytic decomposition pot is 2. with outward
4. 5. cycle condenser b connect into peripheral passage with outer circulation condenser a, Fu Ke hydrolytic decomposition pot 2. with outer circulation condenser b 5. it
Between connect dnockout pump, 6. 2. Fu Ke hydrolytic decomposition pot be also connected with chlorine ketone water washing tank, and 7. 6. chlorine ketone hydrolytic decomposition pot be connected with chlorine ketone recycling can;Fu
Gram retort 1. and Fu Ke hydrolytic decomposition pot 2. between blowing regulation valve is set 8., the import and export of outer circulation condenser is provided with freezing
10. water inlet regulating valve goes out water regulating valve with chilled water
2. Fu Ke hydrolytic decomposition pot uses the mode of outer circulation to hydrolyze Friedel-Crafts reaction liquid, opens Fu Ke hydrolytic decomposition pot in advance and 2. stirs and outward
Cycle condenser a 4., outer circulation condenser b 5., chilled water go out, inlet regulating valve, perform fighting material pump 3. by Fu Ke hydrolytic decomposition pot 2. in
The hydrolyzate got ready is cooled to 8~10 DEG C.Open Friedel-Crafts reaction tank 1. bottom valve, open Fu Ke hydrolytic decomposition pot and 2. feed regulation valve 8. valve
Aperture 100%, adjusts Fu Ke hydrolytic decomposition pot 2. inlet valve valve opening 30% after adding Friedel-Crafts reaction liquid.Ensure outer circulation condenser
The material turnover temperature difference 2 DEG C adjusts chilled water valve opening above according to temperature changing trend.Fu Ke hydrolytic decomposition pot is 2. interior controls temperature
12~18 DEG C, in the range of 30%~50%, adjust Fu Ke hydrolytic decomposition pot 2. according to Fu Ke hydrolytic decomposition pot 2. interior temperature of charge variation tendency
Inlet valve valve opening.Friedel-Crafts reaction liquid is discharged as early as possible, after hydrolysis completes, close 4. outer circulation condenser a, 5. outer follow
Ring condenser b chilled water goes out, inlet regulating valve, puts material in outer circulation condenser and pipeline to 6. chlorine ketone water washing tank, 2. Fu
Static 30 minutes of material in gram hydrolytic decomposition pot, puts to same 6. chlorine ketone water washing tank.
Embodiment 1
In Fu Ke hydrolytic decomposition pot, add 8 tons of hydrolyzates, 10 tons of Friedel-Crafts reaction liquid in Friedel-Crafts reaction tank are joined Fu Keshui
Solving in tank, control chilled water inlet temperature and be-5 DEG C, outlet temperature is 0 DEG C, and chilled-water flow is 43.0t/h, hydrolysis liquid
Flow is 36.5t/h.This process hydrolysis is complete, and the intermediate product purity of generation is high, yield is high.Whole service process is good
Good, the problems such as the burn into damage of equipment, blocking do not occur.
Embodiment 2
In Fu Ke hydrolytic decomposition pot, add 10 tons of hydrolyzates, 13 tons of Friedel-Crafts reaction liquid in Friedel-Crafts reaction tank are joined Fu Keshui
Solving in tank, control chilled water inlet temperature and be-5 DEG C, outlet temperature is 0 DEG C, and chilled-water flow is 43.0t/h, hydrolysis liquid
Flow is 36.5t/h.This process hydrolysis is complete, and the intermediate product purity of generation is high, yield is high.Whole service process is good
Good, the problems such as the burn into damage of equipment, blocking do not occur.
Embodiment 4
In Fu Ke hydrolytic decomposition pot, add 15 tons of hydrolyzates, 19.5 tons of Friedel-Crafts reaction liquid in Friedel-Crafts reaction tank are joined Fu Ke
In hydrolytic decomposition pot, controlling chilled water inlet temperature and be-5 DEG C, outlet temperature is 0 DEG C, and chilled-water flow is 43.0t/h, hydrolysis
Flow quantity is 36.5t/h.This process hydrolysis is complete, and the intermediate product purity of generation is high, yield is high.Whole service process is good
Good, the problems such as the burn into damage of equipment, blocking do not occur.
Embodiment 5
In Fu Ke hydrolytic decomposition pot, add 20 tons of hydrolyzates, 26 tons of Friedel-Crafts reaction liquid in Friedel-Crafts reaction tank are joined Fu Keshui
Solving in tank, control chilled water inlet temperature and be-5 DEG C, outlet temperature is 0 DEG C, and chilled-water flow is 43.0t/h, hydrolysis liquid
Flow is 36.5t/h.This process hydrolysis is complete, and the intermediate product purity of generation is high, yield is high.Whole service process is good
Good, the problems such as the burn into damage of equipment, blocking do not occur.
Claims (5)
1. a brufen production technology, it is characterised in that Friedel-Crafts reaction liquid is hydrolyzed and uses outer circulation type heat-exchanging process, mistake
Journey is as follows: Friedel-Crafts reaction terminates, and material puts into Fu Ke hydrolytic decomposition pot from Friedel-Crafts reaction tank, by adjusting the aperture of blowing regulation valve,
Controlling the reaction temperature in Fu Ke hydrolytic decomposition pot, the hydrolysis liquid in Fu Ke hydrolytic decomposition pot is thrown outer circulation into by dnockout pump and is condensed
Device, goes out the aperture of water regulating valve at external control hydrolysising reacting temperature by controlling chilled water inlet regulating valve and chilled water, when
After hydrolysis completes, material enters chlorine ketone water washing tank, and reclaims solvent therein, wherein said Fu Ke by chlorine ketone recycling can
Reaction temperature in hydrolytic decomposition pot is 12~18 DEG C.
Brufen production technology the most according to claim 1, it is characterised in that described Friedel-Crafts reaction liquid enters Fu Ke hydrolytic decomposition pot
Before, hydrolyzate temperature in Fu Ke hydrolytic decomposition pot is controlled at 8~10 DEG C.
Brufen production technology the most according to claim 1, it is characterised in that described Friedel-Crafts reaction liquid dispensing speed is
15m3/h。
Brufen production technology the most according to claim 1, it is characterised in that the choosing of runner in described outer circulation condenser
It is selected as: the hydrolysis liquid flowed out in Fu Ke hydrolytic decomposition pot walks tube side, and flow velocity is 36.5t/h;Chilled brine walks shell side, and flow velocity is
43t/h。
Brufen production technology the most according to claim 4, it is characterised in that in described tube side, hydrolysis liquid temp is
12~18 DEG C;In shell side, chilled water inlet temperature is-5 DEG C, and chilled water outlet temperature is 0 DEG C, i.e. the chilled water Inlet and outlet water temperature difference is permanent
It is set to 5 DEG C.
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CN112882513B (en) * | 2021-01-15 | 2022-01-28 | 青岛科技大学 | Precise temperature control device and method suitable for ibuprofen Friedel-crafts reaction |
CN114085135B (en) * | 2021-10-29 | 2023-02-03 | 山东新华制药股份有限公司 | Continuous production method suitable for Friedel-crafts reaction of ibuprofen |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1082022A (en) * | 1992-08-14 | 1994-02-16 | 山东新华制药厂 | Molecular transposition prepares the technology of Ibuprofen BP/EP under the catalysis |
JP4334254B2 (en) * | 2002-06-03 | 2009-09-30 | 昭和電工株式会社 | Process for producing aromatic compounds by Friedel-Crafts reaction |
CN102516062A (en) * | 2011-12-02 | 2012-06-27 | 青岛科技大学 | Hydrolysis outer circulation heat exchange process and device for friedel-crafts reaction liquid for synthesis of ibuprofen |
-
2012
- 2012-12-19 CN CN201210552749.8A patent/CN103880622B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1082022A (en) * | 1992-08-14 | 1994-02-16 | 山东新华制药厂 | Molecular transposition prepares the technology of Ibuprofen BP/EP under the catalysis |
JP4334254B2 (en) * | 2002-06-03 | 2009-09-30 | 昭和電工株式会社 | Process for producing aromatic compounds by Friedel-Crafts reaction |
CN102516062A (en) * | 2011-12-02 | 2012-06-27 | 青岛科技大学 | Hydrolysis outer circulation heat exchange process and device for friedel-crafts reaction liquid for synthesis of ibuprofen |
Non-Patent Citations (1)
Title |
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布洛芬产品中重排工艺改进;舒瑞友;《齐鲁药事》;20061231;第25卷(第4期);第242-244页 * |
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