CN107224745B - Quinol solution's system for separating and purifying and method - Google Patents
Quinol solution's system for separating and purifying and method Download PDFInfo
- Publication number
- CN107224745B CN107224745B CN201710579964.XA CN201710579964A CN107224745B CN 107224745 B CN107224745 B CN 107224745B CN 201710579964 A CN201710579964 A CN 201710579964A CN 107224745 B CN107224745 B CN 107224745B
- Authority
- CN
- China
- Prior art keywords
- hydroquinone
- water
- kettle
- condenser
- distillation still
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/02—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in boilers or stills
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/10—Vacuum distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/42—Regulation; Control
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
- C07C37/74—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses the system for separating and purifying of quinol solution a kind of, kettle is collected including distillation still, hydroquinone, distilled water collects kettle, oil condenser, fuel tank, the first water condenser and the second water condenser, feed inlet, air inlet, steam outlet valve and hydroquinone steam outlet valve are provided at the top of the distillation still, quinol solution enters in distillation still from the feed inlet, and the vapor steamed is condensed into distilled water through second water condenser from distillation still outflow and collects in kettle into the distilled water；The hydroquinone gas steamed is condensed into liquid through the oil condenser from distillation still outflow and collects in kettle into the hydroquinone；Oil condenser, fuel tank and first water condenser, which form a cooling oil circuit piping cooling oil flowed in circulation line, to be cooled down, the first water condenser and the shared water cooling system of the second water condenser.A kind of method using the system separating-purifying hydroquinone is also disclosed, the method distilled using two sections.
Description
Technical field
The present invention relates to hydroquinone recovery processings, purification technique field, and in particular to a kind of quinol solution's separation
Purification system and method.
Background technique
When traditional aniline process production hydroquinone, (" long-used soup " is commonly called as) after technical grade solution circulation concentration 2 times, generation
Solution contains the inorganic salts impurity such as more ammonium sulfate, sodium carbonate, as recycled the hydroquinone quality generated after condensing crystallizing
It is decreased obviously, quality criteria requirements is much not achieved.Return oxidation operation is generally taken in industrial production, is made as aniline raw material
With the method business efficiency is not high, the normal productive capacity for not only consuming a large amount of energy, reducing equipment, and reduces production
Direct yield.
Summary of the invention
It is an object of the invention in view of the above-mentioned problems, provide it is a kind of it is safe, at low cost, photographic-grade finished product pair can be obtained
The system and method for resorcinol solution separation, purification.
The technical scheme adopted by the invention to solve the technical problem:
A kind of system for separating and purifying of quinol solution, including distillation still, hydroquinone collect kettle, distilled water is collected
Kettle, oil condenser, fuel tank, the first water condenser and the second water condenser, the distillation still top are provided with feed inlet, air inlet
Mouth, steam outlet valve and hydroquinone steam outlet valve, quinol solution enter in distillation still from the feed inlet, steam
Vapor flowed out from distillation still and be condensed into through second water condenser distilled water and collected in kettle into the distilled water；It steams
Hydroquinone gas flowed out from distillation still and be condensed into through the oil condenser liquid and collected in kettle into the hydroquinone；Oil
Condenser, fuel tank and first water condenser form a cooling oil circuit piping and cooling oil are flowed in circulation line
It is cooled down, the first water condenser and the second water condenser share a water cooling system.
In the above-mentioned technical solutions, the system for separating and purifying further includes vacuum pump, distillation water collecting tank, and hydroquinone is received
Collection kettle, distilled water are collected kettle and are connect respectively with the vacuum pump, and vacuum pump is also connected with distillation water collecting tank.When having collected to benzene two
After phenol finished product, water being passed through from feed inlet, system pipeline being cleaned, kettle and steaming are then collected to hydroquinone using vacuum pump
Distilled water collects kettle and carries out vacuumizing further cleaning respectively, collects moisture remaining in kettle by vacuum pump and enters distilled water collection
In tank.
Inert gas is passed through in the air inlet.It is passed through inert gas in systems before distilling hydroquinone, prevents pair
Benzenediol steam contacts generation with air and dodges quick-fried (it is 156 DEG C that hydroquinone, which dodges burst point), although whole system is closed operation,
No-spark generates, and guarantees the safe operation of system.
The temperature of the oil condenser is controlled at 200~230 DEG C, can be condensed to 287 DEG C of hydroquinone gas.
It is provided with steam condensate (SC) visor on connecting the pipeline that the second water condenser and distilled water collect kettle, can be observed
Whether the moisture in the solution containing hydroquinone evaporates.
Hydroquinone condensate liquid visor, Ke Yiguan are provided on the pipeline that connection oil condenser and hydroquinone collect kettle
Examine whether the hydroquinone in the solution of hydroquinone evaporates.
A kind of quinol solution's process for separation and purification is divided using above-mentioned quinol solution's system for separating and purifying
From purification, include the following steps:
1) solution containing hydroquinone is passed through from feed inlet distillation still, opens distillation still stirring, opens water vapour
Outlet valve closes hydroquinone steam outlet valve, opens the cooling water system that the first water condenser and the second water condenser are formed,
It is distilled using two sections, first segment first distills out the water in solution, and the heating temperature for controlling distillation still is 100 ± 2 DEG C, control distillation
Negative pressure in kettle is in -0.1~-0.2kpa, and vapor flows into the second water condenser from distillation still and is cooled to liquid water, in turn
Distilled water is flowed into collect in kettle；
2) after the moisture in solution is evaporated, second segment distillation is carried out, is first passed through inert gas full of steaming from air inlet
Kettle is evaporated, hydroquinone steam outlet valve is opened, closes steam outlet valve, then controls the temperature of distillation still 287~290
DEG C, oil condenser is opened, controls the temperature of oil condenser at 200~230 DEG C, hydroquinone collection kettle is opened and stirs, in solution
Hydroquinone be evaporated to gas flow into oil condenser in be condensed into liquid enter hydroquinone collect kettle in；
3) after having collected hydroquinone condensate liquid, system is closed, hydroquinone is collected into the material in kettle and is discharged, is obtained pair
Benzenediol product.
The raw material separated, purified can be the quinol solution of 0~99.9% content, be also possible to impurity content not
Qualified solid hydroquinone.
The method of the present invention first takes the water in the solution containing hydroquinone or finished product, semi-finished product at 100 ± 2 DEG C
The method of negative pressure evaporation is separated with impurity such as hydroquinone, inorganic salts；Its secondary control reheating temperature at 289 ± 1 DEG C, because
For hydroquinone boiling point at 287 DEG C, and other inorganic salts boiling points are much larger than this temperature, therefore other inorganic salts quilts in solution
It is retained in slag, hydroquinone is distillated purification；It is passed through nitrogen in system, is that hydroquinone steam is contacted with air in order to prevent
Occur to dodge quick-fried (being 156 DEG C because it dodges burst point), it is contemplated that the safe operation of system is (although the system of haveing suffered is closed operation, and nothing
Spark generates).
The beneficial effects of the present invention are: the system and method are safe and reliable, energy consumption consumption is small, at low cost, it can be from aniline
In various solution, finished product, semi-finished product in the aftertreatment technology of method production hydroquinone, separating-purifying obtains quality etc. pair
Benzenediol finished product, product direct yield are high, hence it is evident that have saved resource and production cost, especially overturned aniline process processing " long-used soup "
The conventional method of solution, while the purification for the more solid hydroquinone of impurity has found new method.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of quinol solution's system for separating and purifying of the invention.
Specific embodiment
Below with reference to embodiment, the invention will be further described, but not thereby limiting the invention.
Embodiment 1 constructs quinol solution's system for separating and purifying
One kind system for separating and purifying containing quinol solution as shown in Figure 1 is constructed, mainly by distillation still 1, hydroquinone
Collect kettle 2, distilled water collects kettle 3, oil condenser 4, fuel tank 5, the first water condenser 6, the second water condenser 7, vacuum pump 8, steams
Distilled water collecting tank 9, steam outlet valve 10 and hydroquinone steam outlet valve 11 form.Feed inlet is provided at the top of distillation still 1
1a, air inlet 1b, steam outlet valve 10 and hydroquinone steam outlet valve 11, quinol solution enter steaming from feed inlet 1a
It evaporates in kettle 1, the vapor steamed is condensed into steaming by steam outlet valve 10, the second water condenser 7 of arrival from the outflow of distillation still 1
Distilled water enters distilled water and collects in kettle 3, and the hydroquinone gas steamed is from the outflow of distillation still 1 by hydroquinone steam outlet valve
11, arrival oil condenser 4 is condensed into liquid and enters in hydroquinone collection kettle 2, oil condenser 4, fuel tank 5 and the first water condenser
6 one cooling oil circuit piping of formation flow cooling oil in circulation line to be cooled down, the first water condenser 6 and second
Water condenser 7 shares a water cooling system, and hydroquinone collects kettle 2, distilled water is collected kettle 3 and connect respectively with vacuum pump 8, very
Sky pump 8 is also connected with distillation water collecting tank 9.It is provided with steam outlet valve 10 in distillation still 1, connect the second water condenser 7 and steams
Steam condensate (SC) visor is provided on the pipeline of distilled water collection kettle 3.Hydroquinone steam outlet valve 11 is provided in distillation still 1,
Hydroquinone condensate liquid visor is provided on the pipeline of connection oil condenser 4 and hydroquinone collection kettle 2.Distillation still 1 is using electricity
Conduction oil mode is added to provide heat source, temperature control range is 10~310 DEG C.
2 separating-purifying quinol solution of embodiment
The solution containing hydroquinone is separated using quinol solution's system for separating and purifying that embodiment 1 constructs
Purification, this method mainly use two sections of distillation techniques, and first segment is first will be in solution under 100 ± 2 DEG C of vapo(u)rizing temperature
Moisture is evaporated, and second segment is to steam the hydroquinone in solution under 289 ± 1 DEG C of vapo(u)rizing temperature after moisture is evaporated
It issues and is collected.Specifically operate in accordance with the following steps:
1) solution containing hydroquinone 3~50% is passed through from feed inlet 1a distillation still 1 (amount per treatment be no more than
The 80% of 1 volume of distillation still), steam outlet valve 10 is opened, hydroquinone steam outlet valve 11 is closed, distillation still 1 is opened and stirs
It mixes, distillation still 1 provides heat source using electricity plus conduction oil mode, and first segment first distills out the water in solution, and control distillation still 1 adds
Hot temperature is 100 ± 2 DEG C, opens the cooling water system that the first water condenser 6 and the second water condenser 7 are formed, and opens vacuum system
System controls the negative pressure in whole system in -0.1~-0.2kpa, notices that controlling cooling water outlet temperature is not greater than 45 DEG C.Water
Steam flows into the second water condenser 7 from distillation still 1 and is cooled to liquid water, and then flows into distilled water and collect in kettle 3.
2) steam condensate (SC) visor is observed, when not having condensed water outflow in visor, opens hydroquinone steam outlet valve
11, the steam outlet valve 10 on reaction kettle is closed, inert gas (such as nitrogen) is passed through from air inlet 1b and is full of whole system,
Second segment distillation is carried out, the temperature of distillation still 1 is controlled 289 ± 1 DEG C (cannot be below 287 DEG C), opens oil condenser 4, control
The temperature of oil condenser 4 opens hydroquinone and collects the stirring of kettle 2, the hydroquinone in solution is evaporated at 200~230 DEG C
It is condensed into liquid in gas inflow oil condenser 4 to enter in hydroquinone collection kettle 2, pays attention to observing hydroquinone condensate liquid view
Mirror.
3) when there is no condensate liquid to pass through in hydroquinone condensate liquid visor, stop heating after five minutes, when temperature is reduced to
At 150 DEG C, the blow valve that hydroquinone collects kettle 2 is opened, stops vacuum system, hydroquinone is collected into the material in kettle and is arranged
Out, quality etc. hydroquinone photographic-grade finished product is obtained.
4) when the temperature for heating distillation still 1 is down to room temperature, tap water cleaning system is put into from feed inlet 1a and is prepared to enter into
It produces next time, ejected wash water enters oxidation operation, and the salt impurity in water, by leaching material open circuit, does not enter to benzene together with oxidation solution
The processes such as reduction, the crystallization of diphenol.
Claims (6)
1. a kind of quinol solution's process for separation and purification, it is characterised in that: using quinol solution's system for separating and purifying into
Row separating-purifying, quinol solution's system for separating and purifying include distillation still (1), hydroquinone collection kettle (2), distillation
Water collects kettle (3), oil condenser (4), fuel tank (5), the first water condenser (6) and the second water condenser (7), the distillation still
(1) top is provided with feed inlet (1a), air inlet (1b), steam outlet valve (10) and hydroquinone steam outlet valve (11),
Quinol solution enters in distillation still (1) from the feed inlet (1a), and the vapor steamed is from described in distillation still (1) outflow warp
Second water condenser (7) is condensed into distilled water and collects in kettle (3) into the distilled water；The hydroquinone gas steamed is from distillation
Kettle (1) outflow is condensed into liquid through the oil condenser (4) and collects in kettle (2) into the hydroquinone；Oil condenser (4),
Fuel tank (5) and first water condenser (6) form a cooling oil circuit piping and cooling oil are flowed in circulation line
It is cooled down, the first water condenser (6) and the second water condenser (7) share a water cooling system；
Process for separation and purification includes the following steps:
1) solution containing hydroquinone is passed through from feed inlet (1a) distillation still (1), opens distillation still (1) stirring, opens
Steam outlet valve (10) is closed hydroquinone steam outlet valve (11), and the first water condenser (6) and the second water condenser are opened
(7) cooling water system formed is distilled using two sections, and first segment first distills out the water in solution, controls the heating of distillation still (1)
Temperature is 100 ± 2 DEG C, and for the negative pressure in control distillation still (1) in -0.1~-0.2kpa, vapor flows into the from distillation still (1)
Two water condensers (7) are cooled to liquid water, and then flow into distilled water and collect in kettle (3)；
2) after the moisture in solution is evaporated, second segment distillation is carried out, is first passed through inert gas full of steaming from air inlet (1b)
It evaporates kettle (1), opens hydroquinone steam outlet valve (11), close steam outlet valve (10), then control the temperature of distillation still (1)
Degree is opened oil condenser (4) at 287~290 DEG C, is controlled the temperature of oil condenser (4) at 200~230 DEG C, is opened hydroquinone
Kettle (2) stirring is collected, the hydroquinone in solution is evaporated to be condensed into liquid entrance pair in gas inflow oil condenser (4)
Benzenediol is collected in kettle (2)；
3) after having collected hydroquinone condensate liquid, system is closed, hydroquinone is collected into the material in kettle (2) and is discharged, is obtained pair
Benzenediol product.
2. quinol solution's process for separation and purification as described in claim 1, it is characterised in that: the quinol solution point
It further include vacuum pump (8), distillation water collecting tank (9) from purification system, hydroquinone collects kettle (2), distilled water collects kettle (3) point
It is not connect with the vacuum pump (8), vacuum pump (8) is also connected with distillation water collecting tank (9).
3. quinol solution's process for separation and purification as claimed in claim 1 or 2, it is characterised in that: the hydroquinone is molten
Inert gas is passed through in the air inlet (1b) of liquid system for separating and purifying.
4. quinol solution's process for separation and purification as claimed in claim 1 or 2, it is characterised in that: the hydroquinone is molten
The temperature of the oil condenser (4) of liquid system for separating and purifying is controlled at 200~230 DEG C.
5. quinol solution's process for separation and purification as claimed in claim 1 or 2, it is characterised in that: the hydroquinone is molten
In liquid system for separating and purifying, steam condensation is provided on the pipeline that kettle (3) are collected in connection the second water condenser (7) and distilled water
Water visor.
6. quinol solution's process for separation and purification as claimed in claim 1 or 2, it is characterised in that: the hydroquinone is molten
In liquid system for separating and purifying, to be provided with hydroquinone cold on the pipeline of connection oil condenser (4) and hydroquinone collection kettle (2)
Lime set visor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710579964.XA CN107224745B (en) | 2017-07-17 | 2017-07-17 | Quinol solution's system for separating and purifying and method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710579964.XA CN107224745B (en) | 2017-07-17 | 2017-07-17 | Quinol solution's system for separating and purifying and method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107224745A CN107224745A (en) | 2017-10-03 |
| CN107224745B true CN107224745B (en) | 2019-05-24 |
Family
ID=59956479
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710579964.XA Active CN107224745B (en) | 2017-07-17 | 2017-07-17 | Quinol solution's system for separating and purifying and method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107224745B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110665246B (en) * | 2019-10-21 | 2021-12-07 | 江苏利田科技股份有限公司 | Device and method for removing and recovering toluene solvent in UV (ultraviolet) photocuring monomer solution |
| CN111013174A (en) * | 2019-12-31 | 2020-04-17 | 上海兆维科技发展有限公司 | Vacuum system and control method thereof |
| CN115364499A (en) * | 2022-08-16 | 2022-11-22 | 重庆上甲电子股份有限公司 | Hydroquinone production system and process capable of recycling steam |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101479224A (en) * | 2006-06-29 | 2009-07-08 | 罗地亚管理公司 | Method for preparing purified hydroquinone and forming same |
| CN207016689U (en) * | 2017-07-17 | 2018-02-16 | 重庆上甲电子股份有限公司 | Quinol solution's system for separating and purifying |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2903100B1 (en) * | 2006-06-29 | 2012-08-03 | Rhodia Recherches & Tech | PROCESS FOR PREPARING PURIFIED HYDROQUINONE |
-
2017
- 2017-07-17 CN CN201710579964.XA patent/CN107224745B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101479224A (en) * | 2006-06-29 | 2009-07-08 | 罗地亚管理公司 | Method for preparing purified hydroquinone and forming same |
| CN207016689U (en) * | 2017-07-17 | 2018-02-16 | 重庆上甲电子股份有限公司 | Quinol solution's system for separating and purifying |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107224745A (en) | 2017-10-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106379920B (en) | Lithium chloride sodium chloride mixed aqueous solution evaporation analysis sodium produces the device and method of pure lithium chloride solution | |
| CN107224745B (en) | Quinol solution's system for separating and purifying and method | |
| CN108715456B (en) | Method for recycling electrode foil corrosion waste nitric acid | |
| CN106673961B (en) | The methanol aqueous solution of sodium chloride evaporates recovery process | |
| CN104817481A (en) | Technological method for recovering DMSO from DMSO aqueous solution | |
| CN105174290A (en) | Separation process of potassium salt and sodium salt in concentrated brine | |
| CN102020389A (en) | Process for recycling ammonium chloride waste water | |
| CN109200610A (en) | A kind of sulphuric acid concentration system | |
| CN110451596A (en) | A kind of carrier gas extraction HPE vapo(u)rization system | |
| WO2024041327A1 (en) | Energy-saving treatment system and process for salt-containing and heavy metal-containing ammonia-nitrogen wastewater | |
| CN211245558U (en) | Glycerol concentration system | |
| CN209507643U (en) | A kind of waste liquid recovery apparatus | |
| US20230398466A1 (en) | Separation tower and method for treating condensed water | |
| CN207734624U (en) | A kind of multi-way concentration purifying plant | |
| CN207016689U (en) | Quinol solution's system for separating and purifying | |
| CN208097833U (en) | Rolled film distillation equipment and the membrane distillation system for using it | |
| CN108996523B (en) | Separation and purification system for desulfurization wastewater | |
| CN114949893B (en) | Evaporation crystallization process and device for producing lithium chloride from salt lake brine | |
| CN110294665A (en) | The recyclable device and recovery method of ethyl alcohol in Doxycycline Hyclate refinement mother liquor | |
| CN107854857A (en) | A kind of multi-way concentration purifying plant and its application method | |
| CN209809543U (en) | Seven-effect tube type falling film evaporator set | |
| CN209456107U (en) | A kind of sea water desulfuration thermal power plant tail end wastewater processing system | |
| CN206172995U (en) | Device that pure lithium chloride solution was prepared to sodium is analysed in evaporation of lithium chloride sodium chloride mixing water solution | |
| CN208649420U (en) | A kind of chlorination mentions the recovery and processing system of germanium and hydrochloric acid in germanium spent acid | |
| CN109534425A (en) | A kind of sea water desulfuration thermal power plant tail end wastewater processing system and method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information |
Inventor after: Ma Juncai Inventor after: Li Shuchun Inventor after: Fu Jing Inventor after: Liao Xinren Inventor before: Ma Juncai Inventor before: Li Shuchun Inventor before: Fu Jing Inventor before: Liao Xinren |
|
| CB03 | Change of inventor or designer information | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |