CN107224745A - Quinol solution's system for separating and purifying and method - Google Patents
Quinol solution's system for separating and purifying and method Download PDFInfo
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- CN107224745A CN107224745A CN201710579964.XA CN201710579964A CN107224745A CN 107224745 A CN107224745 A CN 107224745A CN 201710579964 A CN201710579964 A CN 201710579964A CN 107224745 A CN107224745 A CN 107224745A
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- hydroquinones
- water
- condenser
- kettle
- distillation still
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- 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
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- 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
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- 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
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- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of system for separating and purifying of quinol solution, kettle, distilled water, which are collected, including distillation still, hydroquinones collects kettle, oil condenser, fuel tank, the first water condenser and the second water condenser, charging aperture, air inlet, steam outlet valve and hydroquinones steam outlet valve are provided with the top of the distillation still, quinol solution from the charging aperture enter distillation still in, the vapor steamed from distillation still outflow be condensed into through second water condenser distilled water into the distilled water collect kettle in；The hydroquinones gas steamed from distillation still outflow be condensed into through the oil condenser liquid into the hydroquinones collect kettle in；Oil condenser, one cooling oil circuit piping of fuel tank and first water condenser formation cause cooling oil flows in circulation line to be cooled down, and the first water condenser and the second water condenser share a water cooling system.A kind of method using the system separating-purifying hydroquinones is also disclosed, using the method for two sections of distillations.
Description
Technical field
The present invention relates to hydroquinones recycling, purification technique field, and in particular to a kind of quinol solution's separation
Purification system and method.
Background technology
During traditional aniline process production hydroquinones, the circulation of technical grade solution (is commonly called as " long-used soup ") after concentrating 2 times, generation
Solution contains the inorganic salts impurity such as more ammonium sulfate, sodium carbonate, the hydroquinones quality produced after such as recycling condensing crystallizing
It is decreased obviously, quality criteria requirements is not reached much.Return oxidation operation typically is taken in industrial production, is made as aniline raw material
With the method business efficiency is not high, not only consumes the substantial amounts of energy, reduces the normal productive capacity of equipment, and reduction production
Direct yield.
The content of the invention
It is an object of the invention in view of the above-mentioned problems, providing that a kind of safety, cost are low, can obtain photographic-grade finished product pair
Resorcinol solution separation, the system and method for purification.
The present invention solves the technical scheme that its technical problem is used：
A kind of system for separating and purifying of quinol solution, including distillation still, hydroquinones are collected kettle, distilled water and collected
Charging aperture, air inlet are provided with the top of kettle, oil condenser, fuel tank, the first water condenser and the second water condenser, the distillation still
Mouth, steam outlet valve and hydroquinones steam outlet valve, quinol solution steam from the charging aperture enters distillation still
Vapor from distillation still outflow be condensed into through second water condenser distilled water into the distilled water collect kettle in；Steam
Hydroquinones gas from distillation still outflow be condensed into through the oil condenser liquid into the hydroquinones collect kettle in；Oil
Condenser, one cooling oil circuit piping of fuel tank and first water condenser formation cause cooling oil to be flowed in circulation line
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 also includes vavuum pump, distillation water collecting tank, and hydroquinones is received
Collection kettle, distilled water are collected kettle and are connected respectively with the vavuum pump, and vavuum pump is also connected with distilling water collecting tank.When having collected to benzene two
After phenol finished product, it is passed through water from charging aperture and system pipeline is cleaned, kettle and steaming is then collected to hydroquinones using vavuum pump
Distilled water collects kettle and carries out vacuumizing further cleaning respectively, collects moisture remaining in kettle and is collected by vavuum pump into distilled water
In tank.
Inert gas is passed through in the air inlet.Inert gas is passed through in systems before distillation hydroquinones, is prevented pair
Benzenediol steam occurs to dodge quick-fried (it is 156 DEG C that hydroquinones, which dodges quick-fried point) with air contact, although whole system is closed operation, but
No-spark is produced, it is ensured that the safe operation of system.
The temperature control of the oil condenser can be condensed at 200~230 DEG C to 287 DEG C of hydroquinones gas.
Steam condensate (SC) visor is provided with the pipeline for connecting the second water condenser and distilled water collection kettle, can be observed
Whether the moisture in the solution containing hydroquinones evaporates.
Collected in connection oil condenser and hydroquinones and be provided with hydroquinones condensate liquid visor, Ke Yiguan on the pipeline of kettle
Examine whether the hydroquinones in the solution of hydroquinones 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, comprise the following steps：
1) solution containing hydroquinones is passed through distillation still from charging aperture, opens distillation still stirring, open water vapour
Outlet valve, closes hydroquinones steam outlet valve, opens the cooling water system of the first water condenser and the formation of the second water condenser,
Using two sections of distillations, first paragraph first distills out the water in solution, and the heating-up 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 aqueous water, and then
Distilled water is flowed into collect in kettle；
2) after the moisture evaporation in solution is complete, second segment distillation is carried out, first inert gas is passed through full of steaming from air inlet
Kettle is evaporated, hydroquinones steam outlet valve is opened, steam outlet valve is closed, the temperature of distillation still is then controlled 287~290
DEG C, oil condenser is opened, the temperature of oil condenser is controlled at 200~230 DEG C, hydroquinones is opened and collects in kettle stirring, solution
Hydroquinones be evaporated to gas flow into oil condenser in be condensed into liquid into hydroquinones collect kettle in；
3) collected after hydroquinones condensate liquid, closed system, material hydroquinones collected in kettle is discharged, and is obtained pair
Benzenediol product.
Be separated, purification raw material can be 0~99.9% content quinol solution or impurity content not
Qualified solid hydroquinones.
The inventive method first takes the water in solution or finished product containing hydroquinones, semi-finished product at 100 ± 2 DEG C
The impurity such as the method for negative pressure evaporation and hydroquinones, inorganic salts are separated；Its secondary control reheating temperature at 289 ± 1 DEG C, because
For hydroquinones 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, hydroquinones is distillated purification；Nitrogen is passed through in system, is to prevent hydroquinones steam and air contact
Generation is dodged quick-fried (being 156 DEG C because it dodges quick-fried point), it is contemplated that the safe operation of system (although the system of haveing suffered is closed operation, and nothing
Spark is produced).
The beneficial effects of the invention are as follows：The system and method are safe and reliable, the small, cost of energy consumption consumption is low, can be from aniline
In various solution, finished product, semi-finished product in the aftertreatment technology of method production hydroquinones, separating-purifying obtains excellent pair of quality
Benzenediol finished product, product direct yield is high, hence it is evident that has saved resource and production cost, has particularly overturned aniline process processing " long-used soup "
The conventional method of solution, while the purification for the more solid hydroquinones of impurity have found new method.
Brief description of the drawings
Fig. 1 is the structural representation of quinol solution's system for separating and purifying of the present invention.
Embodiment
With reference to embodiment, the invention will be further described, but not thereby limiting the invention.
Embodiment 1 builds quinol solution's system for separating and purifying
One kind system for separating and purifying containing quinol solution as shown in Figure 1 is built, mainly by distillation still 1, hydroquinones
Collect kettle 2, distilled water and collect kettle 3, oil condenser 4, fuel tank 5, the first water condenser 6, the second water condenser 7, vavuum pump 8, steaming
Distilled water collecting tank 9, steam outlet valve 10 and hydroquinones steam outlet valve 11 are constituted.The top of distillation still 1 is provided with charging aperture
1a, air inlet 1b, steam outlet valve 10 and hydroquinones steam outlet valve 11, quinol solution enters from charging aperture 1a to steam
Evaporate in kettle 1, the vapor steamed is condensed into steaming from the outflow of distillation still 1 by steam outlet valve 10, the second water condenser 7 of arrival
Distilled water enters distilled water and collected in kettle 3, and the hydroquinones gas steamed passes through hydroquinones steam outlet valve from the outflow of distillation still 1
11st, arrival oil condenser 4 is condensed into liquid and collected into hydroquinones in kettle 2, oil condenser 4, the water condenser of fuel tank 5 and first
6, which form a cooling oil circuit piping, causes cooling oil flows in circulation line to be cooled down, the first water condenser 6 and second
Water condenser 7 shares a water cooling system, and hydroquinones is collected kettle 2, distilled water collection kettle 3 and is connected respectively with vavuum pump 8, very
Empty pump 8 is also connected with distilling water collecting tank 9.Steam outlet valve 10, the second water condenser 7 of connection and steaming are provided with distillation still 1
Distilled water is collected and is provided with steam condensate (SC) visor on the pipeline of kettle 3.Hydroquinones steam outlet valve 11 is provided with distillation still 1,
Connection oil condenser 4 and hydroquinones are collected and are provided with hydroquinones condensate liquid visor on the pipeline of kettle 2.Distillation still 1 is using electricity
Plus conduction oil mode provides thermal source, temperature control scope is 10~310 DEG C.
The separating-purifying quinol solution of embodiment 2
The quinol solution's system for separating and purifying built using embodiment 1 is separated to the solution containing hydroquinones
Purification, this method is mainly using two sections of distillation techniques, and first paragraph is first under 100 ± 2 DEG C of vapo(u)rizing temperature by solution
Moisture evaporation comes out, and second segment is to steam the hydroquinones in solution under 289 ± 1 DEG C of vapo(u)rizing temperature after moisture evaporation is complete
Issue and be collected.Specifically operate in accordance with the following steps：
1) by the solution containing hydroquinones 3~50% be passed through from charging aperture 1a distillation still 1 (amount per treatment for be not more than
The volume of distillation still 1 80%), open steam outlet valve 10, close hydroquinones steam outlet valve 11, open distillation still 1 and stir
Mix, distillation still 1 provides thermal source using electricity plus conduction oil mode, first paragraph first distills out the water in solution, control adding for distillation still 1
Hot temperature is 100 ± 2 DEG C, opens the cooling water system of the first water condenser 6 and the formation of the second water condenser 7, opens vacuum system
Negative pressure in system, control whole system notices that control cooling water outlet temperature cannot be greater than 45 DEG C in -0.1~-0.2kpa.Water
Steam flows into the second water condenser 7 from distillation still 1 and is cooled to aqueous water, and then flows into distilled water collection kettle 3.
2) steam condensate (SC) visor is observed, when not having condensed water outflow in visor, hydroquinones steam outlet valve is opened
11, the steam outlet valve 10 closed on reactor is passed through inert gas (such as nitrogen) full of whole system from air inlet 1b,
Second segment distillation is carried out, controls the temperature of distillation still 1 289 ± 1 DEG C (cannot be below 287 DEG C), opens oil condenser 4, control
The temperature of oil condenser 4 is opened hydroquinones collection kettle 2 and stirred, the hydroquinones in solution is evaporated at 200~230 DEG C
Liquid is condensed into gas inflow oil condenser 4 to collect in kettle 2 into hydroquinones, notices that observation hydroquinones condensate liquid is regarded
Mirror.
3) when do not have in hydroquinones condensate liquid visor condensate liquid by when, after 5 minutes stop heating, when temperature is reduced to
At 150 DEG C, the atmospheric valve that hydroquinones collects kettle 2 is opened, stops vacuum system, material hydroquinones collected in kettle is arranged
Go out, obtain the excellent hydroquinones photographic-grade finished product of quality.
4) when the temperature for heating distillation still 1 is down to normal temperature, it is put into running water purging system from charging aperture 1a and is prepared to enter into
Produce next time, the salt impurity that rinse water enters in oxidation operation, water is drenched material open circuit together with oxidation solution, is not entered to benzene
The processes such as reduction, the crystallization of diphenol.
Claims (7)
1. a kind of quinol solution's system for separating and purifying, it is characterised in that：Kettle is collected including distillation still (1), hydroquinones
(2), distilled water collects kettle (3), oil condenser (4), fuel tank (5), the first water condenser (6) and the second water condenser (7), described
Charging aperture (1a), air inlet (1b), steam outlet valve (10) and hydroquinones steam outlet valve are provided with the top of distillation still (1)
(11), quinol solution enters in distillation still (1) from the charging aperture (1a), and the vapor steamed flows out from distillation still (1)
Distilled water is condensed into through second water condenser (7) to collect in kettle (3) into the distilled water；The hydroquinones gas steamed
Liquid is condensed into through the oil condenser (4) from distillation still (1) outflow to collect in kettle (2) into the hydroquinones；Oil cooling is coagulated
Device (4), one cooling oil circuit piping of fuel tank (5) and first water condenser (6) formation cause cooling oil in circulation line
Middle flowing is cooled down, and the first water condenser (6) and the second water condenser (7) share a water cooling system.
2. quinol solution's system for separating and purifying as claimed in claim 1, it is characterised in that：Also include vavuum pump (8), steam
Distilled water collecting tank (9), hydroquinones is collected kettle (2), distilled water collection kettle (3) and is connected respectively with the vavuum pump (8), vavuum pump
(8) it is also connected with distillation water collecting tank (9).
3. quinol solution's system for separating and purifying as claimed in claim 1 or 2, it is characterised in that：The air inlet (1b)
In be passed through inert gas.
4. quinol solution's system for separating and purifying as claimed in claim 1 or 2, it is characterised in that：The oil condenser (4)
Temperature control at 200~230 DEG C.
5. quinol solution's system for separating and purifying as claimed in claim 1 or 2, it is characterised in that：Connecting the second water cooling
Condenser (7) and distilled water are collected and are provided with steam condensate (SC) visor on the pipeline of kettle (3).
6. quinol solution's system for separating and purifying as claimed in claim 1 or 2, it is characterised in that：In connection oil condenser
(4) collect with hydroquinones and be provided with hydroquinones condensate liquid visor on the pipeline of kettle (2).
7. a kind of quinol solution's process for separation and purification, it is characterised in that：Utilize pair described in any one of claim 1 to 6
Resorcinol solution system for separating and purifying carries out separating-purifying, comprises the following steps：
1) solution containing hydroquinones is passed through distillation still (1) from charging aperture (1a), opens distillation still (1) stirring, open
Steam outlet valve (10), closes hydroquinones steam outlet valve (11), opens the first water condenser (6) and the second water condenser
(7) cooling water system formed, using two sections of distillations, first paragraph first distills out the water in solution, the heating of control distillation still (1)
Temperature is 100 ± 2 DEG C, and the negative pressure in control distillation still (1) is in -0.1~-0.2kpa, and vapor flows into the from distillation still (1)
Two water condensers (7) are cooled to aqueous water, and then flow into distilled water collection kettle (3)；
2) after the moisture evaporation in solution is complete, second segment distillation is carried out, first inert gas is passed through full of steaming from air inlet (1b)
Kettle (1) is evaporated, hydroquinones steam outlet valve (11) is opened, steam outlet valve (10) is closed, the temperature of distillation still (1) is then controlled
Degree opens oil condenser (4) at 287~290 DEG C, and the temperature of control oil condenser (4) opens hydroquinones at 200~230 DEG C
The hydroquinones in kettle (2) stirring, solution is collected to be evaporated to be condensed into liquid entrance pair in gas inflow oil condenser (4)
Benzenediol is collected in kettle (2)；
3) collected after hydroquinones condensate liquid, closed system, material hydroquinones collected in kettle (2) is discharged, obtained pair
Benzenediol product.
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 |
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| 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 |
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| Publication Number | Publication Date |
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| CN107224745A true CN107224745A (en) | 2017-10-03 |
| CN107224745B CN107224745B (en) | 2019-05-24 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110665246A (en) * | 2019-10-21 | 2020-01-10 | 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 |
| WO2021135944A1 (en) * | 2019-12-31 | 2021-07-08 | 上海兆维科技发展有限公司 | Vacuum system and control method therefor |
| 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 (3)
| 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 |
| US20100069682A1 (en) * | 2006-06-29 | 2010-03-18 | Jean-Claude Masson | Preparation of purified hydroquinone |
| 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 |
-
2017
- 2017-07-17 CN CN201710579964.XA patent/CN107224745B/en active Active
Patent Citations (3)
| 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 |
| US20100069682A1 (en) * | 2006-06-29 | 2010-03-18 | Jean-Claude Masson | Preparation of purified hydroquinone |
| 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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110665246A (en) * | 2019-10-21 | 2020-01-10 | 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 |
| WO2021135944A1 (en) * | 2019-12-31 | 2021-07-08 | 上海兆维科技发展有限公司 | Vacuum system and control method therefor |
| 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 |
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| CN107224745B (en) | 2019-05-24 |
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