CN106365976B - A kind of phenylacetic acid continuous production processes - Google Patents
A kind of phenylacetic acid continuous production processes Download PDFInfo
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- CN106365976B CN106365976B CN201610774851.0A CN201610774851A CN106365976B CN 106365976 B CN106365976 B CN 106365976B CN 201610774851 A CN201610774851 A CN 201610774851A CN 106365976 B CN106365976 B CN 106365976B
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- phenylacetic acid
- continuous production
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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
- C07C51/02—Preparation of carboxylic acids or their salts, halides or anhydrides from salts of carboxylic acids
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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
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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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
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
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- Oil, Petroleum & Natural Gas (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of phenylacetic acid continuous production processes, are related to phenylacetic acid production technical field.Including technique in detail below: phenylacetate solution and dilute acid soln are mixed, and continue to inject in oil water separator, it persistently produces the liquid phenylacetic acid isolated and enters crystallizer, add water and crystallisation by cooling into the crystallizer simultaneously, it continuously adopts solidliquid mixture outward from the crystallizer to be centrifuged, i.e. acquisition phenylacetic acid crystalline solid.Phenylacetic acid continuous production processes provided by the invention solve the problems, such as current batch production process.Appliance arrangement is less in the present invention, process route is succinct, the costs such as artificial, equipment, the energy are saved, working environment is improved, convenient for using automation control, ensure that safety and the continuous production, stability of technique well, improve the purity of product, product quality is improved, use of large-scale production is suitble to, economic benefit and social benefit are prominent.
Description
Technical field
The present invention relates to phenylacetic acid production technical fields.
Background technique
Phenylacetic acid is colorless plate crystal, 76.5 DEG C of fusing point, is soluble in hot water, is slightly soluble in cold water, be important in medicine
Mesosome, the huge market demand.Current existing production technology is all made of the still reaction of interval, and production efficiency is low, and what is needed sets
Standby quantity is more, and the demand of operative employee is big.In face of the chemical industry of high speed development, realize that the serialization of production becomes as one kind
Gesture.
Summary of the invention
The present invention provides a kind of phenylacetic acid continuous production processes, realizes the continuous production of phenylacetic acid, convenient for using automatic
Change control, has saved cost of labor, had the characteristics that superior product quality, high income.
A kind of phenylacetic acid continuous production processes provided by the invention, including technique in detail below:
Phenylacetate solution and dilute acid soln are mixed and reacted, and reaction solution is persistently injected into oil water separator
Water-oil separating is carried out, the oily phase phenylacetic acid isolated persistently is produced and enters crystallizer, while being added water and stirred simultaneously into the crystallizer
Crystallisation by cooling is continuously adopted solidliquid mixture outward from the crystallizer and is separated by solid-liquid separation, i.e. acquisition phenylacetic acid crystalline solid.
Preferably, the concentration of the phenylacetate solution is 30%~40%.
Preferably, the phenylacetate solution is mixed for one or more of sodium phenylacetate, phenylacetic acid ammonium, phenylacetic acid potassium
It closes.
Preferably, the acid of the dilute acid soln is the mixing of one or more of sulfuric acid, hydrochloric acid, phosphoric acid and nitric acid.
Preferably, controlled at 60 DEG C~100 DEG C after the phenylacetate solution is mixed with dilute acid soln.
Preferably, it is 1~4 that pH is controlled after the phenylacetate solution is mixed with dilute acid soln.
Preferably, the oil into crystallizer is mutually and the mass ratio of water phase is 1:2~4.
Preferably, the temperature in the crystallizer is 30 DEG C~40 DEG C.
Preferably, the water being added into crystallizer is a water.
Preferably, the oil water separator is water-oil separating tower.
It is had the beneficial effect that caused by technical solution of the present invention
Phenylacetic acid continuous production processes provided by the invention solve the problems, such as current batch production process.This hair
Bright middle appliance arrangement is less, and process route is succinct, has saved the costs such as artificial, equipment, the energy, has improved working environment, be convenient for
Using automation control, it ensure that safety and the continuous production, stability of technique well, improve the purity of product,
Product quality is improved, use of large-scale production is suitble to, economic benefit and social benefit are prominent.
Detailed description of the invention
Fig. 1 is the flow chart of phenylacetic acid continuous production processes of the present invention.
Specific embodiment
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
A kind of phenylacetic acid continuous production processes provided by the invention, including technique in detail below:
Phenylacetate solution and dilute acid soln are mixed and reacted, and reaction solution is persistently injected into oil water separator
Water-oil separating is carried out, the oily phase phenylacetic acid isolated persistently is produced and enters crystallizer, while being added water and stirred simultaneously into the crystallizer
Crystallisation by cooling is continuously adopted solidliquid mixture outward from the crystallizer and is separated by solid-liquid separation, i.e. acquisition phenylacetic acid crystalline solid.
In entire process flow, phenylacetate solution and dilute acid soln persistently inject mixing, and mixed liquor persistently carries out grease
Separation, the oily phase phenylacetic acid of extraction continue into crystallizer, and continue extraction and be separated by solid-liquid separation, i.e., completion phenylacetic acid is continuous
Production.
Since phase phenylacetic acid oily in oil water separator and salting liquid density contrast are larger, preferable separating effect can be played.
The separation of solid and liquid can be directly used centrifuge and be separated.It is described to be added water and stirred into crystallizer and crystallisation by cooling is
It in order to promote phenylacetic acid to become crystalline solid, while further cleaning to phenylacetic acid, since crystallizer has cooling system, energy
Keep temperature constant, the oily phase phenylacetic acid of entrance can become crystalline solid at once.
The concentration of the phenylacetate solution is 30%~40%.
The phenylacetate solution is the mixing of one or more of sodium phenylacetate, phenylacetic acid ammonium, phenylacetic acid potassium.
The acid of the dilute acid soln is the mixing of one or more of sulfuric acid, hydrochloric acid, phosphoric acid and nitric acid.
The phenylacetate solution mixed with dilute acid soln after controlled at 60 DEG C~100 DEG C.
Control pH is 1~4 after the phenylacetate solution is mixed with dilute acid soln.
The mass ratio into oil phase and water phase in crystallizer is 1:2~4.
Temperature in the crystallizer is 30 DEG C~40 DEG C.
The water being added into crystallizer is a water, that is, is generated in the not described oil water separator of the water being added
Waste water resulting water after processing, effect is that phenylacetic acid is promoted to become crystalline solid, while further after removal water-oil separating
Impurity in phenylacetic acid.
The oil water separator is water-oil separating tower.The water-oil separating tower is packed tower, and the filler used is ceramics rule
Whole filler, tower height are 10m~40m.Raw material mixed liquor is entered in water-oil separating tower by liquid liquid mixer under pressure.It is mixed
It closes mutually to enter after tower and completes split-phase by density contrast.Oily phase phenylacetic acid is mutually sufficiently separated with waste water in water-oil separating tower, water
It is mutually continuously produced to waste water workshop and is handled by tower reactor；It is oily that mutually coming out warm pipeline by tower top enters crystallization kettle.
Embodiment one:
The sulfuric acid of 30% sodium phenylacetate and 40% is fed intake into mixer simultaneously according to the mass ratio of 1:0.25, is mixed
Temperature control in clutch is 70 DEG C~75 DEG C, and the pH of feed liquid is 1.5 in mixer at this time.Feed liquid after water-oil separating tower,
The water phase continuously produced from tower reactor enters effluent treatment plant, and the oil of overhead extraction mutually continuously enters crystallization kettle.Into crystallization
The mass ratio of the water phase of kettle and oily phase is 1:2, and open cycle water management crystallization kettle temperature is continuously adopted from crystallization kettle at 35 DEG C~40 DEG C
Out-feed liquid is into centrifuge.Entire production process uses PLC automatic control system, realizes the continuous production of phenylacetic acid.Product
Yield reaches 99.75%, and product liquid phase purity is 99.83%, product purity 99.91%.
Embodiment two:
The hydrochloric acid of 35% sodium phenylacetate and 30% is fed intake into mixer simultaneously according to the mass ratio of 1:0.30, is mixed
Temperature control in clutch is 80 DEG C, and the pH of feed liquid is 2 in mixer at this time.Feed liquid connects after oil water separator from tower reactor
The water phase of continuous extraction enters effluent treatment plant, and the oil of overhead extraction mutually continuously enters crystallization kettle.The quality of water phase and oily phase
Than for 1:3, open cycle water management crystallization kettle temperature continuously produces feed liquid into centrifuge from crystallization kettle at 45 DEG C.The benzene being centrifuged out
Acetic acid quality is better than embodiment one, and product yield reaches 99.71%, and product liquid phase purity is 99.88%, and product purity is
99.94%。
Embodiment three:
The nitric acid of 40% sodium phenylacetate and 40% is fed intake into mixer simultaneously according to the mass ratio of 1:0.43, is mixed
Temperature control in clutch is 90 DEG C, and the pH of feed liquid is 2.5 in mixer at this time.Feed liquid is after oil water separator, from tower reactor
The water phase continuously produced enters effluent treatment plant, and the oil of overhead extraction mutually continuously enters crystallization kettle.The matter of water phase and oily phase
Amount is than being 1:4, and open cycle water management crystallization kettle temperature is at 50 DEG C, continuously from crystallization kettle extraction feed liquid into centrifuge.Product yield
Reach 99.65%, product liquid phase purity is 99.90%, product purity 99.95%.
The present embodiment appliance arrangement is less, and process route is succinct, has saved the costs such as artificial, equipment, the energy, has improved work
Make environment, convenient for using automation control, ensure that safety and the continuous production, stability of technique well, improve
The purity of product, improves product quality, is suitble to use of large-scale production, and economic benefit and social benefit are prominent.
Used herein a specific example illustrates the principle and implementation of the invention, and above embodiments are said
It is bright to be merely used to help understand method and its core concept of the invention.It should be pointed out that for the ordinary skill of the art
, without departing from the principle of the present invention, can be with several improvements and modifications are made to the present invention for personnel, these improvement
It is also fallen within the protection scope of the claims of the present invention with modification.
Claims (9)
1. a kind of phenylacetic acid continuous production processes, which is characterized in that including technique in detail below:
Phenylacetate solution and dilute acid soln are mixed and reacted, and reaction solution is persistently injected into oil water separator and is carried out
Water-oil separating persistently produces the oily phase phenylacetic acid isolated and enters crystallizer, while adding water and stirring and cooling down into the crystallizer
Crystallization, continuously adopts solidliquid mixture outward from the crystallizer and is separated by solid-liquid separation, i.e. acquisition phenylacetic acid crystalline solid；
The oil water separator is water-oil separating tower, and the reaction solution enters grease point by liquid liquid mixer under pressure
From in tower, water phase is continuously produced by tower reactor, and oil is mutually by overhead extraction.
2. a kind of phenylacetic acid continuous production processes according to claim 1, which is characterized in that the phenylacetate solution
Concentration is 30%~40%.
3. a kind of phenylacetic acid continuous production processes according to claim 1, which is characterized in that the phenylacetate solution is
The mixing of one or more of sodium phenylacetate, phenylacetic acid ammonium, phenylacetic acid potassium.
4. a kind of phenylacetic acid continuous production processes according to claim 1, which is characterized in that the acid of the dilute acid soln is
The mixing of one or more of sulfuric acid, hydrochloric acid, phosphoric acid and nitric acid.
5. a kind of phenylacetic acid continuous production processes according to claim 1, which is characterized in that the phenylacetate solution
Controlled at 60 DEG C~100 DEG C after being mixed with dilute acid soln.
6. a kind of phenylacetic acid continuous production processes according to claim 1, which is characterized in that the phenylacetate solution
It is 1~4 that pH is controlled after mixing with dilute acid soln.
7. a kind of phenylacetic acid continuous production processes according to claim 1, which is characterized in that described enters in crystallizer
Oil mutually and water phase mass ratio be 1:2~4.
8. a kind of phenylacetic acid continuous production processes according to claim 1, which is characterized in that the temperature in the crystallizer
It is 30 DEG C~40 DEG C.
9. a kind of phenylacetic acid continuous production processes according to claim 1, which is characterized in that described to add into crystallizer
The water entered is a water.
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| CN201610774851.0A CN106365976B (en) | 2016-08-31 | 2016-08-31 | A kind of phenylacetic acid continuous production processes |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113548954A (en) * | 2021-07-30 | 2021-10-26 | 四川信乙化工有限公司 | Phenylacetic acid preparation system |
| CN115300929B (en) * | 2022-08-15 | 2024-05-10 | 四川信乙化工有限公司 | Crystallization equipment and method for phenylacetic acid production |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060691A (en) * | 2010-12-13 | 2011-05-18 | 日照鲁信金禾生化有限公司 | Continuous acidolysis process for calcium hydrogen citrate |
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- 2016-08-31 CN CN201610774851.0A patent/CN106365976B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060691A (en) * | 2010-12-13 | 2011-05-18 | 日照鲁信金禾生化有限公司 | Continuous acidolysis process for calcium hydrogen citrate |
Non-Patent Citations (1)
| Title |
|---|
| 从6- APA和7- ADCA生产废液中回收苯乙酸;李丽娟等;《化工环保》;2007;第27卷(第3期);第260-262页 |
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