CN106365976A - Phenylacetic acid continuous production process - Google Patents
Phenylacetic acid continuous production process Download PDFInfo
- Publication number
- CN106365976A CN106365976A CN201610774851.0A CN201610774851A CN106365976A CN 106365976 A CN106365976 A CN 106365976A CN 201610774851 A CN201610774851 A CN 201610774851A CN 106365976 A CN106365976 A CN 106365976A
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- phenylacetic acid
- continuous production
- crystallizer
- acid
- production processes
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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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a phenylacetic acid continuous production process, and relates to the technical field of phenylacetic acid production. The process comprises the following specific steps that a phenylacetate solution and a dilute acid solution are mixed and then continuously injected into an oil-water separator, and separated liquid phenylacetic acid is extracted continuously and put into a crystallizer; meanwhile, water is added into the crystallizer, cooling crystallization is conducted, a solid-liquid mixture continuous to be extracted from the crystallizer for centrifugation, and then a phenylacetic acid crystal is obtained. According to the phenylacetic acid continuous production process, problems existing in the intermittent production process at present are solved. The phenylacetic acid continuous production process adopts few devices, is simple in process route, reduces the cost of labor, equipment, energy and the like, improves the work environment, adopts automation control conveniently, well ensures the process safety and production continuity and stability, improves the purity and quality of products and is suitable for large-scale production application and prominent in economic benefit and social benefit.
Description
Technical field
The present invention relates to phenylacetic acid production technical field.
Background technology
Phenylacetic acid is colorless plate crystal, and 76.5 DEG C of fusing point is soluble in hot water, is slightly soluble in cold water, is in important medicine
Mesosome, the huge market demand.Existing production technology is all using the still reaction of interval at present, low production efficiency, the setting of needs
Standby quantity is many, and the demand of operative employee is big.In the face of the chemical industry of high speed development, the serialization realizing producing becomes one kind and becomes
Gesture.
Content of the invention
The present invention provides a kind of phenylacetic acid continuous production processes it is achieved that the continuous production of phenylacetic acid, is easy to using automatically
Change and control, saved cost of labor, there is superior product quality, high income.
A kind of phenylacetic acid continuous production processes that the present invention provides, including technique in detail below:
Phenylacetate solution and dilute acid soln mixing are reacted, and reactant liquor is persistently injected in oil water separator carries out
Oil-water separation, persistently produces the oil phase phenylacetic acid isolated and enters crystallizer, add water simultaneously stir and cool down into described crystallizer
Crystallization, continuously outwards adopts solidliquid mixture from described crystallizer and carries out solid-liquid separation, that is, obtain phenylacetic acid crystalline solid.
Preferably, the concentration of described phenylacetate solution is 30%～40%.
Preferably, described phenylacetate solution is that one or more of sodium phenylacetate, phenylacetic acid ammonium, phenylacetic acid potassium mix
Close.
Preferably, the acid of described dilute acid soln is the mixing of one or more of sulphuric acid, hydrochloric acid, phosphoric acid and nitric acid.
Preferably, described phenylacetate solution controls temperature to be 60 DEG C～100 DEG C after mixing with dilute acid soln.
Preferably, described phenylacetate solution controls ph with dilute acid soln after mixing be 1～4.
Preferably, the mass ratio of the described oil phase entering in crystallizer and aqueous phase is 1:2～4.
Preferably, the temperature in described crystallizer is 30 DEG C～40 DEG C.
Preferably, the described water adding into crystallizer is a water.
Preferably, described oil water separator is oil-water separation tower.
Have the beneficial effect that produced by technical scheme of the present invention
The phenylacetic acid continuous production processes that the present invention provides solve problem present in current batch production process.In the present invention
Appliance arrangement is less, and process route is succinct, has saved the artificial, cost such as equipment, energy, has improved working environment, is easy to adopt
Automated condtrol, ensure that safety and continuous production, the stability of technique well, improves the purity of product, improves
Product quality, suitable use of large-scale production, economic benefit and social benefit project.
Brief description
Fig. 1 is the flow chart of phenylacetic acid continuous production processes of the present invention.
Specific embodiment
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
A kind of phenylacetic acid continuous production processes that the present invention provides, including technique in detail below:
Phenylacetate solution and dilute acid soln mixing are reacted, and reactant liquor is persistently injected in oil water separator carries out
Oil-water separation, persistently produces the oil phase phenylacetic acid isolated and enters crystallizer, add water simultaneously stir and cool down into described crystallizer
Crystallization, continuously outwards adopts solidliquid mixture from described crystallizer and carries out solid-liquid separation, that is, obtain phenylacetic acid crystalline solid.
In whole technological process, phenylacetate solution and dilute acid soln persistently inject mixing, and mixed liquor persistently carries out profit
Separate, the oil phase phenylacetic acid of extraction continues into crystallizer, and persistently extraction carries out solid-liquid separation, that is, complete the continuous of phenylacetic acid
Produce.
Because oil phase phenylacetic acid is larger with saline solution density contrast in oil water separator, preferable separating effect can be played.
Described solid-liquid separation can directly carry out separating using centrifuge.Described add water stirring into crystallizer and crystallisation by cooling is
In order to promote phenylacetic acid to become crystalline solid, further remove impurity is carried out to phenylacetic acid, because crystallizer has cooling system, energy simultaneously
Keeping temperature is constant, and the oil phase phenylacetic acid of entrance can become crystalline solid at once.
The concentration of described phenylacetate solution is 30%～40%.
Described phenylacetate solution is that one or more of sodium phenylacetate, phenylacetic acid ammonium, phenylacetic acid potassium mix.
The acid of described dilute acid soln is the mixing of one or more of sulphuric acid, hydrochloric acid, phosphoric acid and nitric acid.
Described phenylacetate solution controls temperature to be 60 DEG C～100 DEG C after mixing with dilute acid soln.
Described phenylacetate solution controls ph with dilute acid soln after mixing be 1～4.
The mass ratio of the described oil phase entering in crystallizer and aqueous phase is 1:2～4.
Temperature in described crystallizer is 30 DEG C～40 DEG C.
The described water adding into crystallizer is a water, that is, the water adding is not to produce in described oil water separator
The water of waste water gained after treatment, its effect is to promote phenylacetic acid to become crystalline solid, after removing oil-water separation further simultaneously
Impurity in phenylacetic acid.
Described oil water separator is oil-water separation tower.Described oil-water separation tower is packed tower, and the filler of employing is pottery rule
Whole filler, tower height is 10m～40m.Raw material mixed liquor is entered in oil-water separation tower by liquid liquid mixer under pressure.Mixed
Close and complete split-phase by density contrast after mutually entering tower.In oil-water separation tower, oil phase phenylacetic acid is mutually sufficiently separated with waste water, water
Continuously produce waste water workshop by tower reactor to be processed；By tower top, out warm pipeline enters crystallization kettle to oil phase.
Embodiment one:
The sulphuric acid of 30% sodium phenylacetate and 40% is fed intake according to the mass ratio of 1:0.25 in blender simultaneously, blender
In temperature control be 70 DEG C～75 DEG C, now in blender feed liquid ph be 1.5.Feed liquid after oil-water separation tower, from tower
The aqueous phase of the continuous extraction of kettle enters into effluent treatment plant, and the oil phase of overhead extraction continuously enters crystallization kettle.Enter crystallization kettle
The mass ratio of aqueous phase and oil phase is 1:2, and open cycle water management crystallization kettle temperature, at 35 DEG C～40 DEG C, continuously produces material from crystallization kettle
Liquid enters centrifuge.Whole production process adopts plc automatic control system it is achieved that the continuous prodution of phenylacetic acid.Product yield
Reach 99.75%, product liquid phase purity is 99.83%, product purity is 99.91%.
Embodiment two:
The hydrochloric acid of 35% sodium phenylacetate and 30% is fed intake according to the mass ratio of 1:0.30 in blender simultaneously, blender
In temperature control be 80 DEG C, now in blender feed liquid ph be 2.Feed liquid, after oil water separator, is continuously adopted from tower reactor
The aqueous phase going out enters into effluent treatment plant, and the oil phase of overhead extraction continuously enters crystallization kettle.The mass ratio of aqueous phase and oil phase is
1:3, open cycle water management crystallization kettle temperature, at 45 DEG C, continuously enters centrifuge from crystallization kettle extraction feed liquid.The phenylacetic acid being centrifuged out
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 according to the mass ratio of 1:0.43 in blender simultaneously, blender
In temperature control be 90 DEG C, now in blender feed liquid ph be 2.5.Feed liquid is after oil water separator, continuous from tower reactor
The aqueous phase of extraction enters into effluent treatment plant, and the oil phase of overhead extraction continuously enters crystallization kettle.Aqueous phase and the mass ratio of oil phase
For 1:4, open cycle water management crystallization kettle temperature, at 50 DEG C, continuously enters centrifuge from crystallization kettle extraction feed liquid.Product yield reaches
99.65%, product liquid phase purity is 99.90%, and product purity is 99.95%.
The present embodiment appliance arrangement is less, and process route is succinct, has saved the artificial, cost such as equipment, energy, has improved work
Make environment, be easy to adopt Automated condtrol, ensure that safety and continuous production, the stability of technique well, improve
The purity of product, improves product quality, suitable use of large-scale production, and economic benefit and social benefit project.
Specific case used herein is set forth to the principle of the present invention and embodiment, the saying of above example
Bright it is only intended to help and understands the method for the present invention and its core concept.It should be pointed out that the ordinary skill for the art
For personnel, under the premise without departing from the principles of the invention, the present invention can also be carried out with some improvement and modify, these improvement
Also fall in the protection domain of the claims in the present invention with modifying.
Claims (10)
1. a kind of phenylacetic acid continuous production processes are it is characterised in that include technique in detail below:
Phenylacetate solution and dilute acid soln mixing are reacted, and reactant liquor is persistently injected in oil water separator carries out
Oil-water separation, persistently produces the oil phase phenylacetic acid isolated and enters crystallizer, add water simultaneously stir and cool down into described crystallizer
Crystallization, continuously outwards adopts solidliquid mixture from described crystallizer and carries out solid-liquid separation, that is, obtain phenylacetic acid crystalline solid.
2. a kind of phenylacetic acid continuous production processes according to claim 1 are it is characterised in that described phenylacetate solution
Concentration is 30%～40%.
3. a kind of phenylacetic acid continuous production processes according to claim 1 are it is characterised in that described phenylacetate solution is
One or more of sodium phenylacetate, phenylacetic acid ammonium, phenylacetic acid potassium mix.
4. a kind of phenylacetic acid continuous production processes according to claim 1 are it is characterised in that the acid of described dilute acid soln is
One or more of sulphuric acid, hydrochloric acid, phosphoric acid and nitric acid mix.
5. a kind of phenylacetic acid continuous production processes according to claim 1 are it is characterised in that described phenylacetate solution
Temperature is controlled to be 60 DEG C～100 DEG C after mixing with dilute acid soln.
6. a kind of phenylacetic acid continuous production processes according to claim 1 are it is characterised in that described phenylacetate solution
Ph is controlled to be 1～4 after mixing with dilute acid soln.
7. a kind of phenylacetic acid continuous production processes according to claim 1 are it is characterised in that in described entrance crystallizer
Oil phase and aqueous phase mass ratio be 1:2～4.
8. a kind of phenylacetic acid continuous production processes according to claim 1 are it is characterised in that temperature in described crystallizer
For 30 DEG C～40 DEG C.
9. a kind of phenylacetic acid continuous production processes according to claim 1 are it is characterised in that described adds into crystallizer
The water entering is a water.
10. a kind of phenylacetic acid continuous production processes according to claim 1 are it is characterised in that described oil water separator is
Oil-water separation tower.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610774851.0A CN106365976B (en) | 2016-08-31 | 2016-08-31 | A kind of phenylacetic acid continuous production processes |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610774851.0A CN106365976B (en) | 2016-08-31 | 2016-08-31 | A kind of phenylacetic acid continuous production processes |
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| CN106365976A true CN106365976A (en) | 2017-02-01 |
| CN106365976B CN106365976B (en) | 2019-03-12 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113548954A (en) * | 2021-07-30 | 2021-10-26 | 四川信乙化工有限公司 | Phenylacetic acid preparation system |
| CN115300929A (en) * | 2022-08-15 | 2022-11-08 | 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 |
-
2016
- 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 |
|---|
| 李丽娟等: "从6- APA和7- ADCA生产废液中回收苯乙酸", 《化工环保》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113548954A (en) * | 2021-07-30 | 2021-10-26 | 四川信乙化工有限公司 | Phenylacetic acid preparation system |
| CN115300929A (en) * | 2022-08-15 | 2022-11-08 | 四川信乙化工有限公司 | Crystallization equipment and method for phenylacetic acid production |
| 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 |
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| CN106365976B (en) | 2019-03-12 |
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Address after: 051130 Yuanshi County, Shijiazhuang, Hebei Province, yuan Zhao Lunan Applicant after: Hebei Chengxin Group Co., Ltd. Address before: 051130 Yuanshi County, Shijiazhuang, Hebei Province, yuan Zhao Lunan Applicant before: Hebei Chengxin Co., Ltd. |
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