CN104998429A - Dehydration technology and device for salicylic acid intermediate sodium phenoxide - Google Patents

Dehydration technology and device for salicylic acid intermediate sodium phenoxide Download PDF

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Publication number
CN104998429A
CN104998429A CN201510506045.0A CN201510506045A CN104998429A CN 104998429 A CN104998429 A CN 104998429A CN 201510506045 A CN201510506045 A CN 201510506045A CN 104998429 A CN104998429 A CN 104998429A
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CN
China
Prior art keywords
sodium phenate
tube evaporator
salicylic acid
acid intermediate
kestner long
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Pending
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CN201510506045.0A
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Chinese (zh)
Inventor
吴孝好
何雪涛
徐文辉
吴迪
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Shandong Xinhua Pharmaceutical Co Ltd
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Shandong Xinhua Pharmaceutical Co Ltd
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Priority to CN201510506045.0A priority Critical patent/CN104998429A/en
Publication of CN104998429A publication Critical patent/CN104998429A/en
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

Abstract

The invention relates to a dehydration technology and device for salicylic acid intermediate sodium phenoxide and belongs to the technical field of dehydration of sodium phenoxide. According to the dehydration technology for the salicylic acid intermediate sodium phenoxide, a prepared sodium phenoxide solution is heated, then a vacuum feeding manner is adopted, the sodium phenoxide solution is delivered to a membrane evaporator for evaporation dehydration, and steam in the membrane evaporator is collected after being condensed. With the adoption of the dehydration technology for the salicylic acid intermediate sodium phenoxide, the technology time is shortened and the heat utilization efficiency is improved; the dehydration device for the salicylic acid intermediate sodium phenoxide is simple to design, scientific and reasonable.

Description

The dewatering process of salicylic acid intermediate sodium phenate and device
Technical field
The present invention relates to a kind of dewatering process and device of salicylic acid intermediate sodium phenate, belong to sodium phenate dehydration technique field.
Background technology
Salicylic purposes is quite extensive, is current extremely important medicine chemical material, mainly for the manufacture of antipyretic, analgesic aspirin, is also the raw material that the multiple important drugs such as gaultherolin, salethyl and salicylamide produces synthesis simultaneously.Only salicylic domestic market scale is at about 20,000 tons, China is salicylic acid spin-off producing country and the exported country such as aspirin, gaultherolin main in the world, therefore salicylic use amount is huge, and therefore short, simple to operate, eco-friendly technique is very necessary the development technology time.
The traditional synthesis technique of salicylic acid produces sodium phenate with phenol or phenol solution with NaOH reaction, the frequent press-dehydrating of aqueous sodium phenolate solution, decompression dehydration, dry with phenol band water again, then carry out carboxylation reaction with carbon dioxide at about 200 DEG C and produce sodium salicylate, add water and generate sodium salicylate solution.Salicylic acid product is bulk raw material product, because normal pressure dewatering time is long, to consume quantity of steam huge, heat utilization efficiency is low.For shortening the process time and improving efficiency of utilization, need the new dewatering process of research and development and device used.
Summary of the invention
The object of this invention is to provide a kind of dewatering process of salicylic acid intermediate sodium phenate, which shorten the process time, improve efficiency of utilization; Invention also provides the dewater unit of salicylic acid intermediate sodium phenate, simplicity of design, scientific and reasonable.
The dewatering process of salicylic acid intermediate sodium phenate of the present invention, by the sodium phenate solution heating prepared, then adopt vacuum feed mode, sodium phenate solution is delivered to kestner long-tube evaporator and carries out dehydration by evaporation, the steam in kestner long-tube evaporator is collected after condensation.
Described sodium phenate solution by phenol and NaOH formulated; The volume of sodium phenate solution is 5000-48500L.
The sodium phenate solution prepared is utilized and is steam heated to 90 ~ 95 DEG C, heat preservation for standby use.
Described kestner long-tube evaporator vacuum degree control is at 0.05 ~ 0.095Mpa; Sodium phenate mass content in kestner long-tube evaporator after dehydration controls 80.07 ~ 94.87%.
Pass into steam in the chuck of described kestner long-tube evaporator to heat, the steam pressure of kestner long-tube evaporator is 0.3 ~ 0.5Mpa.
The heating surface (area) (HS of described separate unit kestner long-tube evaporator is 4M 2, adopt 4 kestner long-tube evaporator parallel runnings.
The dewater unit of described salicylic acid intermediate sodium phenate, comprise sodium phenate preparing tank, kestner long-tube evaporator, condenser, concentrated sodium phenate collector and condensate recovering device, the bottom of sodium phenate preparing tank is connected with the charging aperture at kestner long-tube evaporator top, and the gas outlet at kestner long-tube evaporator top is connected with condensate recovering device successively with condenser; Discharging opening bottom kestner long-tube evaporator is connected with concentrated sodium phenate collector; Kestner long-tube evaporator, condensate recovering device and concentrated sodium phenate collector are equipped with vavuum pump; The pipeline that sodium phenate preparing tank is connected with kestner long-tube evaporator is provided with control valve and spinner flowmeter.
Described concentrated sodium phenate collector is connected with electronic scale.
Described sodium phenate preparing tank top is provided with feed pipe.
The outside of described sodium phenate preparing tank, kestner long-tube evaporator and concentrated sodium phenate collector is equipped with chuck, chuck is equipped with import and outlet.
The present invention has following beneficial effect:
The dewatering process of salicylic acid intermediate sodium phenate of the present invention is simple, shortens about 2 hours process times; Improve efficiency of utilization, the use amount of steam decreases 1/3, and only this saving more than 200 ten thousand yuan every year of steam, meets the technological requirement of energy-conserving and environment-protective; The dewater unit of described salicylic acid intermediate sodium phenate, simplicity of design, scientific and reasonable, operating environment is greatly improved.Because salicylic acid belongs to large tonnage product in China, after using technique of the present invention and device, meet environmental friendliness, Green Chemistry characteristic attribute, there is good economic benefit and social benefit.
Accompanying drawing explanation
Fig. 1 is the dewater unit schematic diagram of salicylic acid intermediate sodium phenate of the present invention;
In figure: 1, feed pipe; 2, spinner flowmeter; 3, kestner long-tube evaporator; 4, vavuum pump; 5, condenser; 6, condensate recovering device; 7, concentrated sodium phenate collector; 8, electronic scale; 9, control valve; 10, sodium phenate preparing tank.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further illustrated, but it does not limit enforcement of the present invention.
The device that the dewatering process of salicylic acid intermediate sodium phenate of the present invention is used, comprise sodium phenate preparing tank 10, kestner long-tube evaporator 3, condenser 5, concentrated sodium phenate collector 7 and condensate recovering device 6, the bottom of sodium phenate preparing tank 10 is connected with the charging aperture at kestner long-tube evaporator 3 top, and the gas outlet at kestner long-tube evaporator 3 top is connected with condensate recovering device 6 successively with condenser 5; Discharging opening bottom kestner long-tube evaporator 3 is connected with concentrated sodium phenate collector 7; Kestner long-tube evaporator 3, condensate recovering device 6 and concentrated sodium phenate collector 7 are equipped with vavuum pump 4; The pipeline that sodium phenate preparing tank 10 is connected with kestner long-tube evaporator 3 is provided with control valve 9 and spinner flowmeter 2.
Described concentrated sodium phenate collector 7 is connected with electronic scale 8.
Described sodium phenate preparing tank 10 top is provided with feed pipe 1.
The outside of described sodium phenate preparing tank 10, kestner long-tube evaporator 3 and concentrated sodium phenate collector 7 is equipped with chuck, chuck is equipped with import and outlet.
Raw materials usedly be commercially available prod.
The concentration of the phenol solution in following examples, sodium hydrate aqueous solution and sodium phenate solution is mass body volume concentrations, and solute is with quality g metering, and solvent measures with volume mL.
Embodiment 1
Be phenol solution and the 1480L concentration of 66.04g/mL by 3530L concentration be the sodium phenate solution that 73.3g/mL sodium hydrate aqueous solution is mixed with that concentration is 59.50g/mL, volume is 5000L, be heated to 90 DEG C by steam to sodium phenate preparing tank; When kestner long-tube evaporator, condensate recovering device, concentrated sodium phenate collector vacuum reach 0.05Mpa, open control valve, open spinner flowmeter, make every platform kestner long-tube evaporator charging rate control at 1000L/h, adopt 4 kestner long-tube evaporator parallel runnings; Kestner long-tube evaporator Steam pressure control is at 0.3Mpa; Concentrated sodium phenate content is 80.07wt%.
Embodiment 2
Be phenol solution and the 8080L concentration of 60.24g/mL by 21950L concentration be the sodium phenate solution that 70.31g/mL sodium hydrate aqueous solution is mixed with that concentration is 54.47g/mL, volume is 30030L, be heated to 93 DEG C by steam to phenol sodium preparing tank; When kestner long-tube evaporator, water outlet receiver, concentrated sodium phenate receiver system vacuum reach 0.078Mpa, drive material cock into, open flowmeter cock, make every platform kestner long-tube evaporator charging rate control at 1500L/h, open four simultaneously; Kestner long-tube evaporator Steam pressure control is at 0.4Mpa; Concentrated sodium phenate content is 90.27wt%.
Embodiment 3
Be phenol solution and the 13520L concentration of 64.24g/mL by 35000L concentration be the sodium phenate solution that 71.5g/mL sodium hydrate aqueous solution is mixed with that concentration is 57.18g/mL, volume is 48500L, be heated to 95 DEG C by steam to sodium phenate preparing tank; When kestner long-tube evaporator, water outlet receiver, concentrated sodium phenate receiver system vacuum reach 0.095Mpa, drive material cock into, open flowmeter cock, make every platform kestner long-tube evaporator charging rate control at 2000L/h, open four simultaneously; Kestner long-tube evaporator Steam pressure control is at 0.5Mpa; Concentrated sodium phenate content is 94.87wt%.

Claims (10)

1. the dewatering process of a salicylic acid intermediate sodium phenate, it is characterized in that: by the sodium phenate solution heating prepared, then vacuum feed mode is adopted, sodium phenate solution is delivered to kestner long-tube evaporator (3) and carries out dehydration by evaporation, the steam in kestner long-tube evaporator (3) is collected after condensation.
2. the dewatering process of salicylic acid intermediate sodium phenate according to claim 1, is characterized in that: sodium phenate solution by phenol and NaOH formulated; The volume of sodium phenate solution is 5000-48500L.
3. the dewatering process of salicylic acid intermediate sodium phenate according to claim 1, is characterized in that: utilized by the sodium phenate solution prepared and be steam heated to 90 ~ 95 DEG C.
4. the dewatering process of salicylic acid intermediate sodium phenate according to claim 1, is characterized in that: kestner long-tube evaporator (3) vacuum degree control is at 0.05 ~ 0.095Mpa; Sodium phenate mass content in kestner long-tube evaporator (3) after dehydration controls 80.07 ~ 94.87%.
5. the dewatering process of salicylic acid intermediate sodium phenate according to claim 1, is characterized in that: pass into steam in the chuck of kestner long-tube evaporator (3) and heat, the steam pressure of kestner long-tube evaporator (3) is 0.3 ~ 0.5Mpa.
6. the dewatering process of salicylic acid intermediate sodium phenate according to claim 1, is characterized in that: the heating surface (area) (HS of separate unit kestner long-tube evaporator (3) is 4M 2, adopt the parallel running of 4 kestner long-tube evaporators (3).
7. the dewater unit of the arbitrary described salicylic acid intermediate sodium phenate of claim 1-6, it is characterized in that: comprise sodium phenate preparing tank (10), kestner long-tube evaporator (3), condenser (5), concentrated sodium phenate collector (7) and condensate recovering device (6), the bottom of sodium phenate preparing tank (10) is connected with the charging aperture at kestner long-tube evaporator (3) top, and the gas outlet at kestner long-tube evaporator (3) top is connected with condensate recovering device (6) successively with condenser (5); The discharging opening of kestner long-tube evaporator (3) bottom is connected with concentrated sodium phenate collector (7); Kestner long-tube evaporator (3), condensate recovering device (6) and concentrated sodium phenate collector (7) are equipped with vavuum pump (4); The pipeline that sodium phenate preparing tank (10) is connected with kestner long-tube evaporator (3) is provided with control valve (9) and spinner flowmeter (2).
8. the dewater unit of salicylic acid intermediate sodium phenate according to claim 7, is characterized in that: concentrated sodium phenate collector (7) is connected with electronic scale (8).
9. the dewater unit of salicylic acid intermediate sodium phenate according to claim 7, is characterized in that: sodium phenate preparing tank (10) top is provided with feed pipe (1).
10. the dewater unit of salicylic acid intermediate sodium phenate according to claim 7, it is characterized in that: the outside of sodium phenate preparing tank (10), kestner long-tube evaporator (3) and concentrated sodium phenate collector (7) is equipped with chuck, chuck is equipped with import and outlet.
CN201510506045.0A 2015-08-17 2015-08-17 Dehydration technology and device for salicylic acid intermediate sodium phenoxide Pending CN104998429A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114345285A (en) * 2022-01-12 2022-04-15 青岛科技大学 Continuous production process of sodium salicylate solution
CN115650842A (en) * 2022-10-25 2023-01-31 江苏普源化工有限公司 Production process of circulating dehydration high-purity salicylic acid

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1371871A (en) * 2001-11-26 2002-10-02 鞍山市凯特环保工程技术有限公司 Phenolic resin sewage treatment method
CN202219095U (en) * 2011-08-12 2012-05-16 启东神农机械有限公司 Heat circulation system for evaporator

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1371871A (en) * 2001-11-26 2002-10-02 鞍山市凯特环保工程技术有限公司 Phenolic resin sewage treatment method
CN202219095U (en) * 2011-08-12 2012-05-16 启东神农机械有限公司 Heat circulation system for evaporator

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114345285A (en) * 2022-01-12 2022-04-15 青岛科技大学 Continuous production process of sodium salicylate solution
CN114345285B (en) * 2022-01-12 2023-09-08 青岛科技大学 Continuous production process of sodium salicylate solution
CN115650842A (en) * 2022-10-25 2023-01-31 江苏普源化工有限公司 Production process of circulating dehydration high-purity salicylic acid

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Application publication date: 20151028