CN205549662U - Benzoic acid purification crystallization device - Google Patents
Benzoic acid purification crystallization device Download PDFInfo
- Publication number
- CN205549662U CN205549662U CN201620378283.8U CN201620378283U CN205549662U CN 205549662 U CN205549662 U CN 205549662U CN 201620378283 U CN201620378283 U CN 201620378283U CN 205549662 U CN205549662 U CN 205549662U
- Authority
- CN
- China
- Prior art keywords
- benzoic acid
- conduction oil
- cavity
- storage tank
- import
- 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
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model relates to a benzoic acid purification crystallization device. Including the falling liquid film crystallizer, falling liquid film crystallizer tank body cavity goes up the cavity by partitions are divided into, well cavity and lower cavity, it is equipped with the import of industrial grade benzoic acid to go up the cavity, the temperature sensor mouth, well cavity upper portion is equipped with the conduction oil import, the lower part is equipped with the conduction oil export, it feeds through through the crystallization pipe with lower cavity to go up the cavity, the internal liquid distributor that installs of epicoele, the cavity bottom is equipped with the benzoic acid export down, the benzoic acid of cavity exports through tube coupling benzoic acid mother liquor storage tank down, the mother liquor recycling pump, the mother liquor recycling pump passes through the import of tube coupling industrial grade benzoic acid, the conduction oil export of well cavity lower part is through tube coupling conduction oil storage tank and heat conduction oil circulation pump, the heat conduction oil circulation pump passes through the conduction oil import on cavity upper portion in the tube coupling, slot type distributor among the internal liquid distributor of epicoele links to each other with the import of industrial grade benzoic acid. Be used for benzoic acid purification crystallization process, no waste water produces, and the running cost is low, and product purity is high.
Description
Technical field
This utility model relates to a kind of crystallization apparatus, a kind of crystallization apparatus for benzoic acid purification, belongs to doctor
Medicine equipment manufacturing technology field.
Background technology
Benzoic acid (Benzoic Acid) is a kind of fine chemical product, is divided into food stage pharmaceutical grade and industry according to purposes
Level, also known as benzoic acid, flakey or acicular crystal, has the abnormal smells from the patient of benzene or formaldehyde, fusing point 122 DEG C, boiling point 249 DEG C, slightly soluble
Yu Shui, is dissolved in the organic solvents such as ethanol, methanol, ether.Typically use frequently as medicine or preservative, have suppression fungus, thin
Bacterium, the effect of fungus growth, be usually coated to time medicinal on skin, in order to treat the dermatosis of tinea class.It addition, can be additionally used in conjunction
Become fiber, resin, coating, rubber etc..Benzoic industrial process mainly has toluene liquid-phase air oxidation process, benzotrichloride
Hydrolyze method, phthalic anhydride decarboxylation method, benzyl zirconyl oxyhalides method etc., benzoic purity >=98.0%, containing being difficult to the miscellaneous of removing
Matter, making product is micro-Huang or micro-green.Along with benzoic acid consumption in medicine and feedstuff increases considerably, food and medicine level benzene
The demand of formic acid is increasing, toluene liquid-phase air oxidation process the benzoic acid produced can be refining to obtain food and medicine level further
Benzoic acid.The benzoic purity of food and medicine level needs >=99.50%.Current domestic many producers use water-soluble crystallization process raw
The benzoic acid of production of high purity, by molten in boiling water for technical grade (GC purity is about 98.5%) benzoic acid, then decrease temperature crystalline, centrifugal,
Being dried, the benzoic content of finished product pharmaceutical grade obtained is high, white color.The product 50ppm Han impurity prepared in aforementioned manners
Hereinafter, effectively removes the impurity such as biphenyl dicarboxylic acid, phenol.But the method produces substantial amounts of waste water, and benzoic acid is in boiling water
Dissolubility only have 10% (mass ratio) left and right often produce one ton of finished acid to discharge about 9 tons of waste water, and waste water to be taken away substantial amounts of
Benzoic acid and derivant (COD reaches about 20000mg/L) thereof, three-waste pollution is big, and raw materials consumption is big, and production cost is high, equipment
Investment height, efficiency is low, and costly, finished product purity further walks raising difficulty.Therefore, seek a kind of equipment investment few, meet environmental protection
Requirement, the benzoic acid purified crystals device that production cost is low, become the eager desire of benzoic acid manufacturing enterprise.
Summary of the invention
The purpose of this utility model is to provide a kind of benzoic acid purified crystals device, to reduce production cost, solves refined
During environmental issue.
The technical scheme in the invention for solving the technical problem is such that a kind of benzoic acid purified crystals dress
Put, including falling-film crystallizer, benzoic acid circulation line, conduction oil circulation line, falling-film crystallizer tank inner chamber by upper spacer and
Lower clapboard is divided into upper cavity, middle cavity and lower chamber, and upper cavity is provided with technical grade benzoic acid import, temperature sensor mouth, lumen
Body top is provided with heat conductive oil inlet, bottom is provided with the vertical crystallization by both ends open of conduction oil outlet, upper cavity and lower chamber
Pipe connects, and is provided with liquid distributor in upper cavity, is provided with benzoic acid outlet bottom lower chamber, and the benzoic acid outlet of lower chamber is by pipe
Road connects benzoic acid mother solution storage tank, Recycling Mother Solution pump, and Recycling Mother Solution pump connects technical grade benzoic acid import, middle cavity by pipeline
The conduction oil outlet of bottom connects conduction oil storage tank and heat conduction oil circulating pump by pipeline, and heat conduction oil circulating pump is connected by pipeline
The heat conductive oil inlet on middle cavity top, the groove type distributor in liquid distributor in upper cavity is connected with technical grade benzoic acid import.
Described crystallization apparatus, conduction oil storage tank has three, respectively is crystallization conduction oil storage tank, the storage of diaphoresis conduction oil
Groove and melted conduction oil storage tank.Electric tracing or steam tracing and temperature sensor mouth it is equipped with on three conduction oil storage tanks.
Liquid distributor is slot type liquid distributor, belongs to the product of public offering on market.
This utility model obtains and provides the benefit that:
This device consumption of raw materials is little, and equipment investment is low, produces without waste water, and operating cost is low, and crystalline product purity is high.
Accompanying drawing explanation
Fig. 1 is structural representation of the present utility model.
Fig. 2 is liquid distributor structural representation
Fig. 3 is groove type distributor lower disc top view.
Fig. 4 is mother liquor overflow tube side view.
In figure, label implication is as follows:
A, falling-film crystallizer B, benzoic acid circulation line C, conduction oil circulation line D, liquid distributor 1, heat conduction oil pocket 2, temperature
Degree sensor port 3, heat conductive oil inlet 4, technical grade benzoic acid import 5, temperature sensor mouth 6, upper cavity 7, upper spacer 8,
Crystallizer 9, baffle plate 10, conduction oil outlet 11, lower clapboard 12, temperature sensor mouth 13, lower chamber 14, benzoic acid outlet
15, high-quality benzoic acid outlet 16, valve I 17, diaphoresis benzoic acid outlet 18, valve II 19, benzoic acid mother liquor outlet
20, valve III 21, benzoic acid mother solution storage tank 22, valve IV 23, Recycling Mother Solution pump 24, heat conduction oil circulating pump 25, valve V
26, crystallization conduction oil storage tank 27, valve VI 28, valve VII 29, diaphoresis conduction oil storage tank 30, valve VIII 31, valve Ⅸ
32, the disk 35 under melted conduction oil storage tank 33, valve Ⅹ 34, groove type distributor, upper mother solution portal 36, upper gear liquid part
37, lower block liquid part 38, level control part 39, support bar 40, lower mother solution portal 41, gear fluid cylinder 42, mother liquor overflow pipe 43, groove
Formula distributor 44, liquid outlet.
Detailed description of the invention
This utility model is further described by the specific embodiment be given below in conjunction with accompanying drawing and accompanying drawing.
As it is shown in figure 1, a kind of benzoic acid purified crystals device, including falling-film crystallizer A, falling-film crystallizer tank inner chamber by
Upper spacer 7, lower clapboard 11 are divided into upper cavity 6, middle cavity 1 and lower chamber 13, and upper cavity 6 side is provided with technical grade benzoic acid import
4, temperature sensor mouth 5, middle cavity 1 top is provided with heat conductive oil inlet 3, and middle cavity bottom is provided with conduction oil outlet 10, middle cavity
Inside being provided with the vertical crystallizer 8 of both ends open, the two-port of vertical crystallizer 8 is opened in upper cavity 6 and lower chamber 13 respectively,
And upper cavity is connected with lower chamber.Liquid distributor D is installed in upper cavity 6, bottom lower chamber 13, is provided with benzoic acid outlet 14, under
The benzoic acid outlet 14 of cavity connects benzoic acid mother solution storage tank 21, Recycling Mother Solution pump 23 by pipeline, connects industry by pipeline
Level benzoic acid import 4, becomes benzoic acid circulation line B；The conduction oil outlet 10 of middle cavity 1 bottom connects conduction oil by pipeline
In the connection of storage tank, heat conduction oil circulating pump 24, the heat conductive oil inlet 3 on cavity top, constitutes conduction oil circulation line C；Liquid distributor D is
Slot type liquid distributor, commercially available.Such as Fig. 2, Fig. 3, the groove type distributor 43 in liquid distributor is connected with technical grade benzoic acid import 4,
Use between the lower disc 34 being welded on groove type distributor and mother liquor overflow pipe 42 and threaded, the circular hole of lower disc is distributed
There is a lot of little liquid outlet 44.See that Fig. 2, liquid distributor D are slot type liquid distributor, mainly include groove type distributor 43, mother liquor overflow pipe 42,
The parts such as gear fluid cylinder 41, upper gear liquid part 36, lower block liquid part 37, level control part 38, support bar 39, wherein on mother liquor overflow pipe 43
Portion is with groove type distributor lower disc 34 for threadeding, and its sidewall surrounding offers upper mother solution obliquely and portals 40, and bottom is opened
Being provided with mother solution in circle and portal 40, surrounding is threadedly secured to slot type distribution around cylindric gear fluid cylinder 41, gear fluid cylinder 41
On the lower disc 34 of device, the external diameter of gear fluid cylinder 41 is more than the external diameter of mother liquor overflow pipe 42；Upper gear liquid part 36 is the fimbriatum stood upside down,
In the underface of mother liquor overflow pipe 42, its race diameter is more than the external diameter of gear fluid cylinder, upper gear liquid part and gear fluid cylinder and mother liquor overflow
Pipe leaves spacing up and down, upper gear liquid part offers lower mother solution and portals；Lower block liquid part 37 is that upright fimbriatum is at upper gear liquid part
The lower section of 36, the race diameter of lower block liquid part 37, less than the race diameter of upper gear liquid part 36, leaves certain between upper lower block liquid part
Interval, lower block liquid part 37 is in the inside of crystallizer 8, and diameter is less than the internal diameter of crystallizer, and support bar is threadingly attached to mother
In hydrorrhea flow tube 42, upper gear liquid part 36 and lower block liquid part 37 are welded on support bar 39；Level control part 38 is wide at the top and narrow at the bottom
Cylindrical body, band annular outer at the width of top, lower section is welded on crystallizer 8, upper lower block liquid part in the inside of level control part 38,
Liquid part 36 is kept off high in the annular outer aspect ratio of level control part 38, lower than mother liquor overflow pipe 42.Crystallization in falling-film crystallizer A
Pipe 8 is stainless steel tube, falling-film crystallizer tank body lower chamber be externally provided with high-quality benzoic acid outlet 15, benzoic acid mother liquor outlet 19,
Diaphoresis benzoic acid outlet 17.Such as Fig. 1, conduction oil storage tank has three, is respectively crystallization conduction oil storage tank 26, diaphoresis conduction oil storage tank
29, melted conduction oil storage tank 32, three conduction oil storage tanks are equipped with electric tracing or steam tracing and temperature sensor mouth.See
Fig. 3, Fig. 4, benzoic acid mother solution flow velocity in crystallizer 8 is by the number of the liquid outlet 44 on the disk 34 below groove type distributor
Amount, upper mother solution on mother liquor overflow pipe 42 portal 35 quantity and angle, upper gear liquid part 36 on lower mother solution portal 40 size,
The size of lower block liquid part 37 and angle and the angle of level control part 38 and height control.In lower block liquid part 37 and crystallizer 8
Span is from for the 1/10 of crystallizer internal diameter.
Its operation principle is as follows:
Crystallization process:
In benzoic acid mother solution storage tank, add the benzoic acid (GC purity 97.5～98.5%) of technical grade, conduction oil will be crystallized
The temperature of storage tank controls at 110～119 DEG C, the valve VI of Open valve V sum, starts heat conduction oil circulating pump VI, makes conduction oil exist
Circulate between conduction oil circulation line and falling-film crystallizer conduction oil cavity, control falling-film crystallizer conduction oil cavity inner temperature and exist
Between 110～119 DEG C, benzoic acid upper cavity and benzoic acid lower chamber temperature, between 125～130 DEG C, close valve I, valve
II, Open valve III and valve IV, start Recycling Mother Solution pump, make technical grade benzoic acid in falling-film crystallizer, liquid distributor and benzene first
Circulate between acid circulation line, when technical grade benzoic acid flows through in falling-film crystallizer crystallizer, understand at crystallizer intercrystalline, as
This circulation crystallization, when percent crystallization in massecuite reaches 50～70%, (percent crystallization in massecuite is the technical grade benzoic acid of benzoic acid Mass and addition of crystallization
The ratio of quality), stop Recycling Mother Solution pump, close valve IV, benzoic acid mother solution in emptying falling-film crystallizer (GC purity be 96.0～
97.0%), close valve III, stop heat conduction oil circulating pump, close the valve VI of valve V sum；
Sweating effort:
Close valve I, valve III, open valve II, control the temperature of diaphoresis conduction oil storage tank, at 120～125 DEG C, to open
Open valve VII and valve VIII, start heat conduction oil circulating pump, control falling-film crystallizer conduction oil cavity inner temperature at 120～125 DEG C
Between, make the crystal diaphoresis in falling-film crystallizer crystallizer, collect diaphoresis benzoic acid (GC purity is 97.0～98.0%), regularly
Sampling, stops heat conduction oil circulating pump when the benzoic content in perspiration is (GC purity is 99.2～99.4%), closes valve VII
With valve VIII, sweating effort terminates；
Melting process:
Close valve II, valve III, open valve I, control the temperature of melted conduction oil storage tank, at 130～135 DEG C, to open
Open valve Ⅸ and valve Ⅹ, start heat conduction oil circulating pump, control falling-film crystallizer conduction oil cavity inner temperature 130～135 DEG C, make
Crystal melt in falling-film crystallizer crystallizer, collects high-quality benzoic acid (GC purity is 99.5～99.9%), when without benzoic acid
During discharge, melting process terminates.
Claims (2)
1. a benzoic acid purified crystals device, including falling-film crystallizer (A), it is characterised in that falling-film crystallizer tank inner chamber by
Upper spacer (7) and lower clapboard (11) are divided into upper cavity (6), middle cavity (1) and lower chamber (13), and upper cavity (6) is provided with technical grade
Benzoic acid import (4), temperature sensor mouth (5), middle cavity (1) top is provided with heat conductive oil inlet (3), bottom is provided with conduction oil and goes out
Mouth (10), upper cavity (6) and lower chamber (13) are connected by the vertical crystallizer (8) of both ends open, and upper cavity is provided with in (6)
Liquid distributor (D), lower chamber (13) bottom is provided with benzoic acid outlet (14), and benzoic acid outlet (14) of lower chamber is connected by pipeline
Benzoic acid mother solution storage tank (21), Recycling Mother Solution pump (23), Recycling Mother Solution pump (23) connects technical grade benzoic acid import by pipeline
(4), conduction oil outlet (10) of middle cavity (1) bottom connects conduction oil storage tank and heat conduction oil circulating pump (24) by pipeline, leads
Circular-pump (24) connected by pipeline in the heat conductive oil inlet (3) on cavity top, in the liquid distributor (D) in upper cavity (6)
Groove type distributor (43) be connected with technical grade benzoic acid import (4) on upper cavity (6).
Crystallization apparatus the most according to claim 1, it is characterised in that conduction oil storage tank has three, respectively is crystallization and leads
Deep fat storage tank (26), diaphoresis conduction oil storage tank (29), melted conduction oil storage tank (32).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620378283.8U CN205549662U (en) | 2016-04-29 | 2016-04-29 | Benzoic acid purification crystallization device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620378283.8U CN205549662U (en) | 2016-04-29 | 2016-04-29 | Benzoic acid purification crystallization device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN205549662U true CN205549662U (en) | 2016-09-07 |
Family
ID=56805267
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201620378283.8U Active CN205549662U (en) | 2016-04-29 | 2016-04-29 | Benzoic acid purification crystallization device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN205549662U (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108681348A (en) * | 2018-08-07 | 2018-10-19 | 天津会自动化科技有限公司 | A kind of chemical industry melting tower intelligent temperature control system |
| CN109251140A (en) * | 2017-07-14 | 2019-01-22 | 辽宁华亿化工实业有限公司 | Benzoic acid method of purification and purifying plant |
| CN111393286A (en) * | 2020-03-20 | 2020-07-10 | 武汉有机实业有限公司 | Device and process for purifying benzoic acid by step-by-step circulating crystallization |
| CN112675568A (en) * | 2019-10-18 | 2021-04-20 | 中国石油化工股份有限公司 | Separation and purification device and separation and purification method |
| CN115400451A (en) * | 2022-08-12 | 2022-11-29 | 上海东庚化工技术有限公司 | Dynamic falling film crystallizer |
| CN117959753A (en) * | 2024-04-02 | 2024-05-03 | 河北惠尔信新材料股份有限公司 | Crystallization device for manufacturing high-grade ferrous sulfate heptahydrate |
-
2016
- 2016-04-29 CN CN201620378283.8U patent/CN205549662U/en active Active
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109251140A (en) * | 2017-07-14 | 2019-01-22 | 辽宁华亿化工实业有限公司 | Benzoic acid method of purification and purifying plant |
| CN108681348A (en) * | 2018-08-07 | 2018-10-19 | 天津会自动化科技有限公司 | A kind of chemical industry melting tower intelligent temperature control system |
| CN112675568A (en) * | 2019-10-18 | 2021-04-20 | 中国石油化工股份有限公司 | Separation and purification device and separation and purification method |
| CN112675568B (en) * | 2019-10-18 | 2022-04-05 | 中国石油化工股份有限公司 | Separation and purification device and separation and purification method |
| CN111393286A (en) * | 2020-03-20 | 2020-07-10 | 武汉有机实业有限公司 | Device and process for purifying benzoic acid by step-by-step circulating crystallization |
| CN115400451A (en) * | 2022-08-12 | 2022-11-29 | 上海东庚化工技术有限公司 | Dynamic falling film crystallizer |
| CN117959753A (en) * | 2024-04-02 | 2024-05-03 | 河北惠尔信新材料股份有限公司 | Crystallization device for manufacturing high-grade ferrous sulfate heptahydrate |
| CN117959753B (en) * | 2024-04-02 | 2024-06-14 | 河北惠尔信新材料股份有限公司 | Crystallization device for manufacturing high-grade ferrous sulfate heptahydrate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN205549662U (en) | Benzoic acid purification crystallization device | |
| CN205893225U (en) | All -in -one is made to vinegar solid state | |
| CN106906124A (en) | Aeration type bioreactor | |
| CN105503573B (en) | Method and device for separation treatment of sodium formate in NPG (neopentyl glycol) production technology | |
| CN201350217Y (en) | Dripping disk, drip storing unit, condensation unit, and drip condensation device unit formed by same and system | |
| CN104291273B (en) | One kind is applied to aromatic hydrocarbons abjection device and its technique after extraction column of hydrogen peroxide | |
| CN208218735U (en) | One kind being synthetically prepared the efficient purifying plant of 2- thiophene acetic acid recrystallization method | |
| CN106244413B (en) | Solid-state vinegar brewing integrated machine | |
| CN207286888U (en) | A kind of decoloration device prepared for environment-friendlyplasticizer plasticizer | |
| CN208182887U (en) | A kind of Ergol low-boiling-point substance continuous production benzoic acid system | |
| CN206621817U (en) | A kind of energy-conserving and environment-protective chlorophenesic acid continuous rectification system | |
| CN101744721A (en) | Drip pan, dripping material storing unit, condensation unit as well as device unit and system formed by thereof | |
| CN210009654U (en) | Ammonium sulfate cooling crystallization device | |
| CN209005247U (en) | A kind of Chinese patent drug production alcohol high efficiente callback tower | |
| CN210765250U (en) | Automatic continuous extraction device for obtaining raw wine from white spirit brewing by-product yellow water | |
| CN204815752U (en) | Steerable crystallization speed's crystallizer | |
| CN206109366U (en) | Novel fruit wine clarification filtration system | |
| CN206809812U (en) | A kind of destructive distillation cypress extract refining plant | |
| CN206008099U (en) | A kind of rotating disc type extraction washing integrated device | |
| CN202786552U (en) | Integrated type hollow fiber membrane spinning machine | |
| CN214808524U (en) | Single-tower continuous refining system for crude furfural | |
| CN205990354U (en) | A kind of iso-octyl palmitate production system | |
| CN205216238U (en) | Crude carbolic acid system of processing | |
| CN215539988U (en) | Washing kettle with quick separation function | |
| CN204563657U (en) | A kind of crystallization still for the preparation of trimethyl pyruvic acid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |