CN102671412B - Sublimation-method pyrogallic acid cold trap recovery device - Google Patents
Sublimation-method pyrogallic acid cold trap recovery device Download PDFInfo
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- CN102671412B CN102671412B CN201210151700.1A CN201210151700A CN102671412B CN 102671412 B CN102671412 B CN 102671412B CN 201210151700 A CN201210151700 A CN 201210151700A CN 102671412 B CN102671412 B CN 102671412B
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- crystallizer
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- trap
- pyrogallic acid
- sublimator
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses a sublimation-method pyrogallic acid cold trap recovery device. The bottom part of a sublimator (2) is provided with an electric heater (1); the outlet of the sublimator (2) is connected with a crystallizer (3); the tail part of the crystallizer (3) is provided with a vacuum system connecting pipe (5); six crystallizer cold traps (4) are arranged above the interior of the crystallizer (3); a receiver (13) is arranged below the interior of the crystallizer (3); the crystallizer cold traps (4) are connected with pipelines outside the crystallizer (3); external connectors above the six crystallizer cold traps (4) are connected onto an inlet pipeline in parallel; butt joint pipe orifices on the side faces of the bottom parts of the six crystallizer cold traps (4) are connected onto an outlet pipeline in parallel; the inlet pipeline above the six crystallizer cold traps (4) is connected with a superheated steam inlet pipe (8) and a cooling water inlet pipe (9); and parallel outlet pipelines on the side faces of the bottom parts of the six crystallizer cold traps (4) are connected with an outlet return pipe (11). According to the sublimation-method pyrogallic acid cold trap recovery device disclosed by the invention, the product purity and the recovery rate are increased, and the occupied area of equipment is greatly reduced.
Description
Technical field
The invention belongs to chemical industry equipment field, relate in particular to a kind of sublimed method pyrogallic acid cold-trap and reclaim crystallization apparatus.
Background technology
Existing pyrogallic acid sublimed method process units, pyrogallic acid reclaims and is natural sedimentation recovery, and its weak point is:
1, because the fine crystal of pyrogallic acid is suspended in the air, be difficult to landing, finally by powerful vacuum system, aspirated in vavuum pump gas washing system, cause product loss.
2, because crystallizer is metal manufacture, the receiver that bears pyrogallic acid is also metal manufacture, and the characteristic of pyrogallic acid is to be easy to generate complex compound with metal ion, thereby affects product purity.
3, because pyrogallic acid reclaims, adopt natural sedimentation to reclaim, make crystallizer very long, floor space is large, and device fabrication cost is relatively high.
Summary of the invention
A kind of product purity and the rate of recovery of having improved that the object of the invention is to overcome above-mentioned shortcoming and provide, the sublimed method pyrogallic acid cold-trap that greatly reduces occupation area of equipment reclaims crystallization apparatus.
Sublimed method pyrogallic acid cold-trap of the present invention reclaims crystallization apparatus, comprises electric heater, sublimator and crystallizer, wherein: electric heater is installed in the bottom of sublimator, and the outlet of sublimator is connected with crystallizer; Crystallizer afterbody is provided with vacuum system tube connector, six crystallizer cold-traps are installed in the top of crystallizer inside, the below of crystallizer inside is provided with receiver, crystallizer cold-trap top and the bottom sides docking mouth of pipe are connected with the pipeline of crystallizer outside, six crystallizer cold-trap top external interfaces are parallel on inlet pipeline, and six crystallizer cold-trap bottom sides docking mouths of pipe are parallel on outlet conduit;
The inlet pipeline of six crystallizer cold-trap tops is connected with cooling water inlet pipe with superheated steam inlet tube;
The outlet conduit in parallel of six crystallizer cold-trap bottom sides is connected with outlet return duct;
Crystallizer is provided with mould temperature meter;
Sublimator below is provided with sublimator thermometer.
Above-mentioned sublimed method pyrogallic acid cold-trap reclaims crystallization apparatus, wherein: vacuum system tube connector is provided with vacuum system tube connector valve.
Above-mentioned sublimed method pyrogallic acid cold-trap reclaims crystallization apparatus, wherein: the cold screen material of crystallizer cold-trap requires as polytetrafluoroethylene (PTFE) or enamel.
Above-mentioned sublimed method pyrogallic acid cold-trap reclaims crystallization apparatus, wherein:, superheated steam inlet tube is provided with superheated steam imported valve, at cooling water inlet Guan Shangshe cooling water inlet valve.
Above-mentioned sublimed method pyrogallic acid cold-trap reclaims crystallization apparatus, wherein:, outlet return duct is provided with outlet return duct valve.
Above-mentioned sublimed method pyrogallic acid cold-trap reclaims crystallization apparatus, wherein: the measuring probe of mould temperature meter contacts with the outer surface of crystallizer cold-trap.
The present invention compared with prior art, there is obvious beneficial effect, as can be known from the above technical solutions: the present invention adopts, in pyrogallic acid crystallizer, cold-trap is set, make to reclaim after the pyrogallic acid condensation of gas of flag heat the method for pyrogallic acid, make the fine crystal of pyrogallic acid that is difficult to landing also can be adsorbed on crystallizer cold-trap at once, reduce pyrogallic acid micro crystal and aspirated into the intrasystem quantity of vavuum pump gas washing by powerful vacuum system, improve product recovery rate.Also reduced contacting of pyrogallic acid crystalline solid and metal ion, the metal ion content of reduction product pyrogallic acid simultaneously; Reduce occupation area of equipment, the equipment volume of former crystallizer is dwindled to one times.
Accompanying drawing explanation
Accompanying drawing is structural representation of the present invention.
Mark in figure:
1, electric heater; 2, sublimator; 3, crystallizer; 4, crystallizer cold-trap; 5, vacuum system tube connector; 6, vacuum system tube connector valve; 7, superheated steam imported valve; 8, superheated steam inlet tube; 9, cooling water inlet pipe; 10, cooling water inlet valve; 11, outlet return duct; 12, outlet return duct valve; 13, receiver; 14, mould temperature meter; 15, sublimator thermometer.
The specific embodiment
Below in conjunction with accompanying drawing and preferred embodiment, the sublimed method pyrogallic acid cold-trap proposing according to the present invention is reclaimed to the crystallization apparatus specific embodiment, feature and effect thereof, be described in detail as follows.
Referring to accompanying drawing, sublimed method pyrogallic acid cold-trap reclaims crystallization apparatus, comprises electric heater 1, sublimator 2 and crystallizer 3, wherein:
Electric heater 1 is installed in the bottom of sublimator 2, and the outlet of sublimator 2 is connected with crystallizer 3 use flanges, is provided with the vacuum system tube connector 5 of access vacuum system at crystallizer 3 afterbodys, and vacuum system tube connector 5 is provided with vacuum system tube connector valve 6; Six crystallizer cold-traps 4 are installed in the top of crystallizer 3 inside, and the cold screen material of crystallizer cold-trap 4 requires as polytetrafluoroethylene (PTFE) or enamel, and the below of crystallizer 3 inside is provided with receiver 13; Crystallizer cold-trap 4 tops and the bottom sides docking mouth of pipe are connected with the pipeline of crystallizer 3 outsides and good seal, prevent from revealing, six crystallizer cold-trap 4 top external interfaces are parallel on inlet pipeline, and six crystallizer cold-trap 4 bottom sides docking mouths of pipe are parallel on outlet conduit;
The inlet pipeline of six crystallizer cold-trap 4 tops is connected with cooling water inlet pipe 9 with superheated steam inlet tube 8, superheated steam inlet tube 8 is provided with superheated steam imported valve 7 and accesses vapour system, establishes cooling water inlet valve 10 and access cooling water system on cooling water inlet pipe 9;
The outlet conduit in parallel of six crystallizer cold-trap bottom sides is connected with outlet return duct 11, and outlet return duct 11 is provided with outlet return duct valve 12 and accesses water reclamation system;
Crystallizer 3 is provided with mould temperature meter 14, and the measuring probe of mould temperature meter 14 must touch the outer surface of crystallizer cold-trap 4;
Sublimator 2 places, below are provided with sublimator thermometer 15, must not touch gallic acid material.
Operation principle is as follows:
Before a, production, below crystallizer 3 inside, put into receiver 13, shut crystallizer 3 afterbody discharge doors;
At the interior input gallic acid of sublimator 2 raw material, the hatch door of sublimator 2 is shut airtightly simultaneously, open vacuum system tube connector valve 6 after opening vacuum system, sublimator 2 and crystallizer 3 are evacuated;
B, open cooling water inlet valve 10, crystallizer cold-trap 4 is carried out cooling, regulate the size of cooling water inlet valve 10, see mould temperature meter 14, allow crystallizer cold-trap 4 panels reach 5 ℃;
C, start electric heater 1, to the interior gallic acid material of sublimator 2 heat, decarboxylation, distillation, temperature is controlled and is seen sublimator thermometer 15;
D, when sublimator 2 is heated to uniform temperature, the gallic acid material in sublimator 2 starts decarboxylation, distillation for pyrogallic acid, discharges CO simultaneously
2gas, the pyrogallic acid under high temperature is also gas, at vacuum state and CO
2under the state of gas drainage, gas pyrogallic acid flows to crystallizer 3 through the connector of sublimator 2 and crystallizer 3;
E, gas pyrogallic acid enter after crystallizer 3, touches and only have 5 ℃
Crystallizer cold-trap 4 panels, gas pyrogallic acid is cooled to crystal at once, and pyrogallic acid crystal after crystallization will condense and is attached on crystallizer cold-trap 4 panels;
F, the interior gallic acid of sublimator 2 constantly carry out decarboxylation, distillation, from sublimator 2, flow to the gas pyrogallic acid of crystallizer 3 and at crystallizer cold-trap 4 panels, adsorbed pyrogallic acid crystal polarizations, utilize this polarity absorption to continue to flow through the gas pyrogallic acid coming, gas pyrogallic acid and crystal pyrogallic acid continue to condense, and are jointly attached on heat exchanger panel;
After g, the whole decarboxylic reactions of the interior gallic acid of sublimator 2, first close electric heater 1, then close cooling water inlet valve 10, and then opening superheated steam imported valve 7, crystallizer cold-trap 4 is set to heating mode, when crystallizer cold-trap 4 panels reach 130 ℃, on crystallizer cold-trap 4 panels, adsorb pyrogallic acid crystal and start gradually melting and be shed in the receiver of polytetrafluoroethylene (PTFE) material, through the pyrogallic acid crystal that adsorbs on crystallizer cold-trap 4 panels for 10 to 20 minutes and can whole meltings come off;
H, close vacuum system tube connector valve 6; put into high-purity nitrogen destruction system vacuum and protect pyrogallic acid material simultaneously; open crystallizer 3 afterbody discharge doors and pull out the receiver 13 of filling pyrogallic acid material, send into that the workshop of selecting materials is pulverized, classification, packing.
The above, it is only preferred embodiment of the present invention, not the present invention is done to any pro forma restriction, any technical solution of the present invention content that do not depart from, any simple modification, equivalent variations and the modification above embodiment done according to technical spirit of the present invention, all still belong in the scope of technical solution of the present invention.
Claims (6)
1. a sublimed method pyrogallic acid cold-trap reclaims crystallization apparatus, comprise electric heater (1), sublimator (2) and crystallizer (3), it is characterized in that: electric heater (1) is installed in the bottom of sublimator (2), and the outlet of sublimator (2) is connected with crystallizer (3); Crystallizer (3) afterbody is provided with vacuum system tube connector (5), six crystallizer cold-traps (4) are installed in the inner top of crystallizer (3), the inner below of crystallizer (3) is provided with receiver (13), crystallizer cold-trap (4) top and the bottom sides docking mouth of pipe pipeline outside with crystallizer (3) are connected, six crystallizer cold-traps (4) top external interface is parallel on inlet pipeline, and six crystallizer cold-traps (4) bottom sides docking mouth of pipe is parallel on outlet conduit;
The inlet pipeline of six crystallizer cold-traps (4) top is connected with cooling water inlet pipe (9) with superheated steam inlet tube (8);
The outlet conduit in parallel of six crystallizer cold-trap bottom sides is connected with outlet return duct (11);
Crystallizer (3) is provided with mould temperature meter (14);
Place, sublimator (2) below is provided with sublimator thermometer (15).
2. sublimed method pyrogallic acid cold-trap as claimed in claim 1 reclaims crystallization apparatus, it is characterized in that: vacuum system tube connector (5) is provided with vacuum system tube connector valve (6).
3. sublimed method pyrogallic acid cold-trap as claimed in claim 1 or 2 reclaims crystallization apparatus, it is characterized in that: the cold screen material of crystallizer cold-trap (4) requires as polytetrafluoroethylene (PTFE) or enamel.
4. sublimed method pyrogallic acid cold-trap as claimed in claim 3 reclaims crystallization apparatus, it is characterized in that: superheated steam inlet tube (8) is provided with superheated steam imported valve (7), establishes cooling water inlet valve (10) on cooling water inlet pipe (9).
5. sublimed method pyrogallic acid cold-trap as claimed in claim 4 reclaims crystallization apparatus, it is characterized in that: outlet return duct (11) is provided with outlet return duct valve (12).
6. sublimed method pyrogallic acid cold-trap as claimed in claim 5 reclaims crystallization apparatus, it is characterized in that: the measuring probe of mould temperature meter (14) contacts with the outer surface of crystallizer cold-trap (4).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210151700.1A CN102671412B (en) | 2012-05-16 | 2012-05-16 | Sublimation-method pyrogallic acid cold trap recovery device |
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| CN201210151700.1A CN102671412B (en) | 2012-05-16 | 2012-05-16 | Sublimation-method pyrogallic acid cold trap recovery device |
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| CN102671412A CN102671412A (en) | 2012-09-19 |
| CN102671412B true CN102671412B (en) | 2014-09-24 |
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| CN107445804A (en) * | 2017-08-25 | 2017-12-08 | 贵州自然生物科技有限公司 | A kind of high-purity pyrogallol production method |
| CN112742061A (en) * | 2020-12-11 | 2021-05-04 | 安徽金禾实业股份有限公司 | Cooling device and cooling method for maltol sublimation section |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2873284Y (en) * | 2005-11-02 | 2007-02-28 | 戴汉松 | Sublimation device for separating and purifying natural product |
| CN101003012A (en) * | 2006-12-27 | 2007-07-25 | 中国科学院成都有机化学有限公司 | Method for producing novel catalytic film reactor |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007044592A (en) * | 2005-08-08 | 2007-02-22 | Canon Inc | Sublimation/purification apparatus |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2873284Y (en) * | 2005-11-02 | 2007-02-28 | 戴汉松 | Sublimation device for separating and purifying natural product |
| CN101003012A (en) * | 2006-12-27 | 2007-07-25 | 中国科学院成都有机化学有限公司 | Method for producing novel catalytic film reactor |
Non-Patent Citations (1)
| Title |
|---|
| JP特开2007-044592A 2007.02.22 |
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Effective date of registration: 20160912 Address after: 553004 Leap Road, Hongqiao New District, Zhongshan Economic Development Zone, Guizhou, Liupanshui Patentee after: Guizhou natural biological science and Technology Co Ltd Address before: Zijin Mountain District in Guizhou province Liupanshui City Road 553004 South Patentee before: Liupanshui Shenchi Biotechnology Co., Ltd. |
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Granted publication date: 20140924 Termination date: 20200516 |