CN106748735A - Oxalic acid crystal circulates preparation facilities - Google Patents
Oxalic acid crystal circulates preparation facilities Download PDFInfo
- Publication number
- CN106748735A CN106748735A CN201611233593.1A CN201611233593A CN106748735A CN 106748735 A CN106748735 A CN 106748735A CN 201611233593 A CN201611233593 A CN 201611233593A CN 106748735 A CN106748735 A CN 106748735A
- Authority
- CN
- China
- Prior art keywords
- oxalic acid
- crystallizer
- forecooler
- mother liquor
- liquid
- 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.)
- Pending
Links
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 title claims abstract description 276
- 235000006408 oxalic acid Nutrition 0.000 title claims abstract description 92
- 239000013078 crystal Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000012452 mother liquor Substances 0.000 claims abstract description 50
- 239000007788 liquid Substances 0.000 claims abstract description 45
- 239000000203 mixture Substances 0.000 claims abstract description 30
- 238000007599 discharging Methods 0.000 claims abstract description 21
- 239000007787 solid Substances 0.000 claims abstract description 18
- 238000003860 storage Methods 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 13
- 230000004087 circulation Effects 0.000 claims abstract description 10
- 239000003507 refrigerant Substances 0.000 claims description 19
- 239000012530 fluid Substances 0.000 claims description 4
- 230000008676 import Effects 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 238000003780 insertion Methods 0.000 claims description 3
- 230000037431 insertion Effects 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 2
- 238000002425 crystallisation Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000004064 recycling Methods 0.000 description 3
- 244000025254 Cannabis sativa Species 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000002826 coolant Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000010413 mother solution Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- XEEVLJKYYUVTRC-UHFFFAOYSA-N oxomalonic acid Chemical compound OC(=O)C(=O)C(O)=O XEEVLJKYYUVTRC-UHFFFAOYSA-N 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000001839 systemic circulation Effects 0.000 description 1
Classifications
-
- 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
-
- 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
Landscapes
- 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 present invention relates to a kind of oxalic acid crystal circulation preparation facilities, belong to the chemical industry equipment for preparing oxalic acid crystal.The technical solution adopted by the present invention is：Oxalic acid crystal circulates preparation facilities, including crystallizer and forecooler, also include oxalic acid mother liquor storage facility and equipment for separating liquid from solid, the oxalic acid mother liquor storage facility is provided with pipeline and is passed through in crystallizer, the inlet of the forecooler accesses the middle and lower part position of crystallizer, the liquid outlet of forecooler accesses the top of crystallizer, the bottom of crystallizer sets solidliquid mixture discharging opening, solidliquid mixture discharging opening is passed through equipment for separating liquid from solid, solidliquid mixture is separated into oxalic acid crystal by equipment for separating liquid from solid, oxalic acid mother liquor and mother liquor containing nucleus and powder, the oxalic acid mother liquor containing nucleus and powder is passed through in crystallizer.
Description
Technical field
The present invention relates to a kind of oxalic acid crystal circulation preparation facilities, belong to the chemical industry equipment for preparing oxalic acid crystal.
Background technology
The preparation process operation of oxalic acid crystal is long, and in order to save the consumption of raw materials in preparing, industrialized oxalic acid is prepared all
Can be by the oxalic acid mother liquid recycling in preparation, to improve the utilization rate of oxalic acid.Existing oxalic acid crystal crystallizer mesoxalic acid is female
Liquid is one way flow, and the circulation process of oxalic acid mother liquor is also a lot, and this requires that the amount of oxalic acid mother liquor is very big, to be able to maintain that grass
Long-term operation prepared by acid crystal.
If can crystallize prepare in directly carry out oxalic acid Recycling Mother Solution, it is to avoid systemic circulation to the demand of oxalic acid mother liquor,
The raw material contribution of early stage will be improved, reduces cost will improve the preparation efficiency of oxalic acid crystal.
The content of the invention
The present invention provides a kind of oxalic acid crystal circulation preparation facilities, solves oxalic acid mother liquor and feeds intake in the circulating cycle greatly, and oxalic acid is brilliant
The low problem of body preparation efficiency.
To achieve the above object, the technical solution adopted by the present invention is：Oxalic acid crystal circulates preparation facilities, including crystallizer
And forecooler, also including oxalic acid mother liquor storage facility and equipment for separating liquid from solid, the oxalic acid mother liquor storage facility is provided with pipeline and leads to
Enter in crystallizer, the inlet of the forecooler accesses the middle and lower part position of crystallizer, the liquid outlet of forecooler accesses crystallizer
Top, the bottom of crystallizer sets solidliquid mixture discharging opening, and solidliquid mixture discharging opening is passed through equipment for separating liquid from solid, solid-liquid point
Solidliquid mixture is separated into oxalic acid crystal, oxalic acid mother liquor and mother liquor containing nucleus and powder from device, it is described to contain nucleus
Oxalic acid mother liquor with powder is passed through in crystallizer.
Preferably, the solidliquid mixture discharging opening of the crystallizer to equipment for separating liquid from solid section is additionally provided with agitator tank, Gu
Liquid mixture discharging opening to the conveyance conduit between agitator tank is provided with product pump.
Further preferably the forecooler is vertical body, and the two ends in forecooler are provided with the collection that dividing plate is closing
Sap cavity, top liquid collecting cavity to the heat exchange runner that insertion is provided between the liquid collecting cavity of bottom, heat exchange runner, forecooler tube wall and liquid collecting cavity
The refrigerant channel of dividing plate composition closing, the top of refrigerant channel is provided with refrigerant import, the bottom refrigerant exit of refrigerant channel.
Further preferred, the bottom of crystallizer is taper, and leakage fluid dram is set at the base angle of taper, and the solidliquid mixture goes out
Material mouth is arranged on the taper surface of taper, and solidliquid mixture discharging opening highest point is not higher than taper surface highest point.
Further preferably, the inlet of forecooler accesses the position of crystallizer in the top of bottom pyramidal, crystallizer
The position of crystallizer is accessed less than the inlet of forecooler in the oxalic acid crystal extreme higher position of interior precipitation.
Further preferred, the pipeline of the inlet access crystallizer middle and lower part of forecooler is provided with circulating pump, circulating pump
Circulation rate for 500 cubic metres per hour.
Further preferred, the pipeline to crystallizer of oxalic acid mother liquor storage facility is provided with surge tank, the front end of surge tank
Pipeline is provided with feed pump, and the rear end pipeline of surge tank is provided with control valve.
The advantage of the invention is that：
In the preparation of oxalic acid crystal, the short cycle is carried out to oxalic acid mother liquor by the crystallizer and forecooler that can circulate oxalic acid mother liquor
Circulation, improves the preparation efficiency of oxalic acid crystal；
By short periodic endless, the raw material input amount of early stage is reduced, reduce production cost；Reduce setting for storage mother liquor
It is standby, the quantity of equipment is reduced, reduce production cost.
Brief description of the drawings
Fig. 1 is the annexation figure of each equipment of the invention.
Fig. 2 is the structure chart of forecooler of the invention.
Reference：
The conveyance conduit 7 of 1 crystallizer, 2 forecooler, 35 solidliquid mixture discharging opening of oxalic acid mother liquor 4 equipment for separating liquid from solid of storage facility 6 is stirred
Mix the leakage fluid dram of 14 conical bottom of tank 8 product pump, 9 liquid collecting cavity, 10 heat exchange runner, 11 refrigerant channel, 12 refrigerant import, 13 refrigerant exit 15
16 circulating pump, 17 surge tank, 18 feed pump 19 controls valve.
Specific embodiment
The annexation of each equipment of oxalic acid crystal circulation preparation facilities of the present invention is as shown in figure 1, a kind of oxalic acid crystal is followed
Ring preparation facilities, including crystallizer 1 and forecooler 2, also including oxalic acid mother liquor storage facility 3 and equipment for separating liquid from solid 4, the grass
Acid mother liquor storage facility 3 is provided with pipeline and is passed through in crystallizer 1, and the inlet of the forecooler 2 accesses the middle and lower part position of crystallizer 1
Put, the liquid outlet of forecooler 2 accesses the top of crystallizer 1, the bottom of crystallizer 1 sets solidliquid mixture discharging opening 5, solid-liquid mixing
Thing discharging opening 5 is passed through equipment for separating liquid from solid 4, and the solidliquid mixture discharging opening 5 of crystallizer 1 is additionally provided between equipment for separating liquid from solid 4
Agitator tank 7, solidliquid mixture discharging opening 5 to the conveyance conduit between agitator tank 7 is provided with product pump 8.
Solidliquid mixture is separated into oxalic acid crystal, the oxalic acid mother liquor containing nucleus and powder and mother by equipment for separating liquid from solid 4
Liquid, the oxalic acid mother liquor containing nucleus and powder is passed through in crystallizer.Oxalic acid mother liquor containing nucleus and powder is in crystallizer
The interior crystallization that can promote oxalic acid mother liquor, improves crystallization rate.The oxalic acid mother liquor for not containing nucleus and powder is passed through oxalic acid homepage
In storage facility, prepare to reuse.
Equipment for separating liquid from solid 4 can be centrifuge, or belt vacuum filter.This can realize dividing for solid to come you
Separating process requirement.
Forecooler 1 is vertical body, and the two ends in forecooler 1 are provided with the liquid collecting cavity 9 that dividing plate is closing, top liquid collecting cavity
The heat exchange runner 10 of insertion, the dividing plate composition of heat exchange runner 10, forecooler tube wall and liquid collecting cavity are provided between 9 to bottom liquid collecting cavity 9
The refrigerant channel 11 of closing, the top of refrigerant channel 11 is provided with refrigerant import 12, the bottom refrigerant exit 13 of refrigerant channel 11.In advance
The pipeline that the inlet of cooler 1 accesses crystallizer middle and lower part is provided with circulating pump 16, and the circulation rate of circulating pump 16 is 500 cubes
Rice is per hour.
Forecooler 1 cools down the oxalic acid liquid in crystallizer, the oxalic acid liquid of cooling in crystallizer crystalline deposit in crystallizer 1
Bottom in conical bottom 14.Leakage fluid dram 15 is set at the base angle of conical bottom 14, the solidliquid mixture discharging opening 5 is arranged on taper
On the taper surface at bottom 14, the highest point of solidliquid mixture discharging opening 5 is not higher than taper surface highest point.
The oxalic acid that the inlet of forecooler 1 accesses precipitation of the position of crystallizer in the top of conical bottom, crystallizer 1 is brilliant
The position of crystallizer is accessed less than the inlet of forecooler in body extreme higher position.Prevent crystal oxalic acid that precooling is drawn in crystallizer
In device.
The pipeline to crystallizer of oxalic acid mother liquor storage facility 3 is provided with surge tank 17, and the front-end pipelines of surge tank 17 are provided with
Feed pump 18, the rear end pipeline of surge tank 18 is provided with control valve 19.After the oxalic acid liquid crystalization of crystallizer, oxalic acid is supplemented in time
Mother liquor, realization is continuously crystallized.
The course of work of the present invention in the preparation of oxalic acid crystal：
1st, the oxalic acid mother liquor for being dissolved with raw material is input into surge tank from storage facility, and be quantitatively adding for oxalic acid mother liquor by surge tank
To in crystallizer.The of short duration storage oxalic acid mother liquor of surge tank.Because the storage facility of oxalic acid mother liquor is defeated using pumping system to crystallizer
Enter, the amount of its input needs precise control.Surge tank is added, the speed of input oxalic acid mother liquor can be reduced, realize adding speed
It is controllable.
2nd, oxalic acid mother liquor crystalline deposit in crystallizer, while forecooler cools down the oxalic acid Recycling Mother Solution in crystallizer,
Improve crystallization rate.
Specific cyclic process of the volume oxalic acid mother liquor in crystallizer between forecooler, the oxalic acid mother liquor of crystalliser feet by
Circulating pump is input in the heat exchange runner 10 of forecooler, is passed through the coolant media of circulation in refrigerant channel 11, coolant media with change
Oxalic acid mother liquor in hot flow path 10 carries out recycle heat, takes away the heat in oxalic acid mother liquor, and the oxalic acid mother liquor after cooling is from crystallization
The top of device is again introduced into crystallizer.The cyclic process is back and forth carried out, and the oxalic acid composition that oxalic acid mother liquor is contained within gradually is crystallized
Precipitation.
3rd, crystalliser feet taper bottom set solidliquid mixture discharging opening 5 will precipitate oxalic acid crystallization and mixing
Oxalic acid mother liquor is delivered in agitator tank by delivery pump, and agitator tank stirs solidliquid mixture, then pass to centrifuge or
Belt vacuum filter realizes that solid is separated with liquid.
4th, finished product is after the solid drying that filter is isolated.The oxalic acid mother liquor containing nucleus and powder isolated
It is passed through in crystallizer again, nucleus and powder can promote the formation of crystal.The oxalic acid mother liquor for not containing nucleus and powder leads to
To enter prepare in the storage facility of oxalic acid mother liquor and reuse.
The present apparatus realizes the preparation for moving in circles of oxalic acid crystal, can save crystallize in prior art and is once accomplished by
Equipment required for then oxalic acid mother liquor is stored into subcrystalline process again again, improves the crystalline rate of oxalic acid.
Claims (7)
1. a kind of oxalic acid crystal circulates preparation facilities, including crystallizer (1) and forecooler (2), it is characterized in that, it is also female including oxalic acid
Liquid storage facility (3) and equipment for separating liquid from solid (4), the oxalic acid mother liquor storage facility (3) are provided with pipeline and are passed through crystallizer (1)
Interior, the inlet of the forecooler (2) accesses the middle and lower part position of crystallizer (1), and the liquid outlet of forecooler (2) accesses crystallizer
(1) top, the bottom of crystallizer (1) sets solidliquid mixture discharging opening (5), and solidliquid mixture discharging opening (5) is passed through solid-liquid point
From device（4）, equipment for separating liquid from solid（4）Solidliquid mixture is separated into oxalic acid crystal, the oxalic acid mother liquor containing nucleus and powder
And mother liquor, the oxalic acid mother liquor containing nucleus and powder is passed through in crystallizer.
2. oxalic acid crystal according to claim 1 circulates preparation facilities, it is characterized in that, the solid-liquid of the crystallizer (1) is mixed
Compound discharging opening (5) is to equipment for separating liquid from solid（4）Between be additionally provided with agitator tank (7), solidliquid mixture discharging opening (5) to agitator tank
(7) conveyance conduit between is provided with product pump (8).
3. oxalic acid crystal according to claim 1 circulates preparation facilities, it is characterized in that, the forecooler (2) is vertical
Body, the two ends in forecooler (2) are provided with the liquid collecting cavity (9) that dividing plate is closing, top liquid collecting cavity (9) to bottom liquid collecting cavity (9)
Between be provided with the heat exchange runner (10) of insertion, the refrigerant of the dividing plate composition closing of heat exchange runner (10), forecooler tube wall and liquid collecting cavity
Runner (11), the top of refrigerant channel (11) is provided with refrigerant import (12), the bottom refrigerant exit (13) of refrigerant channel (11).
4. oxalic acid crystal according to claim 3 circulates preparation facilities, it is characterized in that, the bottom of crystallizer (1) is taper
Bottom (14), sets leakage fluid dram (15) at the base angle of conical bottom (14), the solidliquid mixture discharging opening (5) is arranged on conical bottom (14)
Taper surface on, solidliquid mixture discharging opening (5) highest point is not higher than taper surface highest point.
5. oxalic acid crystal according to claim 4 circulates preparation facilities, it is characterized in that, the inlet of forecooler (2) is accessed
The oxalic acid crystal extreme higher position of precipitation of the position of crystallizer in the top of conical bottom, crystallizer (1) is entered less than forecooler
The position of liquid mouthful access crystallizer.
6. oxalic acid crystal according to claim 1 circulates preparation facilities, it is characterized in that, the inlet of forecooler (1) is accessed
The pipeline of crystallizer middle and lower part is provided with circulating pump (16), the circulation rate of circulating pump (16) for 500 cubic metres per hour.
7. oxalic acid crystal according to claim 1 circulates preparation facilities, it is characterized in that, oxalic acid mother liquor storage facility (3) is extremely
The pipeline of crystallizer is provided with surge tank (17), and the front-end pipelines of surge tank (17) are provided with feed pump (18), after surge tank (18)
End pipe road is provided with control valve (19).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611233593.1A CN106748735A (en) | 2016-12-28 | 2016-12-28 | Oxalic acid crystal circulates preparation facilities |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611233593.1A CN106748735A (en) | 2016-12-28 | 2016-12-28 | Oxalic acid crystal circulates preparation facilities |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106748735A true CN106748735A (en) | 2017-05-31 |
Family
ID=58921422
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611233593.1A Pending CN106748735A (en) | 2016-12-28 | 2016-12-28 | Oxalic acid crystal circulates preparation facilities |
Country Status (1)
| Country | Link |
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| CN (1) | CN106748735A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104478693A (en) * | 2014-12-23 | 2015-04-01 | 山东丰元化学股份有限公司 | Preparation method of refined oxalic acid |
| CN204319825U (en) * | 2014-12-23 | 2015-05-13 | 山东丰元化学股份有限公司 | Equipment of crystallisation by cooling in a kind of refining oxalic acid production process |
| CN105797422A (en) * | 2016-04-20 | 2016-07-27 | 西安航天华威化工生物工程有限公司 | Citric acid continuous cooling crystallization system and method thereof |
| CN206494870U (en) * | 2016-12-28 | 2017-09-15 | 山东丰元化学股份有限公司 | Oxalic acid crystal circulates preparation facilities |
-
2016
- 2016-12-28 CN CN201611233593.1A patent/CN106748735A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104478693A (en) * | 2014-12-23 | 2015-04-01 | 山东丰元化学股份有限公司 | Preparation method of refined oxalic acid |
| CN204319825U (en) * | 2014-12-23 | 2015-05-13 | 山东丰元化学股份有限公司 | Equipment of crystallisation by cooling in a kind of refining oxalic acid production process |
| CN105797422A (en) * | 2016-04-20 | 2016-07-27 | 西安航天华威化工生物工程有限公司 | Citric acid continuous cooling crystallization system and method thereof |
| CN206494870U (en) * | 2016-12-28 | 2017-09-15 | 山东丰元化学股份有限公司 | Oxalic acid crystal circulates preparation facilities |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
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Application publication date: 20170531 |