CN108203374A - Phosphorus pentoxide haze concentrates the method and device of dilute formic acid - Google Patents
Phosphorus pentoxide haze concentrates the method and device of dilute formic acid Download PDFInfo
- Publication number
- CN108203374A CN108203374A CN201611222209.8A CN201611222209A CN108203374A CN 108203374 A CN108203374 A CN 108203374A CN 201611222209 A CN201611222209 A CN 201611222209A CN 108203374 A CN108203374 A CN 108203374A
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- CN
- China
- Prior art keywords
- formic acid
- dilute
- phosphorus pentoxide
- reaction kettle
- dense
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Classifications
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
- B01J2219/00094—Jackets
Abstract
The invention discloses a kind of method and devices of phosphorus pentoxide haze concentration dilute formic acid, it is characterised in that：Pass through the device being made of components such as reaction kettle, packed tower, pump and wind turbines, phosphorus pentoxide is made to generate haze, and it is contacted on filler surface with dilute formic acid, it solves phosphorus pentoxide and dilute formic acid solution reaction is too fast, it is highly exothermic, generate the problem of localized hyperthermia decomposes formic acid, influences the formic acid rate of recovery.Have many advantages, such as that operating process facilitates simple and direct, product and byproduct is superior in quality, non-wastewater discharge, popularization and application will bring good social and economic benefit to manufacturing enterprise.
Description
First, technical field
The invention belongs to Production in Chemical Plant waste water recycling devices, are concentrated particularly with regard to a kind of phosphorus pentoxide haze
The method and device of dilute formic acid.
2nd, background technology
Formic acid generates a large amount of dilute formic acid solution during the uses such as industrial solvent are done.The boiling point of formic acid is 100.7
DEG C, there was only 0.7 DEG C, and constant boiling point is formed with water with the boiling-point difference of water, be difficult concentration dilute formic acid with conventional rectificating method.In the past
The method of purifying formic acid has many document reports, and only a small amount of production application is not all promoted.Such as：Patent of invention《It is a kind of
The processing method of metronidazole waste water》, 201110202387.5, Zhou Yongjun etc..Above-mentioned filter liquor is is steamed by its main thought
Send out, cool down, crystallizing, filtering sodium formate and sodium sulphate salt-mixture, be acidified salt-mixture with sulfuric acid, steam formic acid.But due to energy
Consumption is big, could not realize industrialization.
Someone adds in water absorbing agent phosphorus pentoxide in dilute formic acid solution evaporates after absorption moisture, and condensed steam obtains high concentration
Formic acid, evaporation raffinate are phosphoric acid.But phosphorus pentoxide and dilute formic acid solution reaction are too fast, highly exothermic, and part, which generates high temperature, to be made
Formic acid decomposes and impurity carbonization, influences the formic acid rate of recovery and phosphoric acid quality.Therefore, it is straight to be made waste water by some manufacturers for dilute formic acid
Run in and put, cause greatly to pollute to environment.
3rd, invention content
Present invention aim to solve above-mentioned technical problem, being provided for chemical enterprise a kind of can slow down phosphorus pentoxide
With dilute formic acid solution reaction speed, avoid part generate high temperature make formic acid decompose and impurity carbonization, with improve the formic acid rate of recovery and
The method and device of phosphoric acid quality.
The technical scheme is that：The method and device technological process of phosphorus pentoxide haze concentration dilute formic acid is as follows：
(1) appropriate dilute formic acid m kg are added in into reaction kettle；
(2) according to dilute formic acid mass percentage concentration CIt is dilute, required formic acid product mass percentage concentration CIt is dense, phosphoric acid containing five oxidation
Two phosphorus 72.5% and industrial phosphoric acid mass percentage concentration 85% calculate phosphorus pentoxide input amount M
m(1-CIt is dilute)=m CIt is dilute(1-CIt is dense)/CIt is dense+(M/0.725)(1-0.85)/0.85
m(1-CIt is dilute)-m CIt is dilute(1-CIt is dense)/CIt is dense=(M/0.725) (1-0.85)/0.85
M=[m (1-CIt is dilute)-m CIt is dilute(1-CIt is dense)/CIt is dense]0.725*0.85/(1-0.85)
(3) first start pump, acid solution in reaction kettle is sent to the leaching of packed tower top spray, reaction kettle is flow back under filler surface
In；
(4) start wind turbine afterwards, wind enters packed tower bottom, and tower top is risen to through filler layer gap, and returning to wind turbine through air hose enters
Mouthful；
(5) and then slowly continuous into wind turbine outlet conduits to put into phosphorus pentoxide, phosphorus pentoxide is by wind in air duct
Haze during rising with the wind through filler layer gap, absorbs generation phosphoric acid, with acid solution stream by the water in the acid solution of filler surface
Enter reaction kettle；
(6) M kg phosphorus pentoxides finish, then first Blowing stopper and pump successively, evaporate kettle liquid, generated formic acid steamed
Vapour is cold to doubt to obtain formic acid product, and kettle liquid temperature stops evaporation when being raised to 213 DEG C；
(7) phosphoric acid product that raffinate is 85% is steamed.
A kind of device of phosphorus pentoxide haze concentration dilute formic acid, it is by reaction kettle, packed tower, condenser and storagetank
It is formed Deng part, packed tower, the built-in filler of packed tower is set above reaction kettle；Reaction kettle side middle and lower part sets pump inlet pipe, pumps out
Mouth pipe enters in packed tower to be connected with top showerhead；Reaction kettle side surface upper part sets fan outlet tube, fan inlet pipe and packed tower
Top connects, and strap brake valve pipeline vertically upward is set above fan outlet tube, and pipeline is connected with hopper outlet above gate valve；Reaction
Kettle peripheral hardware heating jacket；The air inlet of condenser interior condenser tube is connected by tracheae with the exhaust outlet at the top of packed tower, and outlet is logical
The pipeline for crossing setting control of product valve is connected with storagetank.
The beneficial effects of the present invention are：In a manner that phosphorus pentoxide haze contacts on filler surface with dilute formic acid,
It solves phosphorus pentoxide and dilute formic acid solution reaction is too fast, highly exothermic, generating localized hyperthermia decomposes formic acid, influences formic acid
The problem of rate of recovery.Have many advantages, such as that operating process facilitates simple and direct, product and byproduct is superior in quality, non-wastewater discharge, push away
Wide application will bring good social and economic benefit to manufacturing enterprise.
4th, it illustrates
Fig. 1 is the structural diagram of the present invention.
In figure：1 is reaction kettle, and 2 be pump, and 3 be nozzle, and 4 be packed tower, and 5 be filler, and 6 be air hose, and 7 be loading hopper, and 8 are
Gate valve, 9 be wind turbine, and 10 be outlet valve, and 11 be heating valve, and 12 be condenser, and 13 be condenser pipe, and 14 be inlet valve, and 15 be product
Control valve, 16 be storagetank.
5th, specific embodiment
As shown in Figure 1, a kind of device of phosphorus pentoxide haze concentration dilute formic acid is by reaction kettle 1, packed tower 4, condensation
Device 12 and 16 grade parts of storagetank composition, 1 top of reaction kettle set packed tower 4,4 built-in filler 5 of packed tower；In 1 side of reaction kettle
Lower part sets 2 inlet tubes of pump, and 2 outlets of pump enter in packed tower 4 to be connected with top showerhead 3；1 side surface upper part of reaction kettle sets wind turbine 9
Outlet, 9 inlet tube of wind turbine connect with 4 top of packed tower, and band 8 pipeline of gate valve vertically upward, gate valve are set above 9 outlet of wind turbine
8 top pipelines are connected with the outlet of loading hopper 7；1 peripheral hardware heating jacket of reaction kettle；The air inlet of 12 interior condenser tube 13 of condenser passes through
Tracheae is connected with the exhaust outlet at 4 top of packed tower, exports by the way that the pipeline of control of product valve 15 is set to be connected with storagetank 16.
It concentrates the method for dilute formic acid and is as follows：
(1) appropriate dilute formic acid m kg are added in into reaction kettle 1；
(2) according to dilute formic acid mass percentage concentration CIt is dilute, required formic acid product mass percentage concentration CIt is dense, phosphoric acid containing five oxidation
Two phosphorus 72.5% and industrial phosphoric acid mass percentage concentration 85% calculate phosphorus pentoxide input amount M
m(1-CIt is dilute)=m CIt is dilute(1-CIt is dense)/CIt is dense+(M/0.725)(1-0.85)/0.85
m(1-CIt is dilute)-m CIt is dilute(1-CIt is dense)/CIt is dense=(M/0.725) (1-0.85)/0.85
M=[m (1-CIt is dilute)-m CIt is dilute(1-CIt is dense)/CIt is dense]0.725*0.85/(1-0.85)
(3) M kg phosphorus pentoxides are added in into loading hopper 7；
(4) first start pump 2, acid solution in reaction kettle 1 is sent to the leaching of 4 top spray of packed tower, is flow back under 5 surface of filler anti-
It answers in kettle 1；
(5) start wind turbine 9 afterwards, wind enters 4 bottom of packed tower, rises to tower top through 5 layer gap of filler, wind is returned to through air hose 6
9 entrance of machine；
(6) and then, gate valve 8 is opened, the slow continuous input phosphorus pentoxide into wind turbine outlet conduits, five oxygen in air duct
Change two phosphorus by wind haze, during rising with the wind through 5 layer gap of filler, generation is absorbed by the water in 5 surface acid solution of filler
Phosphoric acid flows into reaction kettle 1 with acid solution；
(7) phosphorus pentoxide finishes, first Blowing stopper 9 successively, pump 2 and gate valve 8, then, opens heating valve 11, water inlet successively
Valve 14 and control of product valve 15 evaporate kettle liquid, and generated formic acid vapor is cold doubtful that formic acid product, kettle liquid temperature are raised to 213
DEG C when stop evaporation；
(8) phosphoric acid product that raffinate is 85% is steamed.
Claims (2)
- A kind of 1. method of phosphorus pentoxide haze concentration dilute formic acid, it is characterised in that：Technological process is as follows(1) appropriate dilute formic acid m kg are added in into reaction kettle；(2) according to dilute formic acid mass percentage concentration CIt is dilute, required formic acid product mass percentage concentration CIt is dense, phosphoric acid contain phosphorus pentoxide 72.5% and industrial phosphoric acid mass percentage concentration 85%, calculate phosphorus pentoxide input amount Mm(1-CIt is dilute)=m CIt is dilute(1-CIt is dense)/CIt is dense+(M/0.725)(1-0.85)/0.85m(1-CIt is dilute)-m CIt is dilute(1-CIt is dense)/CIt is dense=(M/0.725) (1-0.85)/0.85M=[m (1-CIt is dilute)-m CIt is dilute(1-CIt is dense)/CIt is dense]0.725*0.85/(1-0.85)(3) first start pump, acid solution in reaction kettle is sent to the leaching of packed tower top spray, is flow back into reaction kettle under filler surface；(4) start wind turbine afterwards, wind enters packed tower bottom, rises to tower top through filler layer gap, fans entrance is returned to through air hose；(5) the and then slow continuous input phosphorus pentoxide into wind turbine outlet conduits, in air duct phosphorus pentoxide by wind haze, During rising with the wind through filler layer gap, generation phosphoric acid is absorbed by the water in the acid solution of filler surface, is flowed into acid solution anti- Answer kettle；(6) M kg phosphorus pentoxides finish, first Blowing stopper and pump successively, then, evaporate kettle liquid, and generated formic acid vapor is cold Formic acid product is doubted to obtain, kettle liquid temperature stops evaporation when being raised to 213 DEG C；(7) phosphoric acid product that raffinate is 85% is steamed.
- 2. a kind of device of phosphorus pentoxide haze concentration dilute formic acid, it is by reaction kettle, packed tower, condenser and storagetank etc. Part forms, and packed tower, the built-in filler of packed tower are set above reaction kettle；Reaction kettle side middle and lower part sets pump inlet pipe, pump discharge Pipe enters in packed tower and is connected with top showerhead；Reaction kettle side surface upper part sets fan outlet tube, fan inlet pipe and filler tower top Portion connects, and strap brake valve pipeline vertically upward is set above fan outlet tube, and pipeline is connected with hopper outlet above gate valve；Reaction kettle Peripheral hardware heating jacket；The air inlet of condenser interior condenser tube is connected by tracheae with the exhaust outlet at the top of packed tower, and outlet passes through The pipeline of setting control of product valve is connected with storagetank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611222209.8A CN108203374A (en) | 2016-12-19 | 2016-12-19 | Phosphorus pentoxide haze concentrates the method and device of dilute formic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611222209.8A CN108203374A (en) | 2016-12-19 | 2016-12-19 | Phosphorus pentoxide haze concentrates the method and device of dilute formic acid |
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|---|---|
| CN108203374A true CN108203374A (en) | 2018-06-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201611222209.8A Pending CN108203374A (en) | 2016-12-19 | 2016-12-19 | Phosphorus pentoxide haze concentrates the method and device of dilute formic acid |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101391945A (en) * | 2008-10-27 | 2009-03-25 | 浙江工业大学 | Novel purification method for formic acid |
| CN104261502A (en) * | 2014-09-26 | 2015-01-07 | 马军 | Treatment method and device of wastewater containing organic solvent |
-
2016
- 2016-12-19 CN CN201611222209.8A patent/CN108203374A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101391945A (en) * | 2008-10-27 | 2009-03-25 | 浙江工业大学 | Novel purification method for formic acid |
| CN104261502A (en) * | 2014-09-26 | 2015-01-07 | 马军 | Treatment method and device of wastewater containing organic solvent |
Non-Patent Citations (1)
| Title |
|---|
| 中华人民共和国长江海事局: "《长江危险货物运输应急处置手册》", 30 April 2013, 武汉理工大学出版社 * |
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Application publication date: 20180626 |