CN105854570A - New mercaptopropionic-acid tail gas treating technology - Google Patents
New mercaptopropionic-acid tail gas treating technology Download PDFInfo
- Publication number
- CN105854570A CN105854570A CN201610427464.XA CN201610427464A CN105854570A CN 105854570 A CN105854570 A CN 105854570A CN 201610427464 A CN201610427464 A CN 201610427464A CN 105854570 A CN105854570 A CN 105854570A
- Authority
- CN
- China
- Prior art keywords
- tail gas
- mercaptopropionic
- sodium carbonate
- sodium
- acid
- 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.)
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/77—Liquid phase processes
- B01D53/78—Liquid phase processes with gas-liquid contact
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
- B01D53/52—Hydrogen sulfide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/02—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of thiols
- C07C319/04—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of thiols by addition of hydrogen sulfide or its salts to unsaturated compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/02—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of thiols
- C07C319/12—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of thiols by reactions not involving the formation of mercapto groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/26—Separation; Purification; Stabilisation; Use of additives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/30—Alkali metal compounds
- B01D2251/304—Alkali metal compounds of sodium
Abstract
The invention relates to a treating technology for hydrogen-sulfide tail gas in the mercaptopropionic-acid production process, and aims at providing a new mercaptopropionic-acid tail gas treating technology which is stable in production and capable of reducing production cost. The new mercaptopropionic-acid tail gas treating technology includes the steps that hydrogen-sulfide tail gas is led into a sodium hydroxide water solution, absorption is carried out to obtain absorption liquid, and the content of sodium carbonate in the solution is detected in real time; when the mass fraction of the sodium carbonate is increased to 10%, the absorption liquid is transferred to a reaction kettle, materials which are obtained through calcium chloride crystallizing and have the molar ratio equal to sodium carbonate are added and filtered under the stirring condition, and filtered liquid is used for allowing sodium hydrosulfide ingredients to be returned to a synthesis procedure. According to the new mercaptopropionic-acid tail gas treating technology, the crystallization plugging condition is avoided when the hydrogen-sulfide tail gas is treated, filtered liquid obtained after calcium salt is removed can be newly used for an addition reaction of acrylonitrile and sodium hydrosulfide, filtered calcium carbonate can be used as a product through simple treating, and it is avoided that due to precipitation of sodium carbonate, whole production operation is influenced; the stability of tail-gas treating technology is greatly improved, and the production cost of mercaptopropionic acid is reduced.
Description
Technical field
The present invention relates to one and add mercaptopropionic acid tail gas treatment process, be specifically related to a kind of mercaptopropionic acid and produced
The process technique of hydrogen sulfide tail gas in journey.
Background technology
Mercaptopropionic acid (CAS NO.:107-96-0) is a kind of poisonous transparency liquid, has strong sulfide gas
Taste, its another name has β-mercaptopropionic acid, sulphur for lactic acid, 3-mercaptopropionic acid, Β-sulphur for lactic acid, Β-sulphur hydrogen
Base propionic acid, 3-mercaptopropionic acid, BETA-mercaptopropionic acid, 3-thiolactic acid, 3-thiohydracrylic acid etc..Sulfydryl third
Acid is a kind of important organic synthesis raw material, is the intermediate of medicine fenarol, is also pvc material
Stabilizer.In prior art, after generally using acrylonitrile and NaHS addition reaction, acidolysis synthesis prepares.
In mercaptopropionic acid production process, owing to synthetic reaction requires NaHS excess, in acidification process
The a large amount of hydrogen sulfide gas of middle generation, it is necessary to reclaim and be used, in order to prevent the hydrogen sulfide pollution to environment.
In conventional technological design, hydrogen sulfide gas absorbs through 3 grades of membrane types, with NaOH as absorbent, by
Step obtains the sodium hydrosulfide that content is 20%.Then the absorbing liquid reclaimed returns to burden process, with 70%
NaHS be configured to regulation concentration, be circulated use.
In actual production process, it has been found that absorbing liquid is along with the increase of absorption quantity, in absorbing liquid progressively
Crystal is had to separate out.The when of arriving certain, absorption tower or line clogging, impact is even caused to produce normal
Run.
Summary of the invention
The invention aims to provide a kind of and produce the mercaptopropionic acid tail gas stable, production cost can be reduced
New Process for Treatment.
For achieving the above object, the technical solution used in the present invention is: mercaptopropionic acid vent gas treatment new technology bag
Include step:
A. carry out absorption during hydrogen sulfide tail gas is passed through sodium hydrate aqueous solution to be absorbed liquid, to the carbon in solution
Acid sodium content detects in real time；
B., when sodium carbonate mass fraction increases to 10%, absorbing liquid is transferred in reactor, at stirring condition
Under, add the calcium chloride with sodium carbonate equimolar ratio, react through 0.4-1h, reduce mixing speed stirring
0.5-1h；
C. gained material filters, and filtrate is back to synthesis procedure for NaHS dispensing.
Owing to passing through the analysis separating out crystal in conventional exhaust absorption system pipeline, its main component is carbonic acid
Sodium.Sodium carbonate solubility in sodium hydrosulfide is relatively low, and especially as the decline of temperature, solubility is entered
One step reduces.Thus cause sodium carbonate to separate out.The source of sodium carbonate is mainly raw material NaHS.According to right
The NaHS raw material of 70% is analyzed, and wherein the content of sodium carbonate fluctuates between 1%-5%.This part
Sodium carbonate generates carbon dioxide and sodium chloride with hydrochloric acid reaction synthesizing liquid acidifying when.Sodium chloride enters water
Solution system, carbon dioxide enters exhaust gas recovery system, is absorbed by NaOH and regenerates sodium carbonate.So
Circulation so that in system, carbonate content is stepped up, impact produces.Therefore the present invention strictly controls absorbing liquid
In carbonate content, the absorbing liquid transfiniting sodium carbonate carries out calcium chloride process, the filtrate obtained after filtration
For saline solution, acrylonitrile and NaHS addition reaction can be reused for.
It is further preferred that stirring reaction 0.5h after adding calcium chloride in described step B, reduce mixing speed
Stirring 0.5h.
Further, after reducing mixing speed in described step B, mixing speed is not higher than 30r/min.
It is further preferred that mixing speed is 10-20r/min after reducing mixing speed in described step B.
Further, described filtration step is for be transported in chamber filter press carry out press filtration by material filter pressing pump
Separating, filter cake, through cyclic washing and press filtration again, obtains calcium carbonate filter cake.
The present invention obtains after hydrogen sulfide tail gas processes the situation that Crystallization Plugging will not occur, and removal calcium salt
Filtrate can be reused for acrylonitrile and NaHS addition reaction, and the calcium carbonate leached is through simple process
As product, not only make whole exhaust treatment system to be stably normally carried out, also ensure that synthesis simultaneously
Reaction and being normally carried out of acidolysis reaction, it is to avoid affect whole production run due to the precipitation of sodium carbonate salt,
Substantially increase the stability of tail gas treatment process, reduce the production cost of mercaptopropionic acid.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described.Described embodiment is only the excellent of the present invention
Selecting embodiment, be not limited to the present invention, for a person skilled in the art, the present invention can
There to be various modifications and variations.All within the spirit and principles in the present invention, any amendment of being made, equivalent
Replacement, improvement etc., should be included within the scope of the present invention.
Embodiment one
Hydrogen sulfide tail gas is passed through in sodium hydrate aqueous solution and carries out absorption and be absorbed liquid, to the carbonic acid in solution
Sodium content detects in real time；When sodium carbonate mass fraction increases to 10%, absorbing liquid is transferred to reactor
In, under agitation, add the calcium chloride with sodium carbonate equimolar ratio, react through 1h, reduce stirring
Speed continues stirring 0.5h to 15r/min；Gained material filter pressing pump is transported in chamber filter press carry out press filtration
Separating, filter cake, through cyclic washing and press filtration again, obtains calcium carbonate filter cake, and filtrate is joined for NaHS
Material is back to synthesis procedure.
Embodiment two
Hydrogen sulfide tail gas is passed through in sodium hydrate aqueous solution and carries out absorption and be absorbed liquid, to the carbonic acid in solution
Sodium content detects in real time；When sodium carbonate mass fraction increases to 10%, absorbing liquid is transferred to reactor
In, under agitation, adding the calcium chloride with sodium carbonate equimolar ratio, react through 0.5h, reduction is stirred
Mix speed and continue stirring 0.8h to 30r/min；Gained material filter pressing pump is transported in chamber filter press press
Filter separates, and filter cake, through cyclic washing and press filtration again, obtains calcium carbonate filter cake, and filtrate is used for NaHS
Dispensing is back to synthesis procedure.
Embodiment three
Hydrogen sulfide tail gas is passed through in sodium hydrate aqueous solution and carries out absorption and be absorbed liquid, to the carbonic acid in solution
Sodium content detects in real time；When sodium carbonate mass fraction increases to 10%, absorbing liquid is transferred to reactor
In, under agitation, adding the calcium chloride with sodium carbonate equimolar ratio, react through 0.4h, reduction is stirred
Mix speed and continue stirring 0.5h to 10r/min；Gained material filter pressing pump is transported in chamber filter press press
Filter separates, and filter cake, through cyclic washing and press filtration again, obtains calcium carbonate filter cake, and filtrate is used for NaHS
Dispensing is back to synthesis procedure.
Claims (5)
1. mercaptopropionic acid vent gas treatment new technology, it is characterised in that: include step:
A. carry out absorption during hydrogen sulfide tail gas is passed through sodium hydrate aqueous solution to be absorbed liquid, to the carbon in solution
Acid sodium content detects in real time；
B., when sodium carbonate mass fraction increases to 10%, absorbing liquid is transferred in reactor, at stirring condition
Under, add the calcium chloride with sodium carbonate equimolar ratio, react through 0.4-1h, reduce mixing speed stirring
0.5-1h；
C. gained material filters, and filtrate is back to synthesis procedure for NaHS dispensing.
Mercaptopropionic acid vent gas treatment new technology the most according to claim 1, it is characterised in that: described step
Rapid B adds stirring reaction 0.5h after calcium chloride, reduces mixing speed stirring 0.5h.
Mercaptopropionic acid vent gas treatment new technology the most according to claim 1, it is characterised in that: described step
After reducing mixing speed in rapid B, mixing speed is not higher than 30r/min.
Mercaptopropionic acid vent gas treatment new technology the most according to claim 1, it is characterised in that: described step
In rapid B, after reduction mixing speed, mixing speed is 10-20r/min.
Mercaptopropionic acid vent gas treatment new technology the most according to claim 1, it is characterised in that: described mistake
Filter step is for be transported in chamber filter press carry out press filtration separation by material filter pressing pump, and filter cake is through repeatedly washing
Wash and press filtration again, obtain calcium carbonate filter cake.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610427464.XA CN105854570A (en) | 2016-06-16 | 2016-06-16 | New mercaptopropionic-acid tail gas treating technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610427464.XA CN105854570A (en) | 2016-06-16 | 2016-06-16 | New mercaptopropionic-acid tail gas treating technology |
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| Publication Number | Publication Date |
|---|---|
| CN105854570A true CN105854570A (en) | 2016-08-17 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610427464.XA Pending CN105854570A (en) | 2016-06-16 | 2016-06-16 | New mercaptopropionic-acid tail gas treating technology |
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| Country | Link |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110559828A (en) * | 2019-09-06 | 2019-12-13 | 天津大学 | Small tail gas absorption and deodorization device for sludge composting tail gas treatment |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1997023686A1 (en) * | 1995-12-22 | 1997-07-03 | Combustion Engineering, Inc. | Process for the conversion of calcium sulfide |
| CN101337661A (en) * | 2007-07-04 | 2009-01-07 | 褚亚华 | Method for preparing sodium hydrosulfide |
| CN105198122A (en) * | 2015-10-26 | 2015-12-30 | 刘阳生 | Resource utilization method of waste hydrochloric acid containing heavy metal lead and iron |
-
2016
- 2016-06-16 CN CN201610427464.XA patent/CN105854570A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1997023686A1 (en) * | 1995-12-22 | 1997-07-03 | Combustion Engineering, Inc. | Process for the conversion of calcium sulfide |
| CN101337661A (en) * | 2007-07-04 | 2009-01-07 | 褚亚华 | Method for preparing sodium hydrosulfide |
| CN105198122A (en) * | 2015-10-26 | 2015-12-30 | 刘阳生 | Resource utilization method of waste hydrochloric acid containing heavy metal lead and iron |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110559828A (en) * | 2019-09-06 | 2019-12-13 | 天津大学 | Small tail gas absorption and deodorization device for sludge composting tail gas treatment |
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Application publication date: 20160817 |