CN109621643A - The removing method of peculiar smell in Mizolastine production process - Google Patents
The removing method of peculiar smell in Mizolastine production process Download PDFInfo
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- CN109621643A CN109621643A CN201811531246.6A CN201811531246A CN109621643A CN 109621643 A CN109621643 A CN 109621643A CN 201811531246 A CN201811531246 A CN 201811531246A CN 109621643 A CN109621643 A CN 109621643A
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- methyl mercaptan
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- 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
- B01D53/14—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 by absorption
- B01D53/18—Absorbing units; Liquid distributors therefor
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- 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
- B01D53/14—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 by absorption
- B01D53/1487—Removing organic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/30—Sulfur compounds
- B01D2257/306—Organic sulfur compounds, e.g. mercaptans
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- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
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- Disinfection, Sterilisation Or Deodorisation Of Air (AREA)
Abstract
The present invention relates to a kind of removing methods of peculiar smell in Mizolastine production process, the method includes methyl mercaptan gas is passed through surge tank and sealing exhaust passage, introduce the gas washing pond for filling used ZA200/100 medicament, methyl mercaptan gas generates sulfate by gas washing pond and stays in gas washing pond, to remove methyl mercaptan gas.
Description
Technical field:
The present invention relates to field of medicinal chemistry, in particular to the removing method of peculiar smell in a kind of chemicals synthesis process.
Background technique:
Mizolastine, structural formula are as follows
Chemical name: 2- [[[1- [(4- fluorophenyl) methyl] -1 hydrogen-benzimidazolyl-2 radicals-yl] -4- piperidyl] methyl-ammonia
Base] -4 (3 hydrogen)-pyrimidones
Mizolastine is the periphery histamine H 1 receptor antagonist of a species specificity, selectivity, has antihistamine and resistance state
Reactivity.For seasonal and perennial allergic rhiocnesmus, allergic conjunctivitis, nettle rash and other symptoms of allergic.
The synthetic method of Mizolastine is more, such as the synthetic method in following documents:
Method 1 (quoted from: Chinese drug magazine, 2006,16 (4)；244-245)
Method 2 (quoted from: patent of invention, CN 102140076A)
Two above synthetic route, starting material are different, and synthetic route is variant, but final step be piperidinamine and
Methylthiopyrimidine reactive ketone generates Mizolastine.Exactly this step generates stench, causes production difficult, this step reaction equation is as follows:
It generates Mizolastine and necessarily generates equimolar methyl mercaptan simultaneously.Methyl mercaptan, also known as sulphur hydrogen methane.It is a kind of organic
Compound, chemical formula: CH4S.It is colourless inflammable gas under room temperature, is colourless liquid under low temperature, has beastly smelly
Taste.Country clearly advises the odorant pollutants such as methyl mercaptan in " emission standard for odor pollutants " (GB14554-93)
It is fixed, and stringent limiting emission amount.
Methyl mercaptan, -17.8 DEG C of flash-point, upper explosion limit 21.8, lower explosion limit 3.9, production environment concentration is higher, have it is on fire,
The risk of explosion.The problem of methyl mercaptan is not only elimination peculiar smell is removed, and eliminates the necessary of production safety hidden danger and adjusts.
Stench refers to stimulation human body olfactory organ, causes unhappy and damage living environment gaseous matter.Methyl mercaptan
It can cause headache, nausea and different degrees of anesthetic effect after sucking；High concentration sucking can cause respiratory paralysis and dead, even if
It is the methyl mercaptan of very low concentrations, also has apparent stench taste to will result in if worked in such a case at workers with long time
Work efficiency drop, operation energy are not concentrated, and are reluctant to enter operating area, the negative emotions such as bored to work, normal to enterprise
Production is unfavorable.
No matter from safety in production angle；From meeting national requirements for environmental protection angle；From worker's person health care angle；An urgent demand
Make the effective ways for eliminating production peculiar smell.
The method that the prior art eliminates foul gas has: sodium hydroxide solution absorption process, liquor potassic permanganate absorption process are secondary
Solution chlorate's solution absorption method, hydrogen peroxide solution absorption process, persulfate solution method, methyl mercaptan gas burning null method.
1, sodium hydroxide absorption process: hydrogen-oxygen can be used as acid foul gas and a kind of sour gas in methyl mercaptan
Change sodium to absorb.The advantages of this method is: raw material is easy to get, at low cost；The disadvantage is that: reaction it is reversible, if absorbing liquid is from highly basic
Property changes to neutrality, and methyl mercaptan can release again.The production waste liquid of medicine enterprise forbids strong basicity to discharge, therefore this method
Be not suitable for the use of this enterprise.
2, the exhaust gas such as exhaust gas methyl mercaptan, hydrogen sulfide, sulfur monoxide will methyl mercaptan gas burning null method: be produced in combustion chamber
Burning, is converted to sulfur trioxide, ultimately generates valuable by-product sulfuric acid, can obtain economic effect to sell after centralized collection
Benefit.Although this method exhaust gas is utilized completely, it is invested greatly, and the device is complicated, needs to establish tens people thus even
The production line of up to a hundred people can only be suitble to the large-scale smelting enterprise such as smelting iron and steel enterprise, coking of coal factory of high sulphur content ore.This enterprise
This scale is not reached, it is not necessary that put into a large amount of manpower and material resources for methyl mercaptan and become sulfuric acid sale, therefore this method is not
It is suitble to this enterprise to use.
3, dioxygen water absorption method: methyl mercaptan is absorbed and aoxidizes to form sulfuric acid by hydrogen peroxide, therefore reacting liquid acidity can be more next
It is higher.Acidity increases, and methyl mercaptan absorption becomes difficult, therefore assimilation effect declines rapidly.Since Mizolastine production is a hold
Continuous process, hydrogen peroxide cannot be guaranteed long period efficient absorption methyl mercaptan, therefore be not suitable for the use of this enterprise.
4, hypochlorite solution's solution absorption method: although this removing method is effective to elimination methyl mercaptan, hypochlorous acid sheet
Body has taste, abnormal pungent, therefore is not suitable for the use of this enterprise.
5, potassium permanganate absorption process: it is very suitable to the methyl mercaptan that miniaturization laboratory absorbing reaction generates, advantage is: can be with
It is directly observed by vision, the liquor potassic permanganate color to aubergine is decorporated, and illustrates that potassium permanganate is no longer valid.Laboratory is more
For glass equipment, it is very convenient to observe absorbing liquid color change.But found when industrialized production, potassium permanganate reduzate is
Manganese dioxide is very easy to form hard attachment in equipment inner wall, and cleaning is difficult, and hard manganese dioxide particle even damages
Bad pipeline pump, therefore be not suitable for the use of this enterprise.
6, persulfate method: have the characteristics that reaction speed is fast, product basically odorless, compared to other methods investments
It is small, effect is good, the disadvantage is that needing to spend to buy persulfate to use as raw material.
Summary of the invention:
The present invention provides a kind of method that the methyl mercaptan gas that Mizolastine production process generates is removed by mode of oxidizing,
The method includes by methyl mercaptan gas by surge tank and sealing exhaust passage, used ZA200/ is filled in introducing to we
The gas washing pond of 100 medicaments, methyl mercaptan gas generates sulfate by gas washing pond and stays in gas washing pond, to remove methyl mercaptan gas
Body.
Used ZA200/100 medicament of the present invention comes from following production process:
Enterprise's cooling water needs to be recycled, and cooling water temperature is generally between 20-50 DEG C, this temperature is very suitable to micro-
Biology, moss, hydrobiontic alga growth.Growth position is usually pipeline pipe valve tie point, condenser heat exchange point, if obtained for a long time
Less than killing and clearing up, it is easy to grow green villiform object on condenser, influences heat exchanger and normally exchange heat, it is therefore desirable to periodically make
It is scrubbed and is sterilized with ZA200/100 medicament.
Wherein the ZA200/100 main component is: potassium hydrogen persulfate KHSO5, potassium acid sulfate KHSO4And potassium sulfate
K2SO4 is commonly called as: potassium hydrogen persulfate compound, be common function chemicals Oxone, Caroat, ZA200/100,
The basic active principle of Basolan2448.
Used ZA200/100 medicament is often discarded, and environmental protection is influenced.
It is a discovery of the invention that used ZA200/100 medicament still has strong oxidisability, can by a kind of device,
The methyl mercaptan gas that Mizolastine production process generates is introduced into the gas washing pond containing used ZA200/100 medicament, is produced
Raw redox reaction, to eliminate methyl mercaptan gas in gas washing pond.
The inventors discovered that the foul smell that Mizolastine production process generates is methyl mercaptan gas, this gas has just
Reproducibility.If can react with discarded thimerosal above-mentioned, the harmless treatment of two kinds of industrial wastes can be achieved with.
The present invention solves following problems by experiment.First: being washed foul smell (methyl mercaptan) introducing using suitable mode
Gas pond.Second: the used ZA200/100 medicament in replacement gas washing pond, while the normal production of Mizolastine is not influenced.
Third: being capable of the simple and quick ingredient detected in gas washing pond.
The present inventor provides a kind of method thus, and steps are as follows for the method
The methyl mercaptan gas that Mizolastine production process generates draws by surge tank and sealing exhaust passage on reaction kettle
Enter the first gas washing pond, constantly monitor the content of methyl mercaptan gas in the first gas washing pond, after content reaches saturation, by exhaust passage
The second gas washing pond is accessed, at this time discards the medical fluid of the end of reaction in the first gas washing pond, new used ZA200/ is added
100 medicaments reach saturation to methyl mercaptan gas content in the second gas washing pond, and the first gas washing pond is accessed in transform exhaust channel again,
It loops back and forth like this, the methyl mercaptan gas during total overall reaction can be removed.The present invention can be using operation side in detail below
Method:
Hydrocarbonylation kettle is added in piperidinamine and methylthiopyrimidine ketone, Mizolastine and methyl mercaptan are generated after reaction；Methyl mercaptan gas
Body enters gas washing pond under the guidance of vacuum pump negative pressure, through surge tank and sealing exhaust passage, and is absorbed by medical fluid therein,
Methyl mercaptan generates sulfate and stays in gas washing pond.Using absorbing liquid situation of change in starch potassium iodide paper monitoring gas washing pond, such as
Fruit discovery absorbing liquid can not reabsorb methyl mercaptan gas, reach saturation failure, the exhaust passage pipe valve of switching sealing immediately, by second
Gas washing pond is discharged into sewage disposal system as work gas washing pond, by the waste liquid for having eliminated oxidisability in the first gas washing pond；It repeats
The above operation, until production terminates.
Scheme has the advantage that the present invention above relatively
1, good absorption effect is able to achieve perfect absorption in Mizolastine production overall process.
2, it is at low cost to eliminate peculiar smell, use the discarded production waste liquid of enterprise as absorbent be almost zero cost.
3, useless to abrogate, two kinds of pollutants administer double gain simultaneously.
4, replacement absorbent does not need to stop this normal production of imidazoles.
Specific embodiment:
The present invention is further illustrated by the following examples, but not as limitation of the present invention.
Embodiment 1
1,10 kilograms of this enterprise thimerosal waste liquids are added in gas washing pond, are used as absorbent.
2, connecting pipeline, and start vacuum pump.
3,6.0 kilograms of piperidinamine (17.8 molal quantity) and 2.8 kilograms of methylthiopyrimidine ketone are added in reaction kettle, are started
Stirring and heating.Reach reaction temperature, start to generate product while discharging about 17.8 molal quantity of methyl mercaptan gas.
4, the methyl mercaptan with reproducibility, which is constantly oxidized, becomes sulfate.Constantly from gas washing pond, sample point obtains water sample,
Oxidability is detected with starch potassium iodide paper.If it find that water sample cannot make starch potassium iodide paper become blue, illustrate to need more
Change absorbing liquid.
5, pipeline is switched to spare gas washing pond, continues to absorb.
6, it and so on operates until reaction terminates, kettle heater is reacted in closing.
7, it keeps vacuum pump to start, equipment normal operating condition, the remaining methyl mercaptan of pipeline is purged using nitrogen,
Completely into gas washing pond, the full conversion of methyl mercaptan is completed.
8, absorbing terminates, and suitable hypo solution is added into gas washing pond, completely eliminates thimerosal activity.
9, using methyl mercaptan gas detector, auxiliary monitors the methyl mercaptan in exhaust emissions, calculates methyl mercaptan elimination factor.Even
Allow to take away methyl mercaptan gas detector after continuous production, a methyl mercaptan gas alarm is only installed.
10, Mizolastine fully reacting in about 3.5 hours stops release methyl mercaptan, it is contemplated that blow line residual, methyl mercaptan
Detector detection time is 4 hours tentative.
| Soak time | Methyl mercaptan removal rate (%) | Soak time | Methyl mercaptan removal rate (%) |
| 10 minutes | 100% | 130 minutes | 100% |
| 20 minutes | 100% | 140 minutes | 100% |
| 30 minutes | 100% | 150 minutes | 100% |
| 40 minutes | 100% | 160 minutes | 100% |
| 50 minutes | 100% | 170 minutes | 100% |
| 60 minutes | 100% | 180 minutes | 100% |
| 70 minutes | 100% | 190 minutes | 100% |
| 80 minutes | 100% | 200 minutes | 100% |
| 90 minutes | 100% | 210 minutes | 100% |
| 100 minutes | 100% | 220 minutes | 100% |
| 110 minutes | 100% | 230 minutes | 100% |
| 120 minutes | 100% | 240 minutes | 100% |
The result shows that methyl mercaptan concentration removal rate reaches 100% in solution, detection when there is persulfate in the solution
Device detects numerical stability, workshop free from extraneous odour.
Claims (7)
1. the removing method of peculiar smell in Mizolastine production process, which is characterized in that the method includes leading to methyl mercaptan gas
Surge tank and sealing exhaust passage are crossed, introduces the gas washing pond for filling used ZA200/100 medicament, methyl mercaptan gas is by washing
Gas pond generates sulfate and stays in gas washing pond, to remove methyl mercaptan gas.
2. the method according to claim 1, wherein the used ZA200/100 medicament described in wherein, comes from
Following production process:
Enterprise's cooling water needs to be recycled, and cooling water temperature is generally between 20-50 DEG C, this temperature is very suitable to micro- life
Object, moss, hydrobiontic alga growth.Growth position is usually pipeline pipe valve tie point, condenser heat exchange point, if obtained for a long time not
To killing and clearing up, it is easy to grow green villiform object on condenser, influences heat exchanger and normally exchange heat, it is therefore desirable to periodically use
Medicament is scrubbed and is sterilized.The medicament product name are as follows: ZA200/100 main component is: potassium hydrogen persulfate KHSO5, sulphur
Potassium hydrogen phthalate KHSO4With potassium sulfate K2SO4, used ZA200/100 medicament often discarded, and environmental protection is influenced.
3. the method according to claim 1, wherein wherein, used ZA200/100 medicament still has by force
Oxidisability, can be by a kind of device, the methyl mercaptan gas that Mizolastine production process is generated is introduced containing used
In the gas washing pond of ZA200/100 medicament, redox reaction is generated, to eliminate methyl mercaptan gas in gas washing pond.
4. the method according to claim 1, wherein the method comprises the following steps: Mizolastine production process produces
Raw methyl mercaptan gas introduces the first gas washing pond, constantly monitors first by surge tank and sealing exhaust passage on reaction kettle
Exhaust passage is accessed the second gas washing pond, at this time by first after content reaches saturation by the content of methyl mercaptan gas in gas washing pond
The medical fluid of end of reaction in gas washing pond discards, and new used ZA200/100 medicament is added, to the second gas washing Chi Zhongjia sulphur
Alcohol gas content reaches saturation, and the first gas washing pond is accessed in transform exhaust channel again, is looped back and forth like this, and can remove all anti-
Methyl mercaptan gas during answering.
5. the method according to claim 1, wherein the method comprises the following steps: piperidinamine and methyl mercapto is phonetic
Hydrocarbonylation kettle is added in pyridine ketone, and Mizolastine and methyl mercaptan are generated after reaction；Methyl mercaptan gas passes through under the guidance of vacuum pump negative pressure
Surge tank and sealing exhaust passage enter gas washing pond, and are absorbed by medical fluid therein, and methyl mercaptan generates sulfate and stays in gas washing pond
In.
6. the method according to claim 1, wherein using absorbing liquid in starch potassium iodide paper monitoring gas washing pond
Situation of change reaches saturation failure if it find that absorbing liquid can not reabsorb methyl mercaptan gas, the exhaust passage of switching sealing immediately
The waste liquid that oxidisability has been eliminated in first gas washing pond is discharged at sewage by pipe valve using the second gas washing pond as work gas washing pond
Reason system；It repeats above operation, until production terminates.
7. steps are as follows the method according to claim 1, wherein the method: 10 kilograms of this enterprises are sterilized
Liquid waste liquid is added in gas washing pond, is used as absorbent, connecting pipeline, and starts vacuum pump, by 6.0 kilograms of piperidinamine
(17.8 molal quantity) and 2.8 kilograms of methylthiopyrimidine ketone are added in reaction kettle, starting stirring and heating.Reach reaction temperature,
Start to generate product while discharging about 17.8 molal quantity of methyl mercaptan gas, the methyl mercaptan with reproducibility, which is constantly oxidized, becomes sulphur
Hydrochlorate.Constantly from gas washing pond, sample point obtains water sample, detects oxidability with starch potassium iodide paper.If it find that water sample cannot
So that starch potassium iodide paper is become blue, illustrate to need replacing absorbing liquid, pipeline is switched to spare gas washing pond, continues to absorb, so past
Multiple operation terminates until reaction, closes reaction kettle heater, keeps vacuum pump to start, equipment normal operating condition, uses nitrogen
The remaining methyl mercaptan of pipeline is purged, completely into gas washing pond, completes the full conversion of methyl mercaptan, absorption terminates, to gas washing
Suitable hypo solution is added in pond, completely eliminates thimerosal activity, uses methyl mercaptan gas detector, auxiliary monitoring
Methyl mercaptan in exhaust emissions calculates methyl mercaptan elimination factor.Allow to take methyl mercaptan gas detector, Jin Jinan away after continuous production
A methyl mercaptan gas alarm is filled, Mizolastine fully reacting in about 3.5 hours stops release methyl mercaptan, it is contemplated that blow
Sweeping residual, methyl mercaptan gas detector detection time are 4 hours tentative.
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| CN201811531246.6A CN109621643A (en) | 2018-12-14 | 2018-12-14 | The removing method of peculiar smell in Mizolastine production process |
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