CN108658818A - A kind of preparation method of Mercaptamine - Google Patents
A kind of preparation method of Mercaptamine Download PDFInfo
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- CN108658818A CN108658818A CN201810407396.XA CN201810407396A CN108658818A CN 108658818 A CN108658818 A CN 108658818A CN 201810407396 A CN201810407396 A CN 201810407396A CN 108658818 A CN108658818 A CN 108658818A
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- concentrated sulfuric
- mercaptamine
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/24—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of esters of sulfuric acids
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/16—Purification
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- 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
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D277/00—Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings
- C07D277/02—Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings not condensed with other rings
- C07D277/08—Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member
- C07D277/12—Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D277/16—Sulfur atoms
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Abstract
The present invention relates to a kind of preparation methods of Mercaptamine, and with monoethanolamine, carbon disulfide is primary raw material, can react generation through esterification, cyclization, hydrolysis etc..The second reaction unit that wherein preparation method of Mercaptamine uses, including hydrochloric acid generation tank, first concentrated sulfuric acid tank, second concentrated sulfuric acid tank, reaction kettle and pipeline, by not stopping that the sufficient concentrations of hydrochloric acid of dilute sulfuric acid generation is added dropwise in the hydrochloric acid generation tank equipped with sodium chloride crystal, concentrated hydrochloric acid volatilizees to form wet HCL gases, dry HCL gases are formed after the concentrated sulfuric acid is dried to put into reaction kettle again, to which the hydrochloric acid ensured in reaction kettle is maintained under the conditions of higher concentration, improve reaction speed, reduce production cost, reduce the discharge of waste gas and wastes, energy conservation and environmental protection.
Description
Technical field
The present invention is a kind of preparation method of Mercaptamine, belongs to field of fine chemical, specially a kind of cysteamine
The preparation method of hydrochloride.
Background technology
Mercaptamine is given birth to through reactions such as esterification, cyclization, hydrolysis using monoethanolamine, carbon disulfide as primary raw material
At.Mercaptamine (C2H8CLNS) it is a kind of important industrial chemicals and medicine intermediate, it is raised in cosmetics, animal
Feed additives, medicine and other fields have a wide range of applications.
In hydrolysis process, with hydrochloric acid hydrolysis occurs for 2- thyroidans, generates Mercaptamine crude product.It is hydrolyzing
In technique, sufficient concentrations of hydrochloric acid is the key that ensure that reaction generates Mercaptamine.And the hydrochloric acid consumed in reaction process
And the effusion of concentrated hydrochloric acid acid mist can reduce the concentration of hydrochloric acid in reaction solution, in common process, usually start in hydrolysis
When be passed through 35% concentrated hydrochloric acid of part, reaction is passed through 35% concentrated hydrochloric acid of part again after 5 days, is passed through again after the reaction was continued 5-7 days finally
35% concentrated hydrochloric acid of part, then react 4-5 days.Total reaction time was at 15-17 days or so.In reaction process, because of the consumption meeting of hydrochloric acid
The HCL gases for reducing reaction rate, the reaction time being caused to lengthen, and concentration about 12% is not parked generate and can not utilize to become has
Evil gas.
In conclusion the production technology of prior art Mercaptamine is longer there is the reaction time, production cost is high,
The discharge for having waste gas and wastes in production process simultaneously, not only pollutes air, and cause the waste of resource.Accordingly, it is desirable to provide one
The preparation method of kind Mercaptamine solves the defect of the prior art.
Invention content
To overcome the deficiencies of existing technologies, the present invention provides it is a kind of it is effective accelerate Mercaptamine reaction speed,
Shorten the production time, reduce energy consumption Mercaptamine preparation method and its reaction unit.
A kind of preparation method of Mercaptamine, includes the following steps：
(1) monoethanolamine and the concentrated sulfuric acid are placed in the first reaction unit, and are sufficiently mixed；Monoethanolamine and concentrated sulfuric acid hair
Raw esterification, generates ethylaminoethanol sulfuric ester；
(2) 30% sodium hydroxide solution and carbon disulfide, ethylaminoethanol sulfuric ester and two are added in the first reaction unit
Ring-closure reaction occurs for nitric sulfid, generates 2- thyroidans and metabisulfite solution；
(3) 2- thyroidans obtained in the step (2) are detached by centrifugal separation, it is raw in ring-closure reaction
At metabisulfite solution pass through three-effect evaporation and condensation crystallization generate solid sodium sulfate；
(4) 35% hydrochloric acid is placed in the second reaction unit, 2- thyroidans occur hydrolysis with hydrochloric acid and generate half Guang
Mercaptamine crude product is made in amine hydrochlorate, condensing reflux；
(5) ethanol solution is added in third reaction unit so that Mercaptamine is dissolved completely in ethanol solution；
By the temperature cooling in reaction kettle so that Mercaptamine solubility declines crystal and is precipitated；It is separated by filtration and obtains cysteamine salt
Hydrochlorate and alcohol crystal body obtain finished product Mercaptamine crystal after heating distills out ethyl alcohol.
Preferably, monoethanolamine and the molar ratio of the concentrated sulfuric acid are 1.2: 1 in the step (1), and the temperature of esterification is
110℃。
Preferably, the temperature of ring-closure reaction is 80-90 DEG C in the step (2).
Preferably, the molar ratio of hydrochloric acid and 2- thyroidans is 5: 1 in the step (4), and the temperature of hydrolysis is
105-110℃。
Preferably, the second reaction unit includes hydrochloric acid generation tank, the first concentrated sulfuric acid tank, the second dense sulphur in the step (4)
Sour tank, reaction kettle and pipeline, which is characterized in that the hydrochloric acid generation tank is equipped with first row gas port, the first inlet and first
Discharge port, first discharge port are equipped with the first outlet valve；First concentrated sulfuric acid tank is arranged in the top of hydrochloric acid generation tank, institute
It states the first concentrated sulfuric acid tank and mouth, second exhaust port and the first air inlet is added dropwise equipped with first, described first, which is added dropwise mouth, is equipped with first
Valve is added dropwise, first row air valve is equipped at the second exhaust port, the first intake valve is equipped at first air inlet；Described second
Concentrated sulfuric acid tank is arranged in the top of hydrochloric acid generation tank, second concentrated sulfuric acid tank be equipped with second be added dropwise mouth, third exhaust outlet and
Second air inlet, described second is added dropwise at mouth equipped with the second dropwise addition valve, and the third exhaust ports are equipped with second row air valve, described
The second intake valve is equipped at second air inlet；The reaction kettle is arranged in the side of hydrochloric acid generation tank, and the reaction kettle is equipped with
Second discharge port, the 4th exhaust outlet and third air inlet, second discharge outlet are equipped with the second outlet valve, the 4th exhaust
It is equipped with the 4th air bleeding valve at mouthful, third intake valve is equipped at the third air inlet, the top of the reaction kettle is equipped with condenser pipe；
Mouth is added dropwise in the first of first concentrated sulfuric acid tank and the second dropwise addition mouth of the second concentrated sulfuric acid tank passes through pipeline and hydrochloric acid generation tank
First inlet is connected；Second air inlet of the first air inlet of first concentrated sulfuric acid tank and the second concentrated sulfuric acid tank passes through pipe
Road is connected with the first row gas port of hydrochloric acid generation tank；The second exhaust port of first concentrated sulfuric acid tank and the second concentrated sulfuric acid tank
Third exhaust outlet is connected by pipeline with the third air inlet of reaction kettle.
Preferably, second reaction unit further includes gas buffer tank, and the gas buffer tank setting is in connection second
On the pipeline of the third exhaust outlet of concentrated sulfuric acid tank and the third air inlet of reaction kettle.
Preferably, second reaction unit further includes falling-film absorber, and the falling-film absorber is arranged in reaction kettle
Above condenser pipe, the falling-film absorber is connected by pipeline with reaction kettle.
Preferably, the gas outlet of the gas buffer tank is equipped with third air bleeding valve.
Preferably, the gas outlet of the gas buffer tank is equipped with flowmeter, the flow for controlling HCL gases.
Preferably, the gas buffer tank is equipped with pressure gauge, for monitoring gas buffer pressure inside the tank, prevents tank body broken
Damage, leakage.
Beneficial effects of the present invention：
(1) preparation method of Mercaptamine of the invention can effectively improve reaction relative to traditional preparation method
Speed simplifies process, production efficiency can be improved.In the hydrolysis link of the present invention, the second reaction unit of use includes salt
Sour generation tank, the first concentrated sulfuric acid tank, the second concentrated sulfuric acid tank, reaction kettle and pipeline；Design two concentrated sulfuric acid tanks, one of them dense sulphur
Sour tank is for being added dropwise sulfuric acid, another concentrated sulfuric acid tank moves in circles for the dry HCL gases generated, effectively supplemented with hydrolysis
It is anti-to reduce hydrolysis to which the HCL that ensure that in reaction solution is always held at higher concentration for the HCL gases consumed in reaction
The number that concentrated hydrochloric acid should be added in the process, simplifies production stage, recycles HCL gases, energy conservation and environmental protection.
(2) preparation method of Mercaptamine of the invention, by the improvement for hydrolyzing link make the reaction time from
15-20 days originally shorten to 8-10 days, and the reaction time greatly shortened improves production efficiency, meanwhile, Mercaptamine
Steam consumption in whole reaction process is substantially reduced, and the energy consumption of specific yield is reduced to from original 3300 yuan/ton
2000 yuan/ton.It should be evident that shortening between when reacted, then the Mercaptamine yield in the unit interval is correspondingly improved.
(3) preparation method of Mercaptamine of the invention, the exhaust gas finally generated in reaction kettle is HCL acid mists, H2S
And CO2Mixed gas, used falling-film absorber absorb HCL acid mists, then H2S and CO2Mixed gas burning generates SO2And CO2,
SO2Sodium sulfite solution is generated by absorbing by liquid caustic soda, carbon dioxide is discharged in air, avoids exhaust gas effusion and causes dirt to air
Dye, recycles HCL gases, energy conservation and environmental protection.Meanwhile the metabisulfite solution generated in ring-closure reaction passes through three-effect evaporation and condensation knot
Crystalline substance generates solid sodium sulfate and effectively prevents the wasting of resources as byproduct, reduces the cost of Business survival.
(4) preparation method of Mercaptamine of the invention, concentrated hydrochloric acid generates in hydrochloric acid generation tank, and passes through pipeline
It is delivered in reaction kettle, avoids the effusion of HCL gases, air is polluted, the corrosion to equipment.Greatly reduce corrosion
Property liquid is to the hurtful danger of human body.Meanwhile the mode of traditional artificial multiple addition concentrated hydrochloric acid is changed, it is time saving and energy saving,
Charging efficiency is improved, manually-operated intensity is reduced, greatly reduces corrosive liquids to the hurtful danger of human body.
Description of the drawings
Fig. 1 is the structural schematic diagram of reaction unit used by the preparation method of the Mercaptamine of the present invention.
Specific implementation mode
Technical scheme of the present invention is illustrated below in conjunction with the accompanying drawings, implementing direction of the invention is with the direction of Fig. 1
Standard.
A kind of preparation method of Mercaptamine, includes the following steps：
(1) monoethanolamine and the concentrated sulfuric acid are placed in the first reaction unit, and are sufficiently mixed；Monoethanolamine and concentrated sulfuric acid hair
Raw esterification, generates ethylaminoethanol sulfuric ester；Wherein, monoethanolamine and the molar ratio of the concentrated sulfuric acid are 1.2: 1, esterification
Temperature is 110 DEG C；
(2) 30% sodium hydroxide solution and carbon disulfide are added in the first reaction unit, controls the temperature in reaction kettle
It it is 80-90 DEG C, with carbon disulfide ring-closure reaction occurs for ethylaminoethanol sulfuric ester, generates 2- thyroidans and metabisulfite solution；
(3) 2- thyroidans obtained in step (2) are detached by centrifugal separation, is generated in ring-closure reaction
Metabisulfite solution is crystallized by three-effect evaporation and condensation and generates solid sodium sulfate, as byproduct；
(4) 35% hydrochloric acid is placed in the second reaction unit, it is 105-110 DEG C to control the temperature in the second reaction unit,
2- thyroidans occur hydrolysis with hydrochloric acid and generate Mercaptamine, and Mercaptamine crude product is made in condensing reflux；Its
In, the molar ratio of hydrochloric acid and 2- thyroidans is 5: 1；
(5) ethanol solution is added in third reaction unit, controls the temperature in third reaction kettle and controls at 70-80 DEG C,
So that Mercaptamine is dissolved completely in ethanol solution；Temperature in third reaction unit is cooled to 30 DEG C hereinafter, making
It obtains Mercaptamine solubility and declines crystal precipitation；It is separated by filtration and obtains Mercaptamine and alcohol crystal body, heating is steamed
After distillating ethyl alcohol, finished product Mercaptamine crystal is obtained, wherein the recyclable recycling of ethyl alcohol.
As shown in Figure 1, the second reaction unit used in the preparation method step (4) of the Mercaptamine of the present invention,
It is slow including hydrochloric acid generation tank 1, the first concentrated sulfuric acid tank 2, the second concentrated sulfuric acid tank 3, reaction kettle 4, falling-film absorber 5, pipeline 6 and gas
Tank 7 is rushed, wherein：
Hydrochloric acid generation tank 1 provides reaction compartment, hydrochloric acid generation tank 1 for containing sodium chloride crystal for HCL gases
Upper end be equipped with first row gas port 11 and the first inlet 12, the lower end of hydrochloric acid generation tank 1 is equipped with the first discharge port 13；Wherein,
First discharge port 13 is equipped with the first outlet valve 110.
First concentrated sulfuric acid tank 2 for containing concentrated sulfuric acid liquid, be added dropwise into hydrochloric acid generation tank 1 sulfuric acid or to HCL gases into
Row drying；First concentrated sulfuric acid tank 2 is arranged in the top of hydrochloric acid generation tank 1.The lower end of first concentrated sulfuric acid tank 2 is equipped with first and mouth is added dropwise
21, the upper end of the first concentrated sulfuric acid tank 2 is equipped with second exhaust port 22, and the side wall of the first concentrated sulfuric acid tank 2 is equipped with the first air inlet 23；
Wherein, the first dropwise addition mouth 21 is equipped with first and valve 210 is added dropwise, and first row air valve 220, the first air inlet are equipped at second exhaust port 22
The first intake valve 230 is equipped at 23.
Second concentrated sulfuric acid tank 3 is dried HCL gases or is dripped into hydrochloric acid generation tank 1 for containing concentrated sulfuric acid liquid
Add sulfuric acid；Second concentrated sulfuric acid tank 3 is arranged in the top of hydrochloric acid generation tank 1, and the second concentrated sulfuric acid tank 3 and 2, the first concentrated sulfuric acid tank
In in same level.The lower end of second concentrated sulfuric acid tank 3 is equipped with second and mouth 31, the upper end third row of the second concentrated sulfuric acid tank 3 is added dropwise
Gas port 32, the second air inlet 33 on the side wall of the second concentrated sulfuric acid tank 3；Wherein, it second is added dropwise at mouth 31 equipped with the second dropwise addition valve
310, it is equipped with second row air valve 320 at third exhaust outlet 32, the second intake valve 330 is equipped at the second air inlet 33.
Reaction kettle 4 occurs hydrolysis for 2- thyroidans and hydrochloric acid and provides generation space for containing reaction solution,
Reaction kettle 4 is arranged in the side of hydrochloric acid generation tank 1.The lower end of reaction kettle 4 is equipped with the second discharge port 41, and the upper end of reaction kettle 4 is set
There are the 4th exhaust outlet 42, the side wall of reaction kettle 4 to be equipped with third air inlet 43；Wherein, go out equipped with second at the second discharge port 41
Expect valve 410, the 4th air bleeding valve 420 is equipped at the 4th exhaust outlet 42, third intake valve 430 is equipped at third air inlet 43.Reaction
The top of kettle 4 is equipped with condenser pipe 44, for the gas generated in reaction kettle in reaction process 4 to liquefy afterwards to the cold.
Falling-film absorber 5 is arranged above the condenser pipe 44 of reaction kettle 4, is connected with reaction kettle 4 by pipeline 6；Falling liquid film
Extra HCL acid mist of the absorber 5 for being generated during absorbing reaction.
Wherein, the second dropwise addition mouth 31 of the first dropwise addition mouth 21 of the first concentrated sulfuric acid tank 2 and the second concentrated sulfuric acid tank 3 passes through pipeline
6 are connected with the first inlet 12 of hydrochloric acid generation tank 1；The first air inlet 23 and the second concentrated sulfuric acid tank 3 of first concentrated sulfuric acid tank 2
The second air inlet 33 be connected with the first row gas port 11 of hydrochloric acid generation tank 1 by pipeline 6；The second of first concentrated sulfuric acid tank 2
Exhaust outlet 22 is connected by pipeline 6 with the third air inlet 43 of reaction kettle 4 with the third exhaust outlet 32 of the second concentrated sulfuric acid tank 3.
Gas buffer tank 7 is used to stablize the pressure in pipeline 6 and reaction kettle 4, and redrying will enter in reaction kettle 4
HCL gases.The third in the third exhaust outlet 32 and reaction kettle 4 for connecting 3 upper end of the second concentrated sulfuric acid tank is arranged in gas buffer tank 7
On the pipeline 6 of air inlet 43, the gas outlet of gas buffer tank 7 is equipped with third air bleeding valve 710.Further, gas buffer tank 7
Gas outlet is equipped with flowmeter, the flow for controlling HCL gases according to practical condition；Further, gas buffer tank 7
It is equipped with pressure gauge, for monitoring gas buffer pressure inside the tank, prevents in tank body pressure is excessive to cause breakage, situations such as leakage
Occur.
Operation principle：It in hydrolysis, first opens first and valve 210 is added dropwise so that the sulfuric acid drop in the first concentrated sulfuric acid tank 2
It is added in hydrochloric acid generation tank 1, is reacted with sodium chloride and generate hydrochloric acid；The second intake valve 330 for opening the second concentrated sulfuric acid tank 3 again, makes
In hydrochloric acid generation tank concentrated hydrochloric acid volatilize the wet HCL gases to be formed, pass through pipeline from the first row gas port 11 of hydrochloric acid generation tank 1
It is dried in into the second concentrated sulfuric acid tank 3；The second row air valve 320 of the second concentrated sulfuric acid tank 3 and the third of reaction kettle 4 are opened again
Intake valve 430 so that the HCL gases after the concentrated sulfuric acid is dried enter in reaction kettle, and hydrolysis occurs with 2- thyroidans.
After the second concentrated sulfuric acid tank does not stop to absorb the moisture in HCL gases, concentration continuously decreases, and drying capacity constantly drops
Low, valve 31 is added dropwise in open the second concentrated sulfuric acid tank 3 at this time second so that the dilute sulfuric acid in the second concentrated sulfuric acid tank 3 is added dropwise in hydrochloric acid
In generation tank 1, is reacted with sodium chloride and generate hydrochloric acid；The first intake valve 230 of the first concentrated sulfuric acid tank 2 is opened again so that hydrochloric acid is sent out
Concentrated hydrochloric acid volatilizees the wet HCL gases to be formed in raw tank, enters first by pipeline from the first row gas port 11 of hydrochloric acid generation tank 1
It is dried in concentrated sulfuric acid tank 2；The first row air valve 220 of the first concentrated sulfuric acid tank 2 and the third intake valve of reaction kettle 4 are opened again
430 so that the HCL gases after the concentrated sulfuric acid is dried enter in reaction kettle 4, and hydrolysis occurs with 2- thyroidans；More into one
Step ground, the HCL gases after the concentrated sulfuric acid is dried pass through the redrying of gas buffer tank 7 before entering reaction kettle 4, and buffering has
Conducive to the stable gas pressure kept in pipeline 6 and reaction kettle 4, the concentration height reaction of HCL gases is more abundant.It is final in reaction kettle 4
The exhaust gas of generation is HCL acid mists, H2S and CO2Mixed gas, used falling-film absorber absorb HCL acid mists, then H2S and CO2It is mixed
It closes gas burning and generates SO2And CO2Gas, SO2Gas generates sodium sulfite solution, CO by absorbing by liquid caustic soda2Air is discharged in gas
In.The Mercaptamine produced in reaction kettle 4 is discharged by the second discharge port 41；The sodium sulphate generated in hydrochloric acid generation tank 1
Solution is discharged by the first discharge port 13, is crystallized by three-effect evaporation and condensation and is generated sodium sulfate crystal, as byproduct.
In technical scheme of the present invention, hydrochloric acid generation tank is mainly used for supplementing the consumption of hydrochloric acid in hydrolysis reaction, with
It maintains hydrochloric acid in reaction kettle to be maintained at higher concentration, ensures reaction speed.For convenience of operation, two concentrated sulfuric acid tanks are designed, when
One of concentrated sulfuric acid tank does not stop after absorbing the moisture in wet HCL gases, and concentration continuously decreases, and final drying capacity declines,
The concentrated sulfuric acid in the concentrated sulfuric acid tank has changed into dilute sulfuric acid at this time, occurs with sodium chloride crystal for being added drop-wise in hydrochloric acid generation tank
Reaction generates sufficient concentrations of hydrochloric acid, and concentrated hydrochloric acid volatilizees to form wet HCL gases, and another concentrated sulfuric acid tank is then opened as dry
Dry tank uses, and so recycles.The HCL gases of the drying formed after the concentrated sulfuric acid is dried are put into reaction kettle again, to protect
Hydrochloric acid is maintained under the conditions of higher concentration in card reaction kettle, to improve the speed of hydrolysis, by the original reaction time from 15-
It shortens to 8-10 days within 17 days, effectively reduces energy consumption.Meanwhile needing repeatedly to add concentrated hydrochloric acid in traditional handicraft to maintain reaction kettle
The concentration of interior hydrochloric acid, repeatedly charging is so that technique labor intensity is high, and concentrated hydrochloric acid has volatility, corrosivity, not only to workshop
Interior air pollutes, and concentrated hydrochloric acid splashing is damaged to health and equipment corrosion.Technical scheme of the present invention without
It needs repeatedly manually to add concentrated hydrochloric acid so that labor intensity reduces, and substantially increases safe.
The foregoing is merely the better embodiments of the present invention, and the invention is not limited in the above embodiments, are implementing
There may be the small structural modifications in part in the process, if the various changes or modifications of the present invention are not departed from the essence of the present invention
God and range, and belong within the scope of the claim and equivalent technologies of the present invention, then the present invention is also intended to comprising these changes
And modification.
Claims (10)
1. a kind of preparation method of Mercaptamine, which is characterized in that include the following steps：
(1) monoethanolamine and the concentrated sulfuric acid are placed in the first reaction unit, and are sufficiently mixed；Ester occurs for monoethanolamine and the concentrated sulfuric acid
Change reaction, generates ethylaminoethanol sulfuric ester；
(2) 30% sodium hydroxide solution and carbon disulfide, ethylaminoethanol sulfuric ester and curing are added in the first reaction unit
Ring-closure reaction occurs for carbon, generates 2- thyroidans and metabisulfite solution；
(3) 2- thyroidans obtained in the step (2) are detached by centrifugal separation, is generated in ring-closure reaction
Metabisulfite solution is crystallized by three-effect evaporation and condensation and generates solid sodium sulfate；
(4) 35% hydrochloric acid is placed in the second reaction unit, 2- thyroidans occur hydrolysis with hydrochloric acid and generate cysteamine salt
Mercaptamine crude product is made in hydrochlorate, condensing reflux；
(5) ethanol solution is added in third reaction unit so that Mercaptamine is dissolved completely in ethanol solution；It will be anti-
The temperature in kettle is answered to cool down so that Mercaptamine solubility declines crystal and is precipitated；It is separated by filtration and obtains Mercaptamine
And alcohol crystal body obtains finished product Mercaptamine crystal after heating distills out ethyl alcohol.
2. a kind of preparation method of Mercaptamine according to claim 1, which is characterized in that in the step (1)
Monoethanolamine and the molar ratio of the concentrated sulfuric acid are 1.2: 1, and the temperature of the esterification is 110 DEG C.
3. a kind of preparation method of Mercaptamine according to claim 1, which is characterized in that in the step (2)
The temperature of ring-closure reaction is 80-90 DEG C.
4. a kind of preparation method of Mercaptamine according to claim 1, which is characterized in that in the step (4)
The molar ratio of hydrochloric acid and 2- thyroidans is 5: 1, and the temperature of the hydrolysis is 105-110 DEG C.
5. the preparation method of Mercaptamine according to claim 1, the second reaction unit includes in the step (4)
Hydrochloric acid generation tank, the first concentrated sulfuric acid tank, the second concentrated sulfuric acid tank, reaction kettle and pipeline, which is characterized in that on the hydrochloric acid generation tank
Equipped with first row gas port, the first inlet and the first discharge port, first discharge port is equipped with the first outlet valve；Described first is dense
Sulphuric acid tank is arranged in the top of hydrochloric acid generation tank, and first concentrated sulfuric acid tank is equipped with first and mouth, second exhaust port and the is added dropwise
One air inlet, described first, which is added dropwise mouth, is equipped with first valve is added dropwise, and is equipped with first row air valve at the second exhaust port, and described first
The first intake valve is equipped at air inlet；Second concentrated sulfuric acid tank is arranged in the top of hydrochloric acid generation tank, second concentrated sulfuric acid
Tank is equipped with second and mouth, third exhaust outlet and the second air inlet is added dropwise, and described second is added dropwise at mouth equipped with the second dropwise addition valve, described
Third exhaust ports are equipped with second row air valve, and the second intake valve is equipped at second air inlet；The reaction kettle is arranged in salt
The side of sour generation tank, the reaction kettle are equipped with the second discharge port, the 4th exhaust outlet and third air inlet, second discharging
Mouthful place is equipped with the second outlet valve, and the 4th exhaust ports are equipped with the 4th air bleeding valve, at the third air inlet equipped with third into
The top of air valve, the reaction kettle is equipped with condenser pipe；Mouth and the second concentrated sulfuric acid tank is added dropwise in the first of first concentrated sulfuric acid tank
Second dropwise addition mouth is connected by pipeline with the first inlet of hydrochloric acid generation tank；First air inlet of first concentrated sulfuric acid tank
It is connected with the first row gas port of hydrochloric acid generation tank by pipeline with the second air inlet of the second concentrated sulfuric acid tank；The first dense sulphur
The second exhaust port of sour tank is connected by pipeline with the third air inlet of reaction kettle with the third exhaust outlet of the second concentrated sulfuric acid tank.
6. the preparation method of Mercaptamine according to claim 5, which is characterized in that second reaction unit is also
Including gas buffer tank, the third in the third exhaust outlet and reaction kettle for connecting the second concentrated sulfuric acid tank is arranged in the gas buffer tank
On the pipeline of air inlet.
7. the preparation method of Mercaptamine according to claim 5, which is characterized in that second reaction unit is also
Including falling-film absorber, the falling-film absorber is arranged above the condenser pipe of reaction kettle, and the falling-film absorber passes through pipeline
It is connected with reaction kettle.
8. the preparation method of Mercaptamine according to claim 5, which is characterized in that the gas buffer tank goes out
Gas port is equipped with third air bleeding valve.
9. the preparation method of Mercaptamine according to claim 5, which is characterized in that the gas buffer tank goes out
Gas port is equipped with flowmeter, the flow for controlling HCL gases.
10. the preparation method of Mercaptamine according to claim 5, which is characterized in that on the gas buffer tank
Equipped with pressure gauge tank body breakage, leakage are prevented for monitoring gas buffer pressure inside the tank.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110511165A (en) * | 2019-08-01 | 2019-11-29 | 苏州汉德创宏生化科技有限公司 | A kind of synthetic method of taurine precursor 2- ethylaminoethanol sulfuric ester |
| CN110813210A (en) * | 2019-11-27 | 2020-02-21 | 衡阳丰联精细化工有限公司 | Apparatus for producing of cysteamine hydrochloride |
| CN113462738A (en) * | 2021-08-24 | 2021-10-01 | 蓝科医美科学技术(吉林)有限公司 | Fermentation extraction process of ginseng extract |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57144252A (en) * | 1981-03-03 | 1982-09-06 | Mitsui Toatsu Chem Inc | Preparation of aminoalkylthiol |
| CN106431821A (en) * | 2016-08-25 | 2017-02-22 | 江西金龙化工有限公司 | Method for comprehensively utilizing dehydrated dilute sulphuric acid and byproduct sodium chloride and producing byproduct sodium hydrogen sulfate |
-
2018
- 2018-04-27 CN CN201810407396.XA patent/CN108658818B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57144252A (en) * | 1981-03-03 | 1982-09-06 | Mitsui Toatsu Chem Inc | Preparation of aminoalkylthiol |
| CN106431821A (en) * | 2016-08-25 | 2017-02-22 | 江西金龙化工有限公司 | Method for comprehensively utilizing dehydrated dilute sulphuric acid and byproduct sodium chloride and producing byproduct sodium hydrogen sulfate |
Non-Patent Citations (1)
| Title |
|---|
| WU, SHAO YONG 等: "Synthesis and insecticidal activity of oxazaphospholidines, oxathiaphospholanes", 《AGRICULTURAL AND BIOLOGICAL CHEMISTRY》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110511165A (en) * | 2019-08-01 | 2019-11-29 | 苏州汉德创宏生化科技有限公司 | A kind of synthetic method of taurine precursor 2- ethylaminoethanol sulfuric ester |
| CN110813210A (en) * | 2019-11-27 | 2020-02-21 | 衡阳丰联精细化工有限公司 | Apparatus for producing of cysteamine hydrochloride |
| CN113462738A (en) * | 2021-08-24 | 2021-10-01 | 蓝科医美科学技术(吉林)有限公司 | Fermentation extraction process of ginseng extract |
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