CN104671208B - Preparation device and technology for hydrogen chloride-methanol solution - Google Patents
Preparation device and technology for hydrogen chloride-methanol solution Download PDFInfo
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- CN104671208B CN104671208B CN201510067984.XA CN201510067984A CN104671208B CN 104671208 B CN104671208 B CN 104671208B CN 201510067984 A CN201510067984 A CN 201510067984A CN 104671208 B CN104671208 B CN 104671208B
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- distillation still
- hydrogen chloride
- solution
- methanol solution
- hydrochloric acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a preparation device and technology for hydrogen chloride-methanol solution. The preparation device comprises a distillation kettle, a cooling tower, a buffering tank, and an adsorption kettle, wherein a solution inlet and a vapor outlet are formed in the top of the distillation kettle, and a solution outlet is formed in the bottom end of the distillation kettle; the cooling tower is communicated with the distillation kettle through the vapor outlet of the distillation kettle; the buffering tank is communicated with the cooling tower; and the adsorption kettle is communicated with the buffering tank. Compared with the prior art, hydrogen chloride gas is volatilized by heating the hydrochloric acid solution, the hydrogen chloride-methanol solution is obtained by cooling and methanol absorption, and the low-concentration of hydrochloric acid is used for preparing industrial calcium chloride, thus forming circular economy. The three wastes problem of mixed acid can be can be solved, and the utilization rate of hydrochloric acid can be increased.
Description
Technical field
The present invention relates to the preparation facilities and technique of a kind of hydrogen chloride methanol solution.
Background technology
Existing methanolic hydrogen chloride is added dropwise in hydrochloric acid solution by the concentrated sulfuric acid, using self heat, steams hydrogen chloride, then through first
Alcohol absorbs, and prepares methanolic hydrogen chloride, and the method produces a large amount of nitration mixture, and serious " three wastes " problem is brought to enterprise；And hydrochloric acid solution
Utilization rate is low.
Therefore, it is necessary to further be improved prior art.
The content of the invention
It is an object of the present invention to provide a kind of preparation facilities of hydrogen chloride methanol solution, it is ensureing equipment safety
Under the premise of, gas raw material is made full use of, consumption of raw materials is reduced, improve production efficiency.
Another object of the present invention is to provide a kind of technique for preparing hydrogen chloride methanol solution, nitration mixture " three is which solved
It is useless " problem, improve hydrochloric acid solution utilization rate.
To reach object defined above, a kind of preparation facilities of hydrogen chloride methanol solution of the invention, it includes：Bottom is provided with molten
Liquid is exported；
Cooling tower, it is connected by the steam (vapor) outlet of the distillation still with the distillation still；
Surge tank, it is connected with the cooling tower；
Absorption kettle, it is connected with the surge tank.
Used as a preferred embodiment of the invention, it also includes：
Synthesis reactor, its side offers the first import and the second import, and opposite side offers first outlet,
The bottom of the distillation still is additionally provided with taphole, the synthesis reactor by the taphole of the distillation still and
First import of the synthesis reactor is connected with the distillation still.
As a preferred embodiment of the invention, circulating cooling water inlet and circulating cooling are provided with the cooling tower
Water out.
Further, a kind of technique that hydrogen chloride methanol solution is prepared using above-mentioned device of the present invention, it includes：Its
Hydrochloric acid solution is added in distillation still, the hydrochloric acid solution in the distillation still is heated so as to the hydrogen chloride gas that volatilize, the chlorine for volatilizing
Change methanol absorption of the hydrogen through cooling down in tower cooler, absorption kettle and hydrogen chloride methanol solution is obtained.
Used as a preferred embodiment of the invention, it specifically includes following steps：
(1) toward adding hydrochloric acid solution raw material in distillation still, to adding methyl alcohol in absorption kettle；
(2) thermometer on observation absorption kettle, when temperature is at 0 DEG C, the steam (vapor) outlet of crack distillation still, slow heating distillation
Kettle 1~2 hour, makes pot temperature reach 70~85 DEG C；
(3) continue to be heated to distillation still, maintenance pot temperature is 5~6 hours at 70~85 DEG C；
(4) continue to be slowly heated distillation still, and ensure that the temperature of hydrogen chloride methanol solution in absorption kettle is no more than 10 DEG C；
As a preferred embodiment of the invention, also comprise the following steps after step (4)：
When () continues to be heated to 130 DEG C to distillation still a, the steam (vapor) outlet of distillation still is closed, bottom valve is opened, by molten
Liquid outlet will obtain calcium chloride solution in low concentration of salt acid solution feeding synthesis reactor in distillation still with calcium carbonate reaction；
B the calcium chloride solution obtained in the step (a) is made calcium chloride solid by ().
Used as a preferred embodiment of the invention, the concentration of the methanolic hydrogen chloride for obtaining is more than 26%.
Used as a preferred embodiment of the invention, the concentration of the hydrochloric acid solution is more than 34%.
Used as a preferred embodiment of the invention, the concentration of the low-concentration hcl is less than 20%.
Beneficial effects of the present invention：Compared with prior art, the present invention uses heating hydrochloric acid solution so as to the hydrogen chloride that volatilizees
Gas, hydrogen chloride methanol solution is obtained through cooling, methanol absorption, and gained low-concentration hcl is used to prepare industrial calcium chloride, is formed
Recycling economy.Nitration mixture " three wastes " problem is solved, hydrochloric acid solution utilization rate is improve.
Brief description of the drawings
Technical scheme in order to illustrate more clearly the embodiments of the present invention, below will be to that will use needed for embodiment description
Accompanying drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for this
For the those of ordinary skill of field, without having to pay creative labor, other can also be obtained according to these accompanying drawings
Accompanying drawing.Wherein：
Fig. 1 is a kind of structural representation of the preparation facilities of hydrogen chloride methanol solution of the invention.
Specific embodiment
It is below in conjunction with the accompanying drawings and specific real to enable the above objects, features and advantages of the present invention more obvious understandable
The present invention is further detailed explanation to apply mode.
" one embodiment " or " embodiment " referred to herein refers in may be included at least one implementation of the invention
Special characteristic, structure or characteristic." in one embodiment " that different places occur in this manual not refers both to same
Individual embodiment, nor the single or selective embodiment mutually exclusive with other embodiment.
Fig. 1 is referred to, it is a kind of structural representation of the preparation facilities of hydrogen chloride methanol solution of the invention.
The preparation facilities of the hydrogen chloride methanol solution includes distillation still 1, cooling tower 2, surge tank 3, absorption kettle 4 and synthesis
Kettle 5.
The distillation still 1, its top is provided with solution inlet port 11 and steam (vapor) outlet 12, and its bottom is provided with taphole
13.The solution inlet port 11 is flowed into for hydrochloric acid solution, and the hydrochloric acid volatilization hydrogen chloride gas after being heated through the distillation still 1 are by steaming
Vapor outlet 12 enters the cooling tower 2, and the taphole 13 exits into synthesis reactor 5 for the hydrochloric acid of low concentration.
The cooling tower 2, it is connected by the steam (vapor) outlet 12 of the distillation still 1 with the distillation still 1.The cooling
Circulating cooling water inlet (not shown) and circulating cooling water out (not shown) are provided with tower 2.
The surge tank 3, it is connected with the cooling tower 2.Hydrogen chloride gas after being cooled down through the cooling tower 2 are through pipe
Road is flowed into the surge tank 3.
The absorption kettle 4, it is connected with the surge tank 3.Pass through pipeline through the hydrogen chloride gas after the surge tank 3
In inflow absorption kettle 4, and by the methanol absorption in the absorption kettle 4 up to absorption equilibrium, and then obtain hydrogen chloride methanol solution.
The synthesis reactor 5, its side offers the first import 51 and the second import 52, and opposite side offers first outlet
53.The low-concentration hcl flowed out from the distillation still 1 enters synthesis reactor 5 through first import 51 of synthesis reactor 5, by synthesis reactor
The second import 52 to adding hydrochloric acid and the calcium carbonate of calcium carbonate, low concentration to be carried out in the synthesis reactor 5 in the synthesis reactor 5
Reaction obtains calcium chloride solution, and the calcium chloride solution is flowed out by first outlet 53.
1 the preparation technology of hydrogen chloride methanol solution of the present invention described below in conjunction with the accompanying drawings.The present invention is in distillation still 1
Hydrochloric acid solution is added, the hydrochloric acid solution in the distillation still 1 is heated so as to the hydrogen chloride gas that volatilize, the hydrogen chloride gas for volatilizing
Cooled down through cooling tower 2, the methanol absorption in absorption kettle 4 is obtained hydrogen chloride methanol solution.Specifically include following steps：
(1) toward adding hydrochloric acid solution raw material in distillation still 1, to adding methyl alcohol in absorption kettle 4；
(2) thermometer (not shown) on observation absorption kettle 1, when temperature is at 0 DEG C, the steam valve of crack distillation still 1 delays
The slow heating time of distillation still 1 is 1~2 hour, the temperature of distillation still 1 is reached 70~85 DEG C；
(3) continue to be heated to distillation still 1, the maintenance temperature of distillation still 1 is 5~6 hours at 70~85 DEG C；
(4) continue to be slowly heated distillation still 1, and ensure that the temperature of hydrogen chloride methanol solution in absorption kettle 4 is no more than 10 DEG C.
Further, when the concentration of hydrochloric acid solution reduction in distillation still 1, the hydrochloric acid solution of low concentration can also be recycled
Calcium chloride is prepared with calcium carbonate reaction, its step is as follows：
When () continues to be heated to 130 DEG C to distillation still 1 a, the steam valve of distillation still 1 is closed, open the bottom of distillation still 1
Valve (not shown), is sent into synthesis reactor 5 and calcium carbonate reaction low concentration of salt acid solution in distillation still 1 by taphole 13
Obtain calcium chloride solution；
B the calcium chloride solution obtained in the step (a) is made calcium chloride solid by ().
Embodiment 1
Metered 600L synthetic hydrochloric acids (content is more than 35%, g/ml) in toward the distillation still 1, in the absorption kettle 4
Metered 400L methyl alcohol, opening cooling tower 2 is intake, flowing water Valve, and the chuck coolant media of absorption kettle 4 (is not schemed into and out of valve
Show), methanol temperature is maintained 0 DEG C or so, crack steam valve, temperature escapes chlorine at 79 DEG C in being to slowly warm up to distillation still 1
After changing hydrogen through cooling tower, absorption kettle 4 is entered after buffered tank 3 and is absorbed, until absorption equilibrium, closes distillation still 1 and enter steam valve, buffering
Valve on tank 3, determines methanolic hydrogen chloride concentration for 26.01% (g/ml), remaining low concentration of salt acid solution 583kg, and concentration is
20% (g/ml), export trade, for producing calcium chloride.
Embodiment 2
Metered 750L synthetic hydrochloric acids (content is more than 34.5%, g/ml) in toward distillation still 1, metering adds in absorption kettle 4
Enter 480L methyl alcohol, opening cooling tower 2 is intake, flowing water Valve, the chuck coolant media of absorption kettle 4 ties up methanol temperature into and out of valve
Hold at 0 DEG C or so, crack steam valve, in being to slowly warm up to distillation still 1 temperature at 82 DEG C, after effusion hydrogen chloride is through cooling tower 2,
Enter absorption kettle 4 after buffered tank 3 to absorb, until absorption equilibrium, closes distillation still 1 and enter valve on steam valve, surge tank 3, determine
Methanolic hydrogen chloride concentration is %26.36% (g/ml), and remaining low concentration of salt acid solution 730kg, concentration is 19.6% (g/ml), outward
Pin, for producing calcium chloride.
Embodiment 3
Metered 750L synthetic hydrochloric acids (content is more than 36.6%, g/ml) in toward distillation still 1, metering adds in absorption kettle 4
Enter 530L methyl alcohol, opening cooling tower 2 is intake, flowing water Valve, the chuck coolant media of absorption kettle 4 ties up methanol temperature into and out of valve
Hold at 0 DEG C or so, crack steam valve, in being to slowly warm up to distillation still 1 temperature at 85 DEG C, after effusion hydrogen chloride is through cooling tower 2,
Enter absorption kettle 4 after buffered tank 3 to absorb, until absorption equilibrium, closes distillation still 1 and enter valve on steam valve, surge tank 3, determine
Methanolic hydrogen chloride concentration is 27.04% (g/ml), and remaining low concentration of salt acid solution 713kg, concentration is 19.8% (g/ml), outward
Pin, for producing calcium chloride.
From above-described embodiment, the concentration of methanolic hydrogen chloride obtained in technique of the invention is more than 26%.
Compared with prior art, present invention system uses heating hydrochloric acid solution so as to the hydrogen chloride gas that volatilize, through cooling, methyl alcohol
Absorb and hydrogen chloride methanol solution is obtained, gained low-concentration hcl is used to prepare industrial calcium chloride, forms recycling economy.Solve mixed
Sour " three wastes " problem, improves hydrochloric acid solution utilization rate.
Described above fully discloses specific embodiment of the invention.It is pointed out that being familiar with the field
Scope of any change that technical staff is done to specific embodiment of the invention all without departing from claims of the present invention.
Correspondingly, the scope of claim of the invention is also not limited only to previous embodiment.
Claims (3)
1. a kind of preparation facilities of hydrogen chloride methanol solution, it is characterised in that：It includes：
Distillation still, its top is provided with solution inlet port and steam (vapor) outlet, and its bottom is provided with taphole；
Cooling tower, it is connected by the steam (vapor) outlet of the distillation still with the distillation still；
Surge tank, it is connected with the cooling tower；
Absorption kettle, it is connected with the surge tank,
Synthesis reactor, its side offers the first import and the second import, and opposite side offers first outlet,
The bottom of the distillation still is additionally provided with taphole, and the synthesis reactor is by the taphole of the distillation still and described
First import of synthesis reactor is connected with the distillation still,
Circulating cooling water inlet and circulating cooling water out are provided with the cooling tower,
Use hydrogen chloride methanol solution preparation facilities prepare the technique of hydrogen chloride methanol solution for：Hydrochloric acid is added in distillation still
Solution, heats the hydrochloric acid solution in the distillation still so as to the hydrogen chloride gas that volatilize, and the hydrogen chloride gas for volatilizing are through cooling tower
Methanol absorption in cooling, absorption kettle is obtained hydrogen chloride methanol solution, and it specifically includes following steps：
(1) toward adding hydrochloric acid solution raw material in distillation still, to adding methyl alcohol in absorption kettle；
(2) thermometer on observation absorption kettle, when temperature is at 0 DEG C, the steam (vapor) outlet of crack distillation still is slowly heated distillation still 1
~2 hours, pot temperature is set to reach 70~85 DEG C；
(3) continue to be heated to distillation still, maintenance pot temperature is 5~6 hours at 70~85 DEG C；
(4) continue to be slowly heated distillation still, and ensure the temperature of hydrogen chloride methanol solution in absorption kettle no more than 10 DEG C,
The concentration of the methanolic hydrogen chloride for obtaining is more than 26%,
Also comprise the following steps after step (4)：
When () continues to be heated to 130 DEG C to distillation still a, the steam (vapor) outlet of distillation still is closed, open bottom valve, gone out by solution
Mouth will obtain calcium chloride solution in low concentration of salt acid solution feeding synthesis reactor in distillation still with calcium carbonate reaction；
B calcium chloride solution that () will obtain in step (a) is made calcium chloride solid.
2. the preparation facilities of hydrogen chloride methanol solution according to claim 1, it is characterised in that：The hydrochloric acid solution it is dense
Degree is more than 34%.
3. the preparation facilities of hydrogen chloride methanol solution according to claim 1, it is characterised in that：The concentration of low-concentration hcl
It is less than 20%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510067984.XA CN104671208B (en) | 2015-02-09 | 2015-02-09 | Preparation device and technology for hydrogen chloride-methanol solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510067984.XA CN104671208B (en) | 2015-02-09 | 2015-02-09 | Preparation device and technology for hydrogen chloride-methanol solution |
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| Publication Number | Publication Date |
|---|---|
| CN104671208A CN104671208A (en) | 2015-06-03 |
| CN104671208B true CN104671208B (en) | 2017-05-17 |
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| CN201510067984.XA Active CN104671208B (en) | 2015-02-09 | 2015-02-09 | Preparation device and technology for hydrogen chloride-methanol solution |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1562732A (en) * | 2004-04-01 | 2005-01-12 | 上海交通大学 | Method for preparing strong hydrochloric acid through extracting and distilling deposed dilute hydrochloric acid semi continuously |
| CN1562432A (en) * | 2004-03-19 | 2005-01-12 | 冯留启 | Method for preparing supper clean, and high pure reagent of acid and rectifier unit |
| CN101185835A (en) * | 2007-08-23 | 2008-05-28 | 周滢 | Method for absorbing and using waste gases hydrogen chloride produced in chemical industrial products |
| CN103922887A (en) * | 2014-04-30 | 2014-07-16 | 南通江天化学品有限公司 | Desorption process of methanol-containing hydrochloric acid |
| CN204454572U (en) * | 2015-02-09 | 2015-07-08 | 大丰市天生药业有限公司 | A kind of preparation facilities of hydrogen chloride methanol solution |
-
2015
- 2015-02-09 CN CN201510067984.XA patent/CN104671208B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1562432A (en) * | 2004-03-19 | 2005-01-12 | 冯留启 | Method for preparing supper clean, and high pure reagent of acid and rectifier unit |
| CN1562732A (en) * | 2004-04-01 | 2005-01-12 | 上海交通大学 | Method for preparing strong hydrochloric acid through extracting and distilling deposed dilute hydrochloric acid semi continuously |
| CN101185835A (en) * | 2007-08-23 | 2008-05-28 | 周滢 | Method for absorbing and using waste gases hydrogen chloride produced in chemical industrial products |
| CN103922887A (en) * | 2014-04-30 | 2014-07-16 | 南通江天化学品有限公司 | Desorption process of methanol-containing hydrochloric acid |
| CN204454572U (en) * | 2015-02-09 | 2015-07-08 | 大丰市天生药业有限公司 | A kind of preparation facilities of hydrogen chloride methanol solution |
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| Publication number | Publication date |
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| CN104671208A (en) | 2015-06-03 |
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Effective date of registration: 20170418 Address after: 224100 Jiangsu Dafeng Industrial Park, China, the north side of the weft Road, Yancheng City, two Applicant after: Yancheng City Dafeng Union Pharmaceutical Co., Ltd. Address before: 224100 Yancheng City Huafeng Industrial Park, Dafeng City, Jiangsu on the north side of the road two Applicant before: Dafeng Tiansheng Pharmaceutical Co., Ltd. |
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