CN104341328A - Method for producing ethanethiol by utilizing distilled crude methanol residue liquid in production process of sodium hydrosulfite - Google Patents
Method for producing ethanethiol by utilizing distilled crude methanol residue liquid in production process of sodium hydrosulfite Download PDFInfo
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- CN104341328A CN104341328A CN201410548871.7A CN201410548871A CN104341328A CN 104341328 A CN104341328 A CN 104341328A CN 201410548871 A CN201410548871 A CN 201410548871A CN 104341328 A CN104341328 A CN 104341328A
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- production process
- residual liquid
- vat powder
- sulfur alcohol
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Abstract
The invention belongs to the technical field of ethanethiol preparation, and in particular relates to a method for producing ethanethiol by utilizing a distilled crude methanol residue liquid in a production process of sodium hydrosulfite. The method comprises the following steps: (1) standing the distilled crude methanol residue liquid generated in the production process of the sodium hydrosulfite and then separating organic matters floating above the surface of water so as to separate a material A and a material B; and (2) carrying out separation and purification on the material B obtained in the step (1) via a distillation method so as to obtain the ethanethiol. According to the method, the ethanethiol product is obtained in a separation and purification manner via the distillation method by skillfully utilizing the density and the boiling point of the ethanethiol; the treatment difficulty and the treatment cost of the distilled crude methanol residue liquid in the production process of the sodium hydrosulfite are reduced; and high-value products such as the ethanethiol, methyl formate and the like are efficiently recycled, so that the economic benefit of an enterprise is increased, the production cost of the sodium hydrosulfite is lowered and the market competition ability of the enterprise is enhanced.
Description
Technical field
The invention belongs to sulfur alcohol preparing technical field, particularly relate to a kind of method utilizing crude carbinol distillation residual liquid production sulfur alcohol in vat powder production process.
Background technology
At present, vat powder is produced and is mainly adopted sodium formate method, in order to suppress the generation of side reaction in vat powder production process---namely eliminate the by product Sulfothiorine (Na in vat powder building-up process
2s
2o
3), with the main content of Guarantee Insurance powder, each manufacturing enterprise all adds oxyethane (C in vat powder building-up process
2h
4o) Sulfothiorine that side reaction generates is sheltered.Owing to the addition of oxyethane in vat powder production process, oxyethane and Sulfothiorine are reacted, generate sulfur alcohol (CH
3cH
2sH), methyl-formiate (HCOOCH
3) and sodium sulfate (Na
2sO
4), its reaction equation is: 2C
2h
4o+Na
2s
2o
3+ H
2o=CH
3cH
2sH+HCOOCH
3+ Na
2sO
4.
In prior art, the crude carbinol distillation residual liquid produced in vat powder production process mainly uses the patent of the applicant---and the patent No. is that a kind of " method utilizing crude carbinol distillation residual liquid in vat powder production process to produce sodium formiate " of ZL03112293.0 processes, therefrom reclaim sodium formiate, produce batching for vat powder and use.But, find in production practice: the sodium formiate purity that the concrete technical scheme in the disclosure patent not only reclaims is low, and not to the organism in crude carbinol distillation residual liquid in vat powder production process---sulfur alcohol and methyl-formiate effectively recycle, and be through pre-concentration, after vacuum concentration and Crystalline extraction, produce organic tarry as Hazardous wastes, the unit giving qualification focuses on, cause crude carbinol distillation residual liquid intractability in vat powder production process large, processing cost is high, the Hazardous wastes amount produced is large, and greatly waste a lot of valuable organism, reduce enterprise profit.
Wherein, (1), sulfur alcohol (CH
3cH
2sH) be one of common mercaptans, in structure by the Sauerstoffatom in ethanol by sulphur substitute obtain, be colourless liquid, have strong garlic smell; Fusing point :-147 DEG C, relative density (water=1): 0.84, boiling point: 36.2 DEG C, flash-point :-45 DEG C, is slightly soluble in water, is dissolved in most organic solvent such as ethanol, ether.Sulfur alcohol is a kind of important pesticide intermediate, for the synthesis of organic phosphorous insecticide phorate, thiodemeton, isothioate, Systox, demeton_S_methyl and weedicide sethoxydim etc., in addition, what also can be used as reagent and gas adds stink agent, liquid fuel additive, and sulfur alcohol also can be used for the organic syntheses such as medicine.
(2), methyl-formiate (HCOOCH
3) be colourless liquid, have aromatic odour, fusing point :-99.8 DEG C, boiling point: 32.0 DEG C, relative density (water=1): 0.98, is dissolved in ethanol, ether, methyl alcohol.Methyl-formiate is the epochmaking intermediate of C-1 chemistry, can directly with the smoke fumigant and the sterilant that deal with Yan grass, dried fruit, cereal etc.; Also the solvent of soluble cotton, cellulose acetate is commonly used for; Pharmaceutically, be commonly used for the synthesis material of the medicines such as sulfonic acid methyl pyrimidine, sulfonic acid Sulfamonomethoxine, anti-tussive agents dromethan, in vat powder production process, also can be converted into raw material sodium formiate (HCOONa) and the methyl alcohol (CH of vat powder production
3oH), reaction equation: HCOOCH
3+ NaOH=HCOONa+CH
3oH.
Summary of the invention
The present invention is directed to the deficiency that above-mentioned prior art exists, provide a kind of crude carbinol distillation residual liquid utilized in vat powder production process, the method for High-efficient Production high purity sulfur alcohol.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of method utilizing crude carbinol distillation residual liquid production sulfur alcohol in vat powder production process, and step is as follows:
(1) the crude carbinol distillation residual liquid produced in vat powder production process is carried out leave standstill after, the organism swimming in more than the water surface is separated, isolates material A and material B;
(2) the material B obtained step (1) adopts rectification method to carry out separating-purifying, obtains methyl-formiate and sulfur alcohol respectively.
Wherein, after the crude carbinol distillation residual liquid described in step (1) carries out leaving standstill, according to the separation surface of material A and material B, control its liquid level and be separated.
Material A described in step (1) is the organic crude carbinol distillation residual liquid of removing, and described material B is for containing the organic liquid such as sulfur alcohol, methyl-formiate.
The material A obtained in step (1) adopts the patent No. of the applicant to be that a kind of " method utilizing crude carbinol distillation residual liquid in vat powder production process to produce sodium formiate " of ZL03112293.0 processes, by material A---remove organic crude carbinol distillation residual liquid pressure >=0.3MPa water vapour, pre-concentration is carried out under temperature 100 DEG C ~ 130 DEG C conditions, the secondary steam utilizing pre-concentration to produce is-0.05MPa ~-0.08MPa at vacuum pressure, vacuum concentration is carried out under DEG C condition of temperature≤80, again at pressure-0.05MPa ~-0.08MPa, vacuum crystallization is carried out under DEG C condition of Tc≤90, at pressure-0.05MPa ~-0.08MPa, supernatant after continuation stirring 10min under extraction temperature 50 DEG C ~ 80 DEG C conditions, reclaim sodium formiate, produce batching for vat powder to use.
First material B described in step (2) enters in pre-rectifying tower, pre-rectifying is carried out under controlling the condition of pressure-0.01MPa ~-0.02MPa, vapor pressure 0.1MPa ~ 0.25MPa in tower top temperature 32.5 DEG C ± 1 DEG C, tower, the gas of pre-rectifying tower overhead extraction is after condensation, the material obtained is mainly the low-boiling-point organic compound matter such as methyl-formiate, and this material returns vat powder and produces batching use; Pre-rectifying tower tower reactor Produced Liquid enters in two-stage rectification tower, rectifying is continued under controlling the condition of pressure-0.01MPa ~-0.02MPa, vapor pressure 0.1MPa ~ 0.25MPa in two-stage rectification tower top temperature 36.5 DEG C ± 1 DEG C, tower, the gas of two-stage rectification column overhead extraction, after condensation, obtains sulfur alcohol.
The sulfur alcohol content obtained in step (2) is more than 95%.
The invention has the beneficial effects as follows: the present invention utilizes crude carbinol distillation residual liquid in vat powder production process to produce sulfur alcohol, utilizes density and the boiling point of sulfur alcohol dexterously, adopts two-stage rectification method to carry out separating-purifying, obtained sulfur alcohol product.Wherein, the phlegma of pre-rectifying tower overhead extraction is mainly the low-boiling point materials such as methyl-formiate, and this material returns vat powder and produces batching use, reduces the production cost of vat powder.Present invention reduces intractability and the processing cost of crude carbinol distillation residual liquid in vat powder production process, the refuse that is safe from danger in treating processes produces, the high-value products such as high efficiente callback sulfur alcohol, methyl-formiate, improve the economic benefit of enterprise, reduce vat powder production cost, improve the market competitiveness of enterprise.
Embodiment
Be described principle of the present invention and feature below in conjunction with example, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Embodiment 1
Utilize crude carbinol distillation residual liquid in vat powder production process to produce a method for sulfur alcohol, step is as follows:
(1), after being left standstill in separating tank by the crude carbinol distillation residual liquid in vat powder production process, organism swims in more than the water surface, controls interfacial liquid level and is separated the organism swimming in more than the water surface, isolates material A and material B; Wherein, described material A is the organic crude carbinol distillation residual liquid of removing, and described material B is for containing the organic liquid such as sulfur alcohol, methyl-formiate;
(2) material A processes according to the ZL03112293.0 " a kind of method utilizing crude carbinol distillation residual liquid in vat powder production process to produce sodium formiate " of the applicant, reclaims sodium formiate, produces batching use for vat powder;
(3) material B squeezes in pre-rectifying tower tower reactor by organism impeller pump, pre-rectifying is carried out under controlling the condition of pressure-0.01MPa, vapor pressure 0.1MPa in tower top temperature 32 DEG C, tower, the gas of pre-rectifying tower overhead extraction is after condensation, the material obtained is mainly the low-boiling point materials such as methyl-formiate, and this material returns vat powder and produces batching use; Pre-rectifying tower tower reactor Produced Liquid enters in two-stage rectification tower, rectifying is continued under controlling the condition of pressure-0.01MPa, vapor pressure 0.1MPa in two-stage rectification tower top temperature 36 DEG C, tower, the gas of two-stage rectification column overhead extraction is after condensation, obtain the sulfur alcohol of content 95%, send into sulfur alcohol basin.
Embodiment 2
Utilize crude carbinol distillation residual liquid in vat powder production process to produce a method for sulfur alcohol, step is as follows:
(1), after being left standstill in separating tank by the crude carbinol distillation residual liquid in vat powder production process, organism swims in more than the water surface, controls interfacial liquid level and is separated the organism swimming in more than the water surface, isolates material A and material B; Wherein, described material A is the organic crude carbinol distillation residual liquid of removing, and described material B is for containing the organic liquid such as sulfur alcohol, methyl-formiate;
(2) material A processes according to the ZL03112293.0 " a kind of method utilizing crude carbinol distillation residual liquid in vat powder production process to produce sodium formiate " of the applicant, reclaims sodium formiate, produces batching use for vat powder;
(3) material B squeezes in pre-rectifying tower tower reactor by organism impeller pump, pre-rectifying is carried out under controlling the condition of pressure-0.015MPa, vapor pressure 0.15MPa in tower top temperature 32.5 DEG C, tower, the gas of pre-rectifying tower overhead extraction is after condensation, the material obtained is mainly the low-boiling point materials such as methyl-formiate, and this material returns vat powder and produces batching use; Pre-rectifying tower tower reactor Produced Liquid enters in two-stage rectification tower, rectifying is continued under controlling the condition of pressure-0.015MPa, vapor pressure 0.15MPa in two-stage rectification tower top temperature 36.5 DEG C, tower, the gas of two-stage rectification column overhead extraction is after condensation, obtain the sulfur alcohol of content 96%, send into sulfur alcohol basin.
Embodiment 3
Utilize crude carbinol distillation residual liquid in vat powder production process to produce a method for sulfur alcohol, step is as follows:
(1), after being left standstill in separating tank by the crude carbinol distillation residual liquid in vat powder production process, organism swims in more than the water surface, controls interfacial liquid level and is separated the organism swimming in more than the water surface, isolates material A and material B; Wherein, described material A is the organic crude carbinol distillation residual liquid of removing, and described material B is for containing the organic liquid such as sulfur alcohol, methyl-formiate;
(2) material A processes according to the ZL03112293.0 " a kind of method utilizing crude carbinol distillation residual liquid in vat powder production process to produce sodium formiate " of the applicant, reclaims sodium formiate, produces batching use for vat powder;
(3) material B squeezes in pre-rectifying tower tower reactor by organism impeller pump, pre-rectifying is carried out under controlling the condition of pressure-0.02MPa, vapor pressure 0.2MPa in tower top temperature 33 DEG C, tower, the gas of pre-rectifying tower overhead extraction is after condensation, the material obtained is mainly the low-boiling point materials such as methyl-formiate, and this material returns vat powder and produces batching use; Pre-rectifying tower tower reactor Produced Liquid enters in two-stage rectification tower, rectifying is continued under controlling the condition of pressure-0.02MPa, vapor pressure 0.2MPa in two-stage rectification tower top temperature 37 DEG C, tower, the gas of two-stage rectification column overhead extraction is after condensation, obtain the sulfur alcohol of content 97%, send into sulfur alcohol basin.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. utilize crude carbinol distillation residual liquid in vat powder production process to produce a method for sulfur alcohol, it is characterized in that step is as follows:
(1) the crude carbinol distillation residual liquid produced in vat powder production process is carried out leave standstill after, the organism swimming in more than the water surface is separated, isolates material A and material B;
(2) the material B obtained step (1) adopts rectification method to carry out separating-purifying, obtains methyl-formiate and sulfur alcohol respectively.
2. a kind of method utilizing crude carbinol distillation residual liquid production sulfur alcohol in vat powder production process according to claim 1, it is characterized in that the crude carbinol distillation residual liquid described in step (1) carry out leave standstill after, according to the separation surface of material A and material B, control its liquid level and be separated.
3. a kind of method utilizing crude carbinol distillation residual liquid production sulfur alcohol in vat powder production process according to claim 1, is characterized in that the material A described in step (1) is for the organic crude carbinol distillation residual liquid of removing.
4. a kind of method utilizing crude carbinol distillation residual liquid production sulfur alcohol in vat powder production process according to claim 1, is characterized in that the material B described in step (1) is for containing organic liquid.
5. a kind of method utilizing crude carbinol distillation residual liquid production sulfur alcohol in vat powder production process according to claim 1, it is characterized in that the material A pressure >=0.3MPa water vapour will obtained in step (1), pre-concentration is carried out under temperature 100 DEG C ~ 130 DEG C conditions, the secondary steam utilizing pre-concentration to produce is-0.05MPa ~-0.08MPa at vacuum pressure, vacuum concentration is carried out under DEG C condition of temperature≤80, again at pressure-0.05MPa ~-0.08MPa, vacuum crystallization is carried out under DEG C condition of Tc≤90, at pressure-0.05MPa ~-0.08MPa, supernatant after continuation stirring 10min under extraction temperature 50 DEG C ~ 80 DEG C conditions, reclaim sodium formiate, produce batching for vat powder to use.
6. a kind of method utilizing crude carbinol distillation residual liquid production sulfur alcohol in vat powder production process according to claim 1, it is characterized in that the material B described in step (2) first enters in pre-rectifying tower, pre-rectifying is carried out under controlling the condition of pressure-0.01MPa ~-0.02MPa, vapor pressure 0.1MPa ~ 0.25MPa in tower top temperature 32.5 DEG C ± 1 DEG C, tower, the gas of pre-rectifying tower overhead extraction is after condensation, obtain low-boiling-point organic compound matter, this material returns vat powder and produces batching use; Pre-rectifying tower tower reactor Produced Liquid enters in two-stage rectification tower, under controlling the condition of pressure-0.01MPa ~-0.02MPa, vapor pressure 0.1MPa ~ 0.25MPa in two-stage rectification tower top temperature 36.5 DEG C ± 1 DEG C, tower, continue rectifying, the gas of two-stage rectification column overhead extraction, after condensation, obtains sulfur alcohol.
7. a kind of method utilizing crude carbinol distillation residual liquid production sulfur alcohol in vat powder production process according to claim 6, is characterized in that described low-boiling-point organic compound matter main component is methyl-formiate.
8. a kind of method utilizing crude carbinol distillation residual liquid production sulfur alcohol in vat powder production process according to claim 1, is characterized in that the sulfur alcohol content obtained in step (2) is more than 95%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111518001A (en) * | 2020-04-28 | 2020-08-11 | 烟台市金河保险粉厂有限公司 | Method for preparing 2-mercaptoethanol from sodium hydrosulfite production waste liquid |
| CN115925595A (en) * | 2022-12-02 | 2023-04-07 | 宁夏一帆生物科技有限公司 | Concentration method of low-content mercaptan compound |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111518001A (en) * | 2020-04-28 | 2020-08-11 | 烟台市金河保险粉厂有限公司 | Method for preparing 2-mercaptoethanol from sodium hydrosulfite production waste liquid |
| CN115925595A (en) * | 2022-12-02 | 2023-04-07 | 宁夏一帆生物科技有限公司 | Concentration method of low-content mercaptan compound |
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Denomination of invention: A method for producing ethanethiol from the residue of crude methanol rectification in the production of sodium bicarbonate Effective date of registration: 20220531 Granted publication date: 20160309 Pledgee: Yantai Rural Commercial Bank Co.,Ltd. Pledgor: Yantai Jinhe Sodium Hydrosulfite Co.,Ltd. Registration number: Y2022980006715 |
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Date of cancellation: 20230523 Granted publication date: 20160309 Pledgee: Yantai Rural Commercial Bank Co.,Ltd. Pledgor: Yantai Jinhe Sodium Hydrosulfite Co.,Ltd. Registration number: Y2022980006715 |
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Denomination of invention: A method for producing ethyl mercaptan from crude methanol distillation residue in the production process of sodium hydrosulfite Effective date of registration: 20230529 Granted publication date: 20160309 Pledgee: Yantai Rural Commercial Bank Co.,Ltd. Pledgor: Yantai Jinhe Sodium Hydrosulfite Co.,Ltd. Registration number: Y2023980041912 |