CN106397286B - A kind of processing method of isooctyl thioglycolate rectifying waste material - Google Patents
A kind of processing method of isooctyl thioglycolate rectifying waste material Download PDFInfo
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- CN106397286B CN106397286B CN201610728336.9A CN201610728336A CN106397286B CN 106397286 B CN106397286 B CN 106397286B CN 201610728336 A CN201610728336 A CN 201610728336A CN 106397286 B CN106397286 B CN 106397286B
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- waste material
- isooctyl thioglycolate
- organic phase
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- rectifying waste
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/26—Separation; Purification; Stabilisation; Use of additives
- C07C319/28—Separation; Purification
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- Organic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention provides a kind of processing method of isooctyl thioglycolate rectifying waste material.This method includes following steps：Isooctyl thioglycolate rectifying waste material is washed with diluted alkaline, adjusts organic phase pH value, oxidation processes organic phase, vacuum dehydration drying process after washing.Operation is simple for the processing method of the present invention, cost is cheap, the content of isooctyl thioglycolate is relatively low in product after processing, the content of isooctyl thioglycolate is reduced to 0.20%, reduce the pollution to environment, rectifying waste material after processing can be used for the processing of flexible PVC, and it is well application prospect to have.
Description
Technical field
The present invention relates to a kind of processing method of isooctyl thioglycolate rectifying waste material, and it is different pungent specifically to reduce TGA
Mercaptans content in ester rectifying waste material, the method for improving the purity of sulfide in rectifying waste material.
Background technology
Side reaction can occur during isooctyl thioglycolate is synthesized, generate monosulfide and disulphide.These
The boiling point of accessory substance is far above the boiling point of isooctyl thioglycolate, in isooctyl thioglycolate distillation process, remains in rectifying
Bottom turns into rectifying waste material.
The country is rarely reported on isooctyl thioglycolate waste disposal.Wang Yanjun discloses a kind of different using TGA
The method of the residual night processing in monooctyl ester bottom.Isooctyl thioglycolate bottom residual night is subjected to saponification process, reclaims isooctanol.Such a place
Water-washing step needs to consume substantial amounts of water in reason method, and ultimate yield is not high, and processing cost is higher.This rectifying waste material is used
Processed in flexible PVC, plasticization effect is preferable, but has a small amount of isooctyl thioglycolate in rectifying waste material, sulfide staining be present and asks
Topic, so to reduce the content of isooctyl thioglycolate in rectifying waste material.
Hydrocarbons containing sulfydryl are also known as thiol class substance.Processing on mercaptan has more report in gasoline purification
Road.Mercaptan in gasoline is low-grade thioalcohol mostly, and the solubility in alkali lye is very big, and contained in rectifying waste material in the present invention
Isooctyl thioglycolate belongs to higher mercaptan, and the solubility in alkali lye is limited.A kind of conventional processing method of mercaptan from gasoline
It is exactly to use alkali liquor absorption, oxidation processes then is carried out to the mercaptan in alkali lye again.Or by the gasoline containing mercaptan by containing
The carrier of high-efficient oxidant and catalyst, directly removes mercaptan.These processing methods need the height of specific equipment and costliness
Imitate catalyst and oxidant.For rectifying waste material is handled, cost is too high, is not easy to carry out.And only with alkali liquor absorption
Or direct oxidation method is handled, the content of the isooctyl thioglycolate in final products is higher, it is impossible to effectively lowers sulfydryl
The content of 2-ethyl hexyl ethanoate.
The content of the invention
In order to solve the above problems, the present invention provides a kind of processing method of isooctyl thioglycolate rectifying waste material.The party
Method key is first to carry out diluted alkaline washing to rectifying waste material, then adjusts the pH value of organic phase again, and oxidation processes are carried out to organic phase,
The isooctyl thioglycolate content in rectifying waste material is reduced, improves the purity of sulfide.
The present invention provides a kind of processing method of isooctyl thioglycolate rectifying waste material, comprises the following steps：
(1) diluted alkaline washs：Isooctyl thioglycolate ester rectifying waste material is washed with sig water；
(2) organic phase pH value is adjusted：The organic phase in step (1) is taken to adjust pH value；
(3) oxidation processes organic phase：The organic phase after regulation pH value is taken, oxidant is added and carries out oxidation reaction；
(4) vacuum dehydration is handled after washing：After oxidation reaction carry out liquid separation take oil reservoir, then again washing liquid separation take it is organic
Phase, vacuum dehydration drying process organic phase.
In the method for the invention, the rectifying waste material is in isooctyl thioglycolate production process produced by rectification step
Bottom material.Contained main matter and its content are in the rectifying waste material：Isooctanol 3% or so, isooctyl thioglycolate 5%
Left and right, monosulfide 27% or so, disulphide 62% or so.
In the step (1) of the method for the invention：
Dilute alkaline soln used refers to sodium hydroxide solution of the concentration in 4%-8%, preferably 6%-7%.Hydroxide used
The mass ratio of sodium solution and rectifying waste material is 0.6:1-1.5:1, preferably 0.9:1-1.1:1.Wash time is 10min-30min.
In the method for the invention, in step (2)：
The pH value for adjusting oil phase is 6-9, preferable ph 8-8.6.
In the method for the invention, in step (3)：
The amount of the oxidant of addition, according to mole with isooctyl thioglycolate in isooctyl thioglycolate ester rectifying waste material
Than for 1.5:1-5:1, preferably 2:1-4.5:1.
Oxidant used is hydrogen peroxide or sodium hypochlorite, preferably sodium hypochlorite.
Further, hydrogen peroxide concentration 25-35wt%, sodium hypochlorite concentration are 15-25wt%.
Preferably, hydrogen peroxide concentration 30wt%, sodium hypochlorite concentration are 20wt%.
The oxidizing temperature of step (3) is 70-80 DEG C.Oxidization time is 30min-120min, preferably 50-70min.
Step (4) vacuum dehydration drying temperature is 70-90 DEG C.
The present invention is entered using diluted alkaline washing and the oxidizing method being combined to isooctyl thioglycolate rectifying waste material
Row is handled, and the content of isooctyl thioglycolate is relatively low in the product after processing, and the processing method technology chain is shorter, simple to operate easy
Row, operating cost are cheap.
Embodiment
Following examples are used to illustrate the present invention, but are not limited to the scope of the present invention.
First, rectifying waste material source and its main component.
Rectifying of embodiment of the present invention waste material is different pungent from TGA caused by Hubei Benxing Chemical Co., Ltd.
Ester rectifying waste material.Specific composition and content be isooctanol 3% or so, isooctyl thioglycolate 5% or so, the left side of monosulfide 27%
The right side, disulphide 62% or so.
Embodiment 1 handles the method (1) of isooctyl thioglycolate rectifying waste material
Isooctyl thioglycolate rectifying waste material 250g is taken, is washed with 6%NaOH solution 250g, washs 20min, liquid separation has taken
Machine phase.The pH most 8.2 of oil reservoir is adjusted, adds 20wt%NaClO solution 49.5g, 70-80 DEG C of reaction 1h.Divide after completion of the reaction
Liquid takes organic phase, adds appropriate water washing, and liquid separation again takes organic phase.Organic phase is dried in 80 DEG C of vacuum dehydrations.Sampling detection
The content 0.20% of isooctyl thioglycolate.
Embodiment 2 handles the method (2) of isooctyl thioglycolate rectifying waste material
Isooctyl thioglycolate rectifying waste material 250g is taken, is washed with 7%NaOH solution 200g, washs 15min, liquid separation has taken
Machine phase.The pH most 8.0 of oil reservoir is adjusted, adds 30wt% hydrogen peroxide 30g, 70 DEG C of reaction 70min.Liquid separation has taken after completion of the reaction
Machine phase, appropriate water washing is added, liquid separation again takes organic phase.Organic phase is dried in 90 DEG C of vacuum dehydrations.Sampling detection sulfydryl second
The content 0.53% of the different monooctyl ester of acid.
Embodiment 3 handles the method (3) of isooctyl thioglycolate rectifying waste material
Isooctyl thioglycolate rectifying waste material 250g is taken, is washed with 7%NaOH solution 200g, washs 30min, liquid separation has taken
Machine phase.The pH most 6.2 of oil reservoir is adjusted, adds 30wt% hydrogen peroxide 30g, 60 DEG C of reaction 1.5h.Liquid separation has taken after completion of the reaction
Machine phase, appropriate water washing is added, liquid separation again takes organic phase.Organic phase is dried in 90 DEG C of vacuum dehydrations.Sampling detection sulfydryl second
The content 0.75% of the different monooctyl ester of acid.
Embodiment 4 handles the method (4) of isooctyl thioglycolate rectifying waste material
Isooctyl thioglycolate rectifying waste material 250g is taken, is washed with 6%NaOH solution 250g, washs 15min, liquid separation has taken
Machine phase, add 20wt%NaClO solution 45g, 70-80 DEG C of reaction 1.5h.Liquid separation takes organic phase after completion of the reaction, adds appropriate
Water washing, again liquid separation take organic phase.Organic phase is dried in 80 DEG C of vacuum dehydrations.The content of sampling detection isooctyl thioglycolate
0.27%.
The contrast test of embodiment 5
Isooctyl thioglycolate rectifying waste material 250g is taken, is washed with 8%NaOH solution 250g, washs 20min, liquid separation has taken
Machine phase.250mL water washings are added, liquid separation again takes organic phase.Organic phase is dried in 80 DEG C of vacuum dehydrations.Sampling detection TGA
The content 2.43% of different monooctyl ester.The contrast test of embodiment 6
Take isooctyl thioglycolate rectifying waste material 250g, add 20wt%NaClO solution 150g and the 0.5g concentrated sulfuric acids, 80 DEG C
React 1h.Liquid separation takes organic phase again.Organic phase is dried in 80 DEG C of vacuum dehydrations.The content of sampling detection isooctyl thioglycolate
20.6%.
Although above the present invention is described in detail with a general description of the specific embodiments,
On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements, belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (10)
1. a kind of processing method of isooctyl thioglycolate rectifying waste material, it is characterised in that comprise the following steps：
(1) diluted alkaline washs：Isooctyl thioglycolate ester rectifying waste material is washed with sig water；
Wherein, sig water used in step (1) is the sodium hydroxide solution that concentration is 4%-8%；
(2) organic phase pH value is adjusted：The organic phase in step (1) is taken to adjust pH value；
(3) oxidation processes organic phase：The organic phase after regulation pH value is taken, oxidant is added and carries out oxidation reaction；
Wherein, step (3) described oxidant is hydrogen peroxide or sodium hypochlorite；
(4) vacuum dehydration is handled after washing：Liquid separation is carried out after oxidation reaction and takes oil reservoir, then washing liquid separation takes organic phase again,
Vacuum dehydration drying process organic phase.
2. processing method according to claim 1, it is characterised in that sig water used in step (1) is that concentration is 6%-8%
Sodium hydroxide solution.
3. processing method according to claim 1, it is characterised in that step (1) sig water and isooctyl thioglycolate ester
The mass ratio of rectifying waste material is 0.6:1-1.5:1.
4. processing method according to claim 1, it is characterised in that step (1) wash time is 10-30min.
5. processing method according to claim 1, it is characterised in that the pH value of step (2) regulation oil phase is 6-9.
6. processing method according to claim 1, it is characterised in that the isooctyl thioglycolate rectifying waste material is sulfydryl
Bottom caused by rectification step is expected in 2-ethyl hexyl ethanoate production process；Included in the rectifying waste material：Isooctanol 3%, sulfydryl
2-ethyl hexyl ethanoate 5%, monosulfide 27%, disulphide 62%.
7. processing method according to claim 6, it is characterised in that step (3) add oxidant amount, according to mercapto
The mol ratio of isooctyl thioglycolate is 1.5 in the different monooctyl ester ester rectifying waste material of guanidine-acetic acid:1-5:1.
8. according to any described processing methods of claim 1-7, it is characterised in that the oxidizing temperature of step (3) is 70-80
℃。
9. according to any described processing methods of claim 1-7, it is characterised in that the oxidization time of step (3) is 30min-
120min。
10. according to any described processing methods of claim 1-7, it is characterised in that vacuum dehydration drying temperature in step (4)
For 70-90 DEG C.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318750A (en) * | 2008-07-22 | 2008-12-10 | 湖北犇星化工有限责任公司 | Method for treating waste water from acetic acid mercapto- isooctyl ester |
| CN101445268A (en) * | 2008-12-19 | 2009-06-03 | 兀吉康 | Technique for recovering zinc chloride from waste water in reduction process of isooctyl thioglycolate |
| CN101613309A (en) * | 2009-07-28 | 2009-12-30 | 湖北犇星化工有限责任公司 | The preparation method of isooctyl mercaptoacetate |
-
2016
- 2016-08-25 CN CN201610728336.9A patent/CN106397286B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318750A (en) * | 2008-07-22 | 2008-12-10 | 湖北犇星化工有限责任公司 | Method for treating waste water from acetic acid mercapto- isooctyl ester |
| CN101445268A (en) * | 2008-12-19 | 2009-06-03 | 兀吉康 | Technique for recovering zinc chloride from waste water in reduction process of isooctyl thioglycolate |
| CN101613309A (en) * | 2009-07-28 | 2009-12-30 | 湖北犇星化工有限责任公司 | The preparation method of isooctyl mercaptoacetate |
Non-Patent Citations (2)
| Title |
|---|
| FENTON试剂氧化处理巯基乙酸异辛酯生产废水;倪生良 等;《精细石油化工》;20051231(第3期);第62-64页 * |
| 从巯基乙酸异辛酯釜底残液中回收异辛醇的工艺研究;王彦军;《有色矿冶》;20061231;第22卷(第6期);第60-62页 * |
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Address after: 441300 No. 9 High-tech Industrial Development Zone, Suizhou City, Hubei Province Patentee after: Hubei Gongxing New Materials Co., Ltd. Address before: 441300 No. 9 Economic and Technological Development Zone, Suizhou City, Hubei Province Patentee before: Hubei Benxing Chemical Co., Ltd. |