CN102617425A - Synthetic method for chelator 5- methyl-2-sulfhydryl benzyl alcohol - Google Patents
Synthetic method for chelator 5- methyl-2-sulfhydryl benzyl alcohol Download PDFInfo
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- CN102617425A CN102617425A CN2012100503016A CN201210050301A CN102617425A CN 102617425 A CN102617425 A CN 102617425A CN 2012100503016 A CN2012100503016 A CN 2012100503016A CN 201210050301 A CN201210050301 A CN 201210050301A CN 102617425 A CN102617425 A CN 102617425A
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- methyl
- methylbenzene thiophenol
- thiophenol
- sulfhydryl
- benzyl alcohol
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Abstract
The invention relates to a synthetic method for a novel substance of 5-methyl-2-sulfhydryl benzyl alcohol which is a chelator. Methyl thiophenol and formaldehyde type reagent (formalin, trioxymethylene and paraformaldehyde are possible) are subjected to a nucleophilic addition reaction in an alkaline (sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate and potassium bicarbonate are possible)aqueous solution (concentration is 1.31%-4%) to synthetize the 5-methyl-2-sulfhydryl benzyl alcohol. The synthetic method is simple in process, and isolation and purification of products are facilitated.
Description
The present invention relates to the compound method of a kind of novel substance 5-methyl-2-sulfydryl benzylalcohol.This material is a kind of sequestrant, alkalescence (can sodium hydroxide, Pottasium Hydroxide; Yellow soda ash, salt of wormwood, sodium hydrogencarbonate; Saleratus) in the aqueous solution (concentration is 1.31%~4%), nucleophilic addition is taken place in methylbenzene thiophenol and formaldehyde type reagent (can be formalin, trioxymethylene and Paraformaldehyde 96); Synthetic 5-methyl-2-sulfydryl benzylalcohol, this synthetic method craft is simple, and product is easy to separate and purifies.
The method of a kind of synthetic 5-methyl-2-sulfydryl benzylalcohol
Technical field
The present invention relates to the method for a kind of synthetic 5-methyl-2-sulfydryl benzylalcohol, belong to the technical field that fine chemical product is produced.
Technical background
In recent years, the focus of environment protection growing interest is because expanding economy produces a large amount of effluent containing heavy metal ions when a large amount of heavy metals is exploited.When heavy metal ion content has surpassed the allowance of organism, cause the sex change of biological cell and have toxicity.Suction, the direct absorption of tap water and the inrichment of biological food chain can both influence the content of heavy metal in human body.Wherein the ratio of the shared source of pollution of heavy metal ion is maximum in the water body.Therefore must strict control heavy metal wastewater thereby discharging content.
At present, the heavy metal treatment process mainly contains the precipitator method, oxidation reduction process, electrolytic process, embrane method, biological process, absorption method, ion exchange method etc.Wherein the precipitator method are on running cost or running cost, all than additive method incomparable advantage to be arranged, and are methods the most frequently used in the heavy metal containing wastewater treatment.But traditional precipitator method can't be handled heavy metal complexing waste water, and research shows that the chelating precipitator method can advanced treatment for heavy metal complexing waste water.Because heavy metal ion has special electron structure, be prone to combine formation chelating body structure and precipitating with containing O, N, S, the equiatomic sequestrant of P.And sequestrant is because it is highly sensitive, and can be recycled becomes a kind of important method of water treatment.
At present, great majority adopt and to contain two sulfydryls or amino-mercapto type sequestrant is handled heavy metal ion.Above-mentioned sequestrant has significant limitation in the heavy metal containing wastewater treatment process, two sulfydryl type sequestrants discharge highly toxic substance H easily under acidic conditions
2S is oxidized to sulfoxide and inactivation in air, the amino-type sequestrant also is prone to be oxidised with air to nitroso compound and inactivation.The present invention is to the methyl thiophenol to be the synthetic 5-methyl of raw material-2-sulfydryl benzylalcohol; Utilize Sauerstoffatom environmentally friendly; Advantage to air-stable; And the design sequestrant can form the mode of stablize six-ring with metals ion and improve chelating ability, expects to obtain a kind of novel low toxicity, heavy metal chelant efficiently.
Summary of the invention
The present invention provides the compound method of a kind of synthetic 5-methyl-2-sulfydryl benzylalcohol.This method is synthetic simple, and product is easy to separate and purifies.
The present invention realizes through following technical scheme.To be the synthetic 5-methyl of raw material-2-sulfydryl benzylalcohol technological process to the methylbenzene thiophenol, it is characterized in that: alkali (can sodium hydroxide, Pottasium Hydroxide; Yellow soda ash, salt of wormwood, sodium hydrogencarbonate; Saleratus) in the property aqueous solution (concentration is 1.31%~4%), adds methylbenzene thiophenol and 1.0~1.5 times and formaldehyde type reagent (can be formalin, trioxymethylene and Paraformaldehyde 96) to methylbenzene thiophenol amount of substance; Heat up 40~70 ℃, behind stirring and refluxing 8~24h, be cooled to 30 ℃ slightly; Add 0.5 times of sodium hydroxide or Pottasium Hydroxide to the methylbenzene thiophenol, unreacted to remove to the methylbenzene thiophenol.Continue stirring and be cooled to room temperature, filter, washing is to neutral, and is air-dry in air, obtains white solid 5-methyl-2-sulfydryl benzylalcohol.
The invention has the advantages that the compound method that a kind of new sequestrant is provided, its compound method is simple, and product is easy to separate and purifies.
Embodiment
In the there-necked flask of 100mL, add methylbenzene thiophenol 0.62g, sodium hydroxide 0.08g, zero(ppm) water 6mL and 40% formalin 0.52mL, heat up and put 50 ℃ and remain unchanged, refluxing and stirring finished reaction after 12 hours.When question response liquid is cooled to 30 ℃, add the sodium hydroxide of 0.1g, continue to be cooled to room temperature under stirring, the adularescent crystal is separated out, and crystal is filtered, and washing obtains white mealy crystal 5-methyl-2-sulfydryl benzylalcohol to neutral after the drying.
1. one kind to be the method for the synthetic 5-methyl of raw material-2-sulfydryl benzylalcohol to the methylbenzene thiophenol, it is characterized in that: alkali (can sodium hydroxide, Pottasium Hydroxide; Yellow soda ash, salt of wormwood, sodium hydrogencarbonate; Saleratus) in the property aqueous solution (concentration is 1.31%~4%), adding methylbenzene thiophenol and 1.0~1.5 times (can be formalin to the formaldehyde type reagent to methylbenzene thiophenol amount of substance; Trioxymethylene and Paraformaldehyde 96), heat up 40~70 ℃, behind stirring and refluxing 8~24h; Be cooled to 30 ℃ slightly, add 0.5 times to sodium hydroxide or Pottasium Hydroxide to methylbenzene thiophenol amount of substance, unreacted to remove to the methylbenzene thiophenol.The continuation stirring is cooled to room temperature and separates out crystal, filters, and washing is to neutrality, and is air-dry in air, obtains white solid 5-methyl-2-sulfydryl benzylalcohol.
Claims (2)
1. one kind to be the method for the synthetic 5-methyl of raw material-2-sulfydryl benzylalcohol to the methylbenzene thiophenol, it is characterized in that: alkali (can sodium hydroxide, Pottasium Hydroxide; Yellow soda ash, salt of wormwood, sodium hydrogencarbonate; Saleratus) in the property aqueous solution (concentration is 1.31% ~ 4%), adding methylbenzene thiophenol and 1.0 ~ 1.5 times (can be formalin to the formaldehyde type reagent to methylbenzene thiophenol amount of substance; Trioxymethylene and Paraformaldehyde 96), heat up 40 ~ 70 ℃, behind stirring and refluxing 8 ~ 24h; Be cooled to 30 ℃ slightly, add 0.5 times to sodium hydroxide or Pottasium Hydroxide to methylbenzene thiophenol amount of substance, unreacted to remove to the methylbenzene thiophenol.
2. the continuation stirring is cooled to room temperature and separates out crystal, filters, and washing is to neutrality, and is air-dry in air, obtains white solid 5-methyl-2-sulfydryl benzylalcohol.
Priority Applications (1)
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CN2012100503016A CN102617425A (en) | 2012-02-29 | 2012-02-29 | Synthetic method for chelator 5- methyl-2-sulfhydryl benzyl alcohol |
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CN2012100503016A CN102617425A (en) | 2012-02-29 | 2012-02-29 | Synthetic method for chelator 5- methyl-2-sulfhydryl benzyl alcohol |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108585280A (en) * | 2018-05-16 | 2018-09-28 | 东莞市三人行环境科技有限公司 | A kind for the treatment of process of the nickel waste water containing chromium-copper |
Citations (2)
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US3714264A (en) * | 1970-08-17 | 1973-01-30 | Goodyear Tire & Rubber | Alylation product of 4(methylthio) phenol |
CN102249963A (en) * | 2011-05-18 | 2011-11-23 | 长沙理工大学 | Method for synthesizing 4-methyl-2-amino thiophenol |
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2012
- 2012-02-29 CN CN2012100503016A patent/CN102617425A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3714264A (en) * | 1970-08-17 | 1973-01-30 | Goodyear Tire & Rubber | Alylation product of 4(methylthio) phenol |
CN102249963A (en) * | 2011-05-18 | 2011-11-23 | 长沙理工大学 | Method for synthesizing 4-methyl-2-amino thiophenol |
Non-Patent Citations (1)
Title |
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彭青林等: "一种巯基螯合剂的合成及处理镍矿废水的研究", 《矿冶工程》 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108585280A (en) * | 2018-05-16 | 2018-09-28 | 东莞市三人行环境科技有限公司 | A kind for the treatment of process of the nickel waste water containing chromium-copper |
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Application publication date: 20120801 |