CN104370781A - Method for removing sodium nitrite out of waste dimethyl sulfoxide salt by using composite oxidizing agent - Google Patents
Method for removing sodium nitrite out of waste dimethyl sulfoxide salt by using composite oxidizing agent Download PDFInfo
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- CN104370781A CN104370781A CN201410598309.5A CN201410598309A CN104370781A CN 104370781 A CN104370781 A CN 104370781A CN 201410598309 A CN201410598309 A CN 201410598309A CN 104370781 A CN104370781 A CN 104370781A
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- dimethyl sulfoxide
- dmso
- sodium nitrite
- abraum salt
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Abstract
The invention discloses a method for removing sodium nitrite out of waste dimethyl sulfoxide salt by using a composite oxidizing agent. The method comprises the following steps: a, pretreating the waste dimethyl sulfoxide salt: heating a certain amount of waste dimethyl sulfoxide salt to 80-100 DEG C, stirring at a speed of 150-300rpm, adding a concentrated acid for carrying out pretreatment for 5-10min, wherein the use amount of acid is 2-6% of the mass of the waste dimethyl sulfoxide salt; and b, carrying out oxidization treatment: holding the temperature of the solution obtained after pretreatment at 80-100 DEG C, slowly adding a composite oxidizing agent while stirring, reacting for 30-60min, and cooling to room temperature, wherein the use amount of the composite oxidizing agent is 6-12% of the mass of the waste dimethyl sulfoxide salt. By application of the method disclosed by the invention, the removal rate of sodium nitrite in the waste salt can reach more than 96%, the emission of sodium nitrite is reduced, the pollution to the environment is reduced, the process flow is simple, the energy consumption is low and industrial production can be realized easily.
Description
Technical field
The present invention relates to a kind of minimizing technology utilizing composite oxidant dimethyl sulfoxide (DMSO) abraum salt Sodium Nitrite.
Background technology
Dimethyl sulfoxide (DMSO) (DMSO) molecular formula is (CH
30)
2sO, normal temperature is colourless transparent liquid, and have high polarity, high-hygroscopicity, high boiling point and combustibility, toxicity is low, Heat stability is good, and most of organism such as energy is water-soluble, ethanol, acetone, benzene and chloroform are a kind of strong polar aprotic solvent.Dimethyl sulfoxide (DMSO), one, to being called as " Dimethyl Sulfoxide " and " panacea ", is widely used in petrochemical complex medicine, agricultural chemicals, Aromatics Extractive Project, lanital, electronics and national defense industry.The production technology of DMSO mainly comprises the synthesis of dimethyl thioether and oxidation two reaction members of dimethyl thioether.Dimethyl thioether synthetic method mainly contains hydrogen sulfide method, dithiocarbonic anhydride method and sodium sulfide method, and hydrogen sulfide method reaction process easily controls, and yield is higher, and hydrogen sulfide is the by product of other production process, cheap and easy to get.Dimethyl thioether oxidation dimethyl sulfoxide (DMSO) processed mainly contains nitric acid oxidation method, hydrogen peroxide method, By Ozone and nitrogen peroxide method, and nitric acid oxidation method equipment corrosion is serious, and consumes a large amount of soda acid; Hydrogen peroxide high cost; Ozonation transformation efficiency is too low; Therefore, domestic each factory generally adopts nitrogen peroxide oxidation style.During nitrogen peroxide oxidation style production dimethyl sulfoxide (DMSO), need sodium hydroxide solution to absorb excessive oxynitride, generate containing abraum salts such as SODIUMNITRATE, Sodium Nitrite and dimethyl sulfone.After testing, abraum salt is less than 5% containing Sodium Nitrite.These abraum salt utilization ratios are low at present, and major part works as offal treatment, and Sodium Nitrite is a kind of potential carcinogenic substance, poisonous, big for environment pollution.
For above situation, inventors have developed a kind of method removing dimethyl sulfoxide (DMSO) abraum salt Sodium Nitrite, through retrieval, also do not have similar approach to deliver in pertinent literature and patent up to now.
Summary of the invention
The object of the present invention is to provide a kind of method removing dimethyl sulfoxide (DMSO) abraum salt Sodium Nitrite, can more than 96% be reached by the method dimethyl sulfoxide (DMSO) abraum salt Sodium Nitrite clearance.
A kind of method removing dimethyl sulfoxide (DMSO) abraum salt Sodium Nitrite of the present invention, implemented by the following technical solutions:
Implemented by the following technical solutions:
A, the pre-treatment of dimethyl sulfoxide (DMSO) abraum salt: get a certain amount of dimethyl sulfoxide (DMSO) abraum salt, be heated to 80 DEG C-100 DEG C gradually, under certain stirring velocity, add a certain amount of acid carry out pre-treatment, stirring velocity controls as 150rpm-300rpm, the acid added is strong phosphoric acid mass concentration 85%, concentrated nitric acid mass concentration 65% or vitriol oil mass concentration 98% one wherein, the consumption of acid is 2%-6% of dimethyl sulfoxide (DMSO) abraum salt quality, controls pretreatment time 5 min-10min; Described dimethyl sulfoxide (DMSO) abraum salt refers to the by-product solid waste residue in dimethyl sulfoxide (DMSO) production process, and its main component is SODIUMNITRATE and a small amount of Sodium Nitrite, dimethyl sulfone etc., and wherein SODIUMNITRATE content is greater than 80%, and content of sodium nitrite is 1%-3%;
B, oxide treatment: the solution of pre-treatment gained is kept temperature 80 DEG C-100 DEG C, slowly add a certain amount of composite oxidant under agitation, the composite oxidant adopted is the mixing solutions of ferrous sulfate and hydrogen peroxide, wherein mass percent shared by ferrous sulfate is 4%, mass percent 40% shared by hydrogen peroxide, and surplus is water, the consumption of composite oxidant is 6%-12% of dimethyl sulfoxide (DMSO) abraum salt quality,, after reaction 30min-60min, be cooled to room temperature.
Adopt method of the present invention, dimethyl sulfoxide (DMSO) abraum salt Sodium Nitrite clearance can reach more than 96%, reduces the discharge of sodium nitrite in industrial waste salt, reduces the pollution to environment, and technical process is simple, and energy consumption is little, is easy to realize industrialization.
Embodiment
the composite oxidant adopted in embodiment is below the mixing solutions of ferrous sulfate and hydrogen peroxide, and wherein mass percent shared by ferrous sulfate is 4%, mass percent 40% shared by hydrogen peroxide, and surplus is water.Described dimethyl sulfoxide (DMSO) abraum salt refers to the by-product solid waste residue in dimethyl sulfoxide (DMSO) production process, and its main component is SODIUMNITRATE and a small amount of Sodium Nitrite, dimethyl sulfone etc., and wherein SODIUMNITRATE content is greater than 80%, and content of sodium nitrite is 1%-3%.
embodiment 1
Get 100g dimethyl sulfoxide (DMSO) abraum salt, Sodium Nitrite mass percent is 2.86%, adds in reactor, be warming up to 80 DEG C, under stirring 300rpm, add 6g nitric acid, 80 DEG C of insulation 10min, slowly add the composite oxidant of 6g under agitation, after reaction 30min, be cooled to room temperature, obtain product, after testing, Sodium Nitrite mass percent is 0.042%, and Sodium Nitrite clearance is 98.5%.
embodiment 2
Get 100g dimethyl sulfoxide (DMSO) abraum salt, Sodium Nitrite mass percent is 2.86%, adds in reactor, be warming up to 90 DEG C, under stirring 250rpm, add 4g sulfuric acid, 90 DEG C of insulation 8min, slowly add the composite oxidant of 9g under agitation, after reaction 45min, be cooled to room temperature, obtain product, after testing, Sodium Nitrite mass percent is 0.065%, and Sodium Nitrite clearance is 97.7%.
embodiment 3
Get 100g dimethyl sulfoxide (DMSO) abraum salt, Sodium Nitrite mass percent is 2.86%, adds in reactor, be warming up to 100 DEG C of composite oxidants, under stirring 150rpm, add 2g phosphoric acid, 100 DEG C of insulation 5min, slowly add the composite oxidant of 12g under agitation, after reaction 60min, be cooled to room temperature, obtain product, after testing, Sodium Nitrite mass percent is 0.096%, and Sodium Nitrite clearance is 96.6%.
Claims (1)
1. remove a method for dimethyl sulfoxide (DMSO) abraum salt Sodium Nitrite, it is characterized in that being implemented by the following technical solutions:
A, the pre-treatment of dimethyl sulfoxide (DMSO) abraum salt: get a certain amount of dimethyl sulfoxide (DMSO) abraum salt, be heated to 80 DEG C-100 DEG C gradually, under certain stirring velocity, add a certain amount of acid carry out pre-treatment, stirring velocity controls as 150rpm-300rpm, the acid added is strong phosphoric acid mass concentration 85%, concentrated nitric acid mass concentration 65% or vitriol oil mass concentration 98% one wherein, the consumption of acid is 2%-6% of dimethyl sulfoxide (DMSO) abraum salt quality, controls pretreatment time 5 min-10min; Described dimethyl sulfoxide (DMSO) abraum salt refers to the by-product solid waste residue in dimethyl sulfoxide (DMSO) production process, and its main component is SODIUMNITRATE and a small amount of Sodium Nitrite, dimethyl sulfone etc., and wherein SODIUMNITRATE content is greater than 80%, and content of sodium nitrite is 1%-3%;
B, oxide treatment: the solution of pre-treatment gained is kept temperature 80 DEG C-100 DEG C, slowly add a certain amount of composite oxidant under agitation, the composite oxidant adopted is the mixing solutions of ferrous sulfate and hydrogen peroxide, wherein ferrous sulfate accounts for mass percent is 4%, and hydrogen peroxide accounts for mass percent 40%, and surplus is water, the consumption of composite oxidant is 6%-12% of dimethyl sulfoxide (DMSO) abraum salt quality,, after reaction 30min-60min, be cooled to room temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410598309.5A CN104370781A (en) | 2014-10-31 | 2014-10-31 | Method for removing sodium nitrite out of waste dimethyl sulfoxide salt by using composite oxidizing agent |
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| CN201410598309.5A CN104370781A (en) | 2014-10-31 | 2014-10-31 | Method for removing sodium nitrite out of waste dimethyl sulfoxide salt by using composite oxidizing agent |
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| CN104370781A true CN104370781A (en) | 2015-02-25 |
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| CN201410598309.5A Pending CN104370781A (en) | 2014-10-31 | 2014-10-31 | Method for removing sodium nitrite out of waste dimethyl sulfoxide salt by using composite oxidizing agent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105294729A (en) * | 2015-11-12 | 2016-02-03 | 大连九信生物化工科技有限公司 | Method for eliminating by-product dimethyl sulfide during Moxidectin production process |
| CN105461601A (en) * | 2015-11-19 | 2016-04-06 | 瓮福（集团）有限责任公司 | An oxidation removing method of sodium nitrite in industrial waste residue of dimethyl sulfoxide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB957048A (en) * | 1959-07-30 | 1964-05-06 | Montedison Spa | Process for recovering sodium borohydride from a suspension thereof with sodium methylate in petroleum oil |
| CN101195595A (en) * | 2007-12-12 | 2008-06-11 | 湖北兴发化工集团股份有限公司 | Method for recycling dimethyl sulfone and sodium nitrate from dimethyl sulfoxide waste slag |
| CN102010354A (en) * | 2010-11-30 | 2011-04-13 | 湖北兴发化工集团股份有限公司 | Method for recycling dimethyl sulfoxide waste residue |
-
2014
- 2014-10-31 CN CN201410598309.5A patent/CN104370781A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB957048A (en) * | 1959-07-30 | 1964-05-06 | Montedison Spa | Process for recovering sodium borohydride from a suspension thereof with sodium methylate in petroleum oil |
| CN101195595A (en) * | 2007-12-12 | 2008-06-11 | 湖北兴发化工集团股份有限公司 | Method for recycling dimethyl sulfone and sodium nitrate from dimethyl sulfoxide waste slag |
| CN102010354A (en) * | 2010-11-30 | 2011-04-13 | 湖北兴发化工集团股份有限公司 | Method for recycling dimethyl sulfoxide waste residue |
Non-Patent Citations (1)
| Title |
|---|
| 朱其虎: "催化剂对双氧水氧化淀粉的催化效果研究", 《轻工科技》, no. 6, 15 June 2014 (2014-06-15), pages 57 - 58 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105294729A (en) * | 2015-11-12 | 2016-02-03 | 大连九信生物化工科技有限公司 | Method for eliminating by-product dimethyl sulfide during Moxidectin production process |
| CN105461601A (en) * | 2015-11-19 | 2016-04-06 | 瓮福（集团）有限责任公司 | An oxidation removing method of sodium nitrite in industrial waste residue of dimethyl sulfoxide |
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Application publication date: 20150225 |