CN101665258A - Process for recovering magnesium salts from Grignard reaction wastewater - Google Patents
Process for recovering magnesium salts from Grignard reaction wastewater Download PDFInfo
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- CN101665258A CN101665258A CN200810042398A CN200810042398A CN101665258A CN 101665258 A CN101665258 A CN 101665258A CN 200810042398 A CN200810042398 A CN 200810042398A CN 200810042398 A CN200810042398 A CN 200810042398A CN 101665258 A CN101665258 A CN 101665258A
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Abstract
The invention provides a method for recovering magnesium salts from Grignard reaction wastewater, which comprises the following steps of: using alkali metal hydroxide to adjust the pH value of the Grignard reaction wastewater to be between 4 and 5; then adding carbonate into the wastewater to adjust the pH value to be between 8 and 12; and filtering and collecting a precipitate. The method has a simple process as well as simple and convenient operation, a used reagent is cheap and easy to obtain (all reagents can be bought from the market), the magnesium salts can be recovered at a high recovery rate and a low recovery cost, and an obtained product, namely basic magnesium carbonate has broad application, so the method has great industrial applicability.
Description
Technical field
The invention belongs to the synthetic field of chemical industry, be specifically related to from the waste water of grignard reaction, reclaim the method for magnesium salts.
Background technology
Alkyl magnesium halide RMgX is called for short Grignard reagent, is one of reagent that is most widely used in the organic synthesis.The reaction that relates to Grignard reagent is called grignard reaction, and this is the important reaction of a class in chemical industry widespread uses such as fine chemistry industry, medicine, agricultural chemicals.Usually the magnesium among the Grignard reagent RMgX is converted into the inorganic salt magnesium halide after reaction finishes, and is dissolved in the waste water of grignard reaction.The waste water of magnesium halide containing directly is discharged as chemical engineering sewage generally speaking.This causes serious pollution to environment on the one hand, has also caused the significant wastage of resource on the other hand.
It is acid that the waste water that grignard reaction produces is usually, and what comprehensive utilization value was wherein arranged mainly is halide-ions and magnesium ion.Document CN200410073583 has reported by generating sal epsom and has reclaimed magnesium ion, this removal process needs earlier a large amount of aqueous solution to be concentrated, add a large amount of vitriol oils then and generate sal epsom, back needs very high energy consumption, the vitriol oil in one step of back can cause serious corrosion to equipment, have secondary pollution, and sal epsom in the aqueous solution, have certain solubleness (20 ℃, 35.1g/100g water; 25 ℃ of 37.4g/100g water).So just caused the recovery magnesium ion incomplete, still can pollute after the discharging environment.CN101130485 has reported by generating magnesium chloride and has reclaimed magnesium ion, magnesium chloride is water miscible salt, need during recovery the whole evaporates to dryness of water, need very big energy consumption, and may there be other ion in the aqueous solution, also can because of the evaporate to dryness of the aqueous solution with the magnesium ion coprecipitation, can not reach the purpose of Separation and Recovery.
Because the magnesium in the waste water is dissolved in the water with the form of inorganic salt magnesium halide, is difficult for reclaiming and purifies.If solution is transferred to alkalescence, then magnesium ion can be produced magnesium hydrate precipitate and separate from waste water, and very thin colloidal precipitates but magnesium hydroxide is a kind of particle, wants to reach very difficulty of solid-liquid separation by filtration.How the magnesium salts in the depleted Gram-waste water is converted into useful, be easy to isolating magnesium salts, problem to be solved by this invention just.
Summary of the invention
The technical problem to be solved in the present invention provide a kind of easy and simple to handle, with low cost, the rate of recovery is high reclaims the method for magnesium salts from Grignard reaction wastewater.
Method of the present invention comprises the steps: that earlier be 4-5 with alkali metal hydroxide with the pH regulator of Grignard reaction wastewater; Adding carbonate adjusting pH then is 8-12; Filter collection precipitation.
The alkali metal hydroxide that the present invention adopts can be sodium hydroxide, potassium hydroxide, also can be other alkali metal oxyhydroxide, still, consider from the angle of economy, and be preferred with sodium hydroxide.Used alkali metal hydroxide can be that solid also can be the aqueous solution.
The carbonate that the present invention adopts is can yellow soda ash, salt of wormwood etc., considers with yellow soda ash to be preferred from the angle of economy.Used carbonate can be that solid also can the aqueous solution, is preferred with the solid.
During with the pH of carbonate regulation system, be adjustable as pH 8-12, be preferably pH9-10.
The magnesium basic carbonate that the inventive method processing Grignard reaction wastewater generates is water-soluble hardly, precipitates very easy and water sepn, and filter operation is simple.Can further wash behind the sedimentation and filtration and drying.
Magnesium basic carbonate has purposes widely, can be used for the preparation of magnesium salts, rubber, medicine, insulating material, dentistry preparation, high glass, especially in recent years be used to industrial sectors such as flour, food, makeup as additive and modifying agent, had effect preferably.
Method technology of the present invention is simple, easy and simple to handle, used reagent (commercially available product is all arranged) cheap and easy to get, and the rate of recovery height of magnesium salts, and cost recovery is cheap, therefore has very big industrial applicibility.
Embodiment
The present invention is further elaborated below by embodiment, and embodiment is for understanding the unrestricted claim scope of invention.
Embodiment one:
Get the 1000g Grignard reaction wastewater, adding 30% aqueous sodium hydroxide solution 82g regulation system pH is 4, and then adding solid sodium carbonate 120.0g, regulation system pH is 9, stir 30 minutes after-filtration, filter cake obtains white solid with 200ml water washing twice, 80 ℃ of following normal pressure oven dry get white powder solid magnesium basic carbonate 129g.
Embodiment two:
Get the 1000g Grignard reaction wastewater, adding 30% potassium hydroxide aqueous solution 115g regulation system pH is 5, and then adding solid carbonic acid potassium 156.2g, regulation system pH is 10, stir 30 minutes after-filtration, filter cake obtains white solid with 200ml water washing twice, 80 ℃ of following normal pressure oven dry get white powder solid magnesium basic carbonate 130g.
Claims (10)
1. method that reclaims magnesium salts from Gram-waste water comprises the steps: that earlier be 4-5 with alkali metal hydroxide with the pH regulator of Grignard reaction wastewater; Adding carbonate adjusting pH then is 8-12; Filter collection precipitation.
2. the method for claim 1, wherein said alkali metal hydroxide is selected from sodium hydroxide and potassium hydroxide.
3. method as claimed in claim 2, wherein said alkali metal hydroxide are sodium hydroxide.
4. the method for claim 1, wherein said alkali metal hydroxide is the aqueous solution.
5. the method for claim 1, wherein said carbonate is selected from yellow soda ash and salt of wormwood.
6. method as claimed in claim 5, wherein said carbonate are yellow soda ash.
7. the method for claim 1, wherein said carbonate is solid.
8. the method for claim 1, the pH that wherein said carbonate is regulated is 9-10.
9. the method for claim 1, the wherein said magnesium basic carbonate that is precipitated as.
10. the method for claim 1 further comprises precipitation washing and dry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN200810042398A CN101665258A (en) | 2008-09-03 | 2008-09-03 | Process for recovering magnesium salts from Grignard reaction wastewater |
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| Application Number | Priority Date | Filing Date | Title |
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| CN200810042398A CN101665258A (en) | 2008-09-03 | 2008-09-03 | Process for recovering magnesium salts from Grignard reaction wastewater |
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| CN101665258A true CN101665258A (en) | 2010-03-10 |
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| CN200810042398A Pending CN101665258A (en) | 2008-09-03 | 2008-09-03 | Process for recovering magnesium salts from Grignard reaction wastewater |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013020717A1 (en) * | 2011-08-08 | 2013-02-14 | Basf Se | Method for producing ultrapure magnesium hydroxide and magnesium oxide |
| CN109399674A (en) * | 2018-10-24 | 2019-03-01 | 国家海洋局天津海水淡化与综合利用研究所 | A method of extracting bromine magnesium compound from Grignard reaction wastewater and mother liquor |
| CN109761326A (en) * | 2019-03-13 | 2019-05-17 | 联化科技(盐城)有限公司 | Processing method without aluminum ions waste water |
| CN109790043A (en) * | 2016-09-12 | 2019-05-21 | 丹石产业株式会社 | Synthesize hydromagnesite particle and preparation method thereof |
| CN111689506A (en) * | 2020-07-21 | 2020-09-22 | 河南华龙香料有限公司 | Method for recovering magnesium chloride and tetrahydrofuran from Grignard reaction wastewater |
| CN112551772A (en) * | 2020-11-24 | 2021-03-26 | 衢州学院 | Resource treatment method for Grignard reaction wastewater |
| CN112573550A (en) * | 2020-11-24 | 2021-03-30 | 衢州学院 | Method for preparing magnesium-based flame retardant by utilizing Grignard wastewater |
-
2008
- 2008-09-03 CN CN200810042398A patent/CN101665258A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013020717A1 (en) * | 2011-08-08 | 2013-02-14 | Basf Se | Method for producing ultrapure magnesium hydroxide and magnesium oxide |
| CN109790043A (en) * | 2016-09-12 | 2019-05-21 | 丹石产业株式会社 | Synthesize hydromagnesite particle and preparation method thereof |
| CN109399674A (en) * | 2018-10-24 | 2019-03-01 | 国家海洋局天津海水淡化与综合利用研究所 | A method of extracting bromine magnesium compound from Grignard reaction wastewater and mother liquor |
| CN109761326A (en) * | 2019-03-13 | 2019-05-17 | 联化科技(盐城)有限公司 | Processing method without aluminum ions waste water |
| CN111689506A (en) * | 2020-07-21 | 2020-09-22 | 河南华龙香料有限公司 | Method for recovering magnesium chloride and tetrahydrofuran from Grignard reaction wastewater |
| CN112551772A (en) * | 2020-11-24 | 2021-03-26 | 衢州学院 | Resource treatment method for Grignard reaction wastewater |
| CN112573550A (en) * | 2020-11-24 | 2021-03-30 | 衢州学院 | Method for preparing magnesium-based flame retardant by utilizing Grignard wastewater |
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Open date: 20100310 |