CN103130487A - Recovery processing method of Grignard reaction wastewater - Google Patents
Recovery processing method of Grignard reaction wastewater Download PDFInfo
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- CN103130487A CN103130487A CN2011103959581A CN201110395958A CN103130487A CN 103130487 A CN103130487 A CN 103130487A CN 2011103959581 A CN2011103959581 A CN 2011103959581A CN 201110395958 A CN201110395958 A CN 201110395958A CN 103130487 A CN103130487 A CN 103130487A
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Abstract
The invention belongs to the technical field of chemical synthesis, in particular to a recovery processing method of Grignard reaction wastewater. According to the recovery processing method, the Grignard reaction wastewater is directly added in production technology of magnesium cement fire prevention boards and magnesite composite material manhole covers so that magnesium chloride and magnesium sulfate in the Grignard reaction wastewater can be fully recycled, and therefore production cost of the magnesium cement fire prevention boards and the magnesite composite material manhole covers is reduced, the Grignard reaction wastewater is recycled, and resource waste and environment pollution are avoided.
Description
Technical field:
The invention belongs to technical field of chemical synthesis, be specifically related to a kind of recovery and treatment method of Grignard reaction wastewater.
Background technology:
The Grignard reagents such as vinylchlorid, chloroparaffin, chlorinated aromatic hydrocarbons are widely used in Chemical Manufacture, but the waste water of a large amount of magnesium chloride containings that produce after its hydrolysis, sal epsom is difficult to process.Often adopt the mode of evaporative crystallization therefrom first to isolate sal epsom in production, and the final concentrated magnesium chloride that obtains, but this treatment process investment is large, complex process, energy consumption are large, equipment corrosion is serious.In view of one of important source material of producing magnesium cement fireproof board and magnesite combined manhole cover is exactly magnesium chloride, sal epsom, and in the waste water that grignard reaction produces, the mass ratio of magnesium chloride, sal epsom just meets the ratio requirement of these two kinds of products, therefore, Grignard reaction wastewater being recycled production magnesium cement fireproof board and magnesite combined manhole cover is the most simple and effective the most direct recoverying and utilizing method.
Summary of the invention:
Purpose of the present invention is exactly the deficiency for prior art, and provide a kind of recovery and treatment method of Grignard reaction wastewater, Grignard reaction wastewater is directly joined in the production technique of magnesium cement fireproof board and manhole cover made of magnesite composite material, make magnesium chloride, sal epsom in Grignard reaction wastewater fully recycle, both reduced the production cost of magnesium cement fireproof board and magnesite combined manhole cover material, recycle again Grignard reaction wastewater, avoided the wasting of resources and environmental pollution.
Technology solution of the present invention is as follows:
Get the grignard reaction factory effluent, general containing magnesium sulfate 20～30%, magnesium chloride containing 20～30%, after stripping reclaims wherein minute quantity solvent with it as raw material production magnesium cement fireproof board and magnesite combined manhole cover.
A kind of recovery and treatment method of Grignard reaction wastewater, it is characterized in that: with Grignard reaction wastewater for the production of in magnesium cement fireproof board technique, its raw material proportioning by weight is: Grignard reaction wastewater 20-200 part, phosphoric acid 0.1-5 part, light calcined magnesia 10-300 part, perlite 1-30 part, light filler 1-30 part, heavy stopping composition 10-300 part, 2 parts of fibrous mesh cloths.
Further, described heavy stopping composition be water-ground limestone, ground dolomite, quartz sand, talcous one or more, light filler is one or more of sawdust, wheat bran, straw bits.
The method of producing magnesium cement fireproof board is: take weight as unit, take grignard reaction waste water and the phosphoric acid of formula ratio, pour in stirrer, add appropriate water and stir, the degree Beaume of regulating waste water is 27, adds light calcined magnesia, perlite, light filler, the heavy stopping composition of formula ratio, stir 15min, then blowing, carry out moulding on the PLASTIC LAMINATED production line with double-deck 2 fibrous mesh cloths, can carry out the demoulding, cutting after it reaches some strength.
A kind of recovery and treatment method of Grignard reaction wastewater is characterized in that: for the production of in magnesite combined manhole cover technique, its raw material proportioning by weight is: Grignard reaction wastewater 50～200 with Grignard reaction wastewater, magnesium oxide 100, silica 1 00, phosphoric acid 0.5-3.0, Tai-Ace S 150 1-6, sulfuric acid 2-8, organosilicon crylic acid latex 1-8, alum 2-5.0, black alum 1.5-4.5, water-resisting agent 5-15, steel fiber 1-6.
the method of producing the magnesite combined manhole cover is: take weight as unit, take the Grignard reaction wastewater of formula ratio, regulating degree Beaume is 27, then mix with magnesium oxide, pour in stirrer, add successively again the silicon-dioxide of formula ratio, phosphoric acid, Tai-Ace S 150, sulfuric acid, organosilicon crylic acid latex, alum, black alum, water-resisting agent and steel fiber, add again entry 10-50kg, temperature is controlled at 20-40 ℃, stir 15min, then be cast on the mould that the surface was coated with releasing agent, solidification value 25-30 ℃, demould time is greater than 16h, be positioned over temperature and be 50-80 ℃ after nonventilated indoor 9 days, it is the highest that intensity reaches.
Beneficial effect of the present invention is:
The present invention takes full advantage of the brine waste that produces in Chemical Manufacture with its resource utilization, has namely solved the disposal difficulties of chemical production wastewater, again decrease the production cost of magnesium cement fireproof board and manhole cover made of magnesite composite material, reach the effect of achieving many things at one stroke.
Embodiment:
Embodiment:
Get the grignard reaction factory effluent, general containing magnesium sulfate 20～30%, magnesium chloride containing 20～30%, after stripping reclaims wherein minute quantity solvent with it as raw material production magnesium cement fireproof board and magnesite combined manhole cover.
For the production of in magnesium cement fireproof board technique, its raw material proportioning by weight is with Grignard reaction wastewater: Grignard reaction wastewater 20-200 part, phosphoric acid 0.1-5 part, light calcined magnesia 10-300 part, perlite 1-30 part, light filler 1-30 part, heavy stopping composition 10-300 part, 2 parts of fibrous mesh cloths.The method of producing magnesium cement fireproof board is: take weight as unit, take grignard reaction waste water and the phosphoric acid of formula ratio, pour in stirrer, add appropriate water and stir, the degree Beaume of regulating waste water is 27, adds light calcined magnesia, perlite, light filler, the heavy stopping composition of formula ratio, stir 15min, then blowing, carry out moulding on the PLASTIC LAMINATED production line with double-deck 2 fibrous mesh cloths, can carry out the demoulding, cutting after it reaches some strength.Described heavy stopping composition be water-ground limestone, ground dolomite, quartz sand, talcous one or more, light filler is one or more of sawdust, wheat bran, straw bits.
With Grignard reaction wastewater for the production of in magnesite combined manhole cover technique, its raw material proportioning by weight is: Grignard reaction wastewater 50～200, magnesium oxide 100, silica 1 00, phosphoric acid 0.5-3.0, Tai-Ace S 150 1-6, sulfuric acid 2-8, organosilicon crylic acid latex 1-8, alum 2-5.0, black alum 1.5-4.5, water-resisting agent 5-15, steel fiber 1-6.
the method of producing the magnesite combined manhole cover is: take weight as unit, take the Grignard reaction wastewater of formula ratio, regulating degree Beaume is 27, then mix with magnesium oxide, pour in stirrer, add successively again the silicon-dioxide of formula ratio, phosphoric acid, Tai-Ace S 150, sulfuric acid, organosilicon crylic acid latex, alum, black alum, water-resisting agent and steel fiber, add again entry 10-50kg, temperature is controlled at 20-40 ℃, stir 15min, then be cast on the mould that the surface was coated with releasing agent, solidification value 25-30 ℃, demould time is greater than 16h, be positioned over temperature and be 50-80 ℃ after nonventilated indoor 9 days, it is the highest that intensity reaches.
Claims (5)
1. the recovery and treatment method of a Grignard reaction wastewater, it is characterized in that: with Grignard reaction wastewater for the production of in magnesium cement fireproof board technique, its raw material proportioning by weight is: Grignard reaction wastewater 20-200 part, phosphoric acid 0.1-5 part, light calcined magnesia 10-300 part, perlite 1-30 part, light filler 1-30 part, heavy stopping composition 10-300 part, 2 parts of fibrous mesh cloths.
2. the recovery and treatment method of a kind of Grignard reaction wastewater according to claim 1, it is characterized in that: the heavy stopping composition be water-ground limestone, ground dolomite, quartz sand, talcous one or more, light filler is one or more of sawdust, wheat bran, straw bits.
3. the recovery and treatment method of a kind of Grignard reaction wastewater according to claim 1, it is characterized in that: the method for Grignard reaction wastewater being produced magnesium cement fireproof board is: take weight as unit, take grignard reaction waste water and the phosphoric acid of formula ratio, pour in stirrer, adding appropriate water stirs, the degree Beaume of regulating waste water is 27, the light calcined magnesia that adds formula ratio, perlite, light filler, the heavy stopping composition, stir 15min, then blowing, carry out moulding on the PLASTIC LAMINATED production line with double-deck 2 fibrous mesh cloths, after reaching some strength, it can carry out the demoulding, cutting.
4. the recovery and treatment method of a Grignard reaction wastewater, it is characterized in that: for the production of in magnesite combined manhole cover technique, its raw material proportioning by weight is: Grignard reaction wastewater 50～200 with Grignard reaction wastewater, magnesium oxide 100, silica 1 00, phosphoric acid 0.5-3.0, Tai-Ace S 150 1-6, sulfuric acid 2-8, organosilicon crylic acid latex 1-8, alum 2-5.0, black alum 1.5-4.5, water-resisting agent 5-15, steel fiber 1-6.
5. the recovery and treatment method of a kind of Grignard reaction wastewater according to claim 4, it is characterized in that: the method for Grignard reaction wastewater being produced the magnesite combined manhole cover is: take weight as unit, take the Grignard reaction wastewater of formula ratio, regulating degree Beaume is 27, then mix with magnesium oxide, pour in stirrer, add successively again the silicon-dioxide of formula ratio, phosphoric acid, Tai-Ace S 150, sulfuric acid, organosilicon crylic acid latex, alum, black alum, water-resisting agent and steel fiber, add again entry 10-50kg, temperature is controlled at 20-40 ℃, stir 15min, then be cast on the mould that the surface was coated with releasing agent, solidification value 25-30 ℃, demould time is greater than 16h, be positioned over temperature and be 50-80 ℃ after nonventilated indoor 9 days, it is the highest that intensity reaches.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011103959581A CN103130487A (en) | 2011-11-26 | 2011-11-26 | Recovery processing method of Grignard reaction wastewater |
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| CN2011103959581A CN103130487A (en) | 2011-11-26 | 2011-11-26 | Recovery processing method of Grignard reaction wastewater |
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| CN103130487A true CN103130487A (en) | 2013-06-05 |
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| CN2011103959581A Pending CN103130487A (en) | 2011-11-26 | 2011-11-26 | Recovery processing method of Grignard reaction wastewater |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104829162A (en) * | 2015-05-29 | 2015-08-12 | 盐城工学院 | Magnesium oxychloride cement modifier and preparation method and application thereof |
| CN106745112A (en) * | 2016-12-15 | 2017-05-31 | 河南豫辰药业股份有限公司 | The preparation method of Magnesium dichloride hexahydrate is reclaimed in a kind of waste residue hydrolyzate from grignard |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3565579A (en) * | 1968-11-18 | 1971-02-23 | Nalco Chemical Co | Recovery of magnesium chloride dihydrate |
| US3594120A (en) * | 1968-12-23 | 1971-07-20 | Nalco Chemical Co | Anhydrous magnesium chloride |
| CN1648065A (en) * | 2004-12-23 | 2005-08-03 | 浙江大学 | Recovering process for Gram-waste water |
| CN101386517A (en) * | 2008-10-27 | 2009-03-18 | 陈小石 | Foaming magnesite compound material and processing method thereof |
| CN101638991A (en) * | 2009-08-28 | 2010-02-03 | 长沙威特消防新材料科技有限公司 | High-tenacity waterproof and fireproof board specially used for tunnel and preparation method thereof |
| CN102190477A (en) * | 2010-03-10 | 2011-09-21 | 吴长峰 | Composite modified magnesite concrete formula |
-
2011
- 2011-11-26 CN CN2011103959581A patent/CN103130487A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3565579A (en) * | 1968-11-18 | 1971-02-23 | Nalco Chemical Co | Recovery of magnesium chloride dihydrate |
| US3594120A (en) * | 1968-12-23 | 1971-07-20 | Nalco Chemical Co | Anhydrous magnesium chloride |
| CN1648065A (en) * | 2004-12-23 | 2005-08-03 | 浙江大学 | Recovering process for Gram-waste water |
| CN101386517A (en) * | 2008-10-27 | 2009-03-18 | 陈小石 | Foaming magnesite compound material and processing method thereof |
| CN101638991A (en) * | 2009-08-28 | 2010-02-03 | 长沙威特消防新材料科技有限公司 | High-tenacity waterproof and fireproof board specially used for tunnel and preparation method thereof |
| CN102190477A (en) * | 2010-03-10 | 2011-09-21 | 吴长峰 | Composite modified magnesite concrete formula |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104829162A (en) * | 2015-05-29 | 2015-08-12 | 盐城工学院 | Magnesium oxychloride cement modifier and preparation method and application thereof |
| CN106745112A (en) * | 2016-12-15 | 2017-05-31 | 河南豫辰药业股份有限公司 | The preparation method of Magnesium dichloride hexahydrate is reclaimed in a kind of waste residue hydrolyzate from grignard |
| CN106745112B (en) * | 2016-12-15 | 2018-04-06 | 河南豫辰药业股份有限公司 | The preparation method of Magnesium dichloride hexahydrate is reclaimed in a kind of waste residue hydrolyzate from grignard |
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Application publication date: 20130605 |