CN103059056A - Method for preparing methyl silicate and magnesium fluoride from silicon tetrafluoride, methanol and magnesium - Google Patents
Method for preparing methyl silicate and magnesium fluoride from silicon tetrafluoride, methanol and magnesium Download PDFInfo
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- CN103059056A CN103059056A CN2012104274020A CN201210427402A CN103059056A CN 103059056 A CN103059056 A CN 103059056A CN 2012104274020 A CN2012104274020 A CN 2012104274020A CN 201210427402 A CN201210427402 A CN 201210427402A CN 103059056 A CN103059056 A CN 103059056A
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- magnesium
- silicon tetrafluoride
- methanol
- methyl alcohol
- magnesium fluoride
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Abstract
The invention relates to the technical field of chemical industry and in particular relates to a method for preparing methyl silicate and magnesium fluoride by utilizing reactions of silicon tetrafluoride, methanol and magnesium. The method comprises the following steps of: a. adding methanol and magnesium powder to a reaction kettle; b. raising the temperature of the reaction system to a preset temperature to react; c. after reaction is completed, cooling the reaction system, adding prepared methanol solution of silicon tetrafluoride to the reaction kettle until the reaction system is neutral; d. separating solid from liquid through filtration; e. washing the solid obtained in step d with methanol and drying the washed solid to obtain the target product magnesium fluoride; and f. distilling the filtrate obtained in step d to remove methanol, thus obtaining methyl silicate with high boiling point. The method can be used for producing by-product silicon tetrafluoride by efficiently utilizing phosphate fertilizers.
Description
Technical field
The present invention relates to chemical technology field, particularly a kind of method of utilizing silicon tetrafluoride gas, methyl alcohol and magnesium powder to produce methyl silicate and magnesium fluoride is especially to the method for fluorine, the comprehensive utilization of silicon resource high benefit in the phosphatic fertilizer company by product.
Background technology
Methyl silicate is colourless transparent liquid for special odor, deliquescent outward appearance are arranged, and GR is arranged at present, CP, the packing of all sizes such as AR.The methyl silicate ester occurs mainly as the intermediate raw material of the derived product such as synthesizing silane coupler, and the past is less as circulation of commodities, and this is with its downstream industry scale is less relevant before this.Through development for many years, the industrialized developing of the aspects such as methyl silicate derived product silane coupling agent, silicone resin, coating, nano material and even polysilicon launches gradually, and the future market prospect is very wide.
Magnesium fluoride is colourless crystallization or white powder.Lattice of rutile type, little have a purple fluorescence, and atomic water-soluble (18 ℃, 87 mg/L) are slightly soluble in diluted acid (particularly nitric acid).Magnesium fluoride is a kind of meticulous derived product of fluorine chemical industry, it also is a kind of important Inorganic Chemicals, can be used as the raw material of producing special cermacis, glass, hot pressing crystal, fusing assistant as smelting magnesium and magnesium, in the welding as welding compound, as the agent that is being coated with of pigment, also can be used for preparing the precise parts such as fluorescent material in various eyeglasses in the opticinstrument and filter coating, the negative ray screen.Along with the development of science and technology, in recent years ultraviolet and infrared research day by day to be goed deep into, its application is more and more wider, and the application demand to magnesium fluoride on the market will progressively increase.
SiF
4It is the by product of phosphoric acid by wet process and production of phosphate fertilizer.At present, the SiF of China's phosphate fertilizer industry by-product
4All be that the form with silicofluoric acid reclaimed after water absorbed, and to produce the Sodium Silicofluoride byproduct as main, because manufacturer is numerous, supply exceed demand for product, Business Economic Benefit is low, part small business even abandoned the recovery of silicofluoric acid so not only causes valuable fluorine, the loss of silicon resource, simultaneously also havoc and contaminate environment.To the fluorine of by product, traditional technology and the product specification of silicon resource comprehensive utilization, no matter adopt which kind of operational path with regard to China's phosphate fertilizer industry, all exist added value of product low, range of product is few, and economic benefit is hanged down and the poor shortcoming of environmental benefit.The phosphate fertilizer industry utilizes method to fail to accomplish the high benefit comprehensive utilization to the tradition of fluorine, silicon resource in the by product.
Summary of the invention
The object of the invention is to overcome and existing silicon tetrafluoride is utilized irrational technological deficiency, a kind of methyl silicate and magnesium fluoride that utilizes phosphatic fertilizer company by product silicon tetrafluoride to prepare high added value with the reaction of magnesium powder in methyl alcohol is provided, and can not produce the waste of reluctant environmental pollution in the process, can utilize efficiently a kind of method of production of phosphate fertilizer by product silicon tetrafluoride.
Silicon tetrafluoride of the present invention reacts the method for preparing methyl silicate and magnesium fluoride with the magnesium powder and comprises that following several step: a. joins methyl alcohol and magnesium powder in the reactor in methyl alcohol; B. the temperature with reaction system is increased to the preset temperature reaction; C. react complete after, cooling joins the methanol solution of the silicon tetrafluoride that configures in the reactor, until reaction system is neutral; D. filter solid-liquid is separated; E. the solid that steps d is obtained with methyl alcohol clean, drying obtains the target product magnesium fluoride; F. the filtrate that steps d is obtained is carried out distillation for removing methanol, obtains high boiling methyl silicate.
Among the step a, the granular size of magnesium powder is the 5-270 micron.
Among the step b, temperature of reaction is 18-65 ℃, and the reaction times is 1-4 h.
Among the step c, the methanol solution mass percent of silicon tetrafluoride is 10%-30%, and the neutralization reaction time is 0.5-4 h.
Among the step f, distillation pressure is 0.1-1 bar, and distillation temperature is 30-70 ℃.
Principle of the present invention is described and illustrates according to following equation:
Novelty of the present invention is to adopt brand-new chemical principle, can prepare with simple single stage method product---methyl silicate and the magnesium fluoride of two kinds of high added values, operational path is novel, step is simple, economical rationality, has high environmental value and economic worth.
Environmental value of the present invention is that silicon tetrafluoride can react completely, and remaining methyl alcohol can recycle, and discharges without waste, does not have environmental pollution.
Economic worth of the present invention has been to extend the industrial chain that phosphatic fertilizer company utilizes the fluorine silicon resource, and single stage method has obtained two kinds of high value-added products simultaneously, has accomplished the comprehensive high-efficiency utilization to the fluorine silicon resource.
The present invention is owing to being in water-less environment, can directly make to be equivalent to the high-quality anhydrous magnesium fluoride that dry process goes out.
New process of the present invention can adopt existing technology and realize through the unit equipment of large-scale industrial production checking.
Embodiment
The method that silicon tetrafluoride of the present invention, methyl alcohol and magnesium prepare methyl silicate and magnesium fluoride will be described in detail in following embodiment, but be not limited to embodiment.
Embodiment 1
The magnesium powder of 50 mL methyl alcohol and 38 microns sizes of 1.5 g is joined in the reactor, after stirring 3 h under the room temperature, be that 24% silicon tetrafluoride methanol solution 13.5 g join in the reactor with massfraction, until reaction system is neutral, behind stir about 0.5 h, reaction system is filtered, filter cake with methanol wash again drying obtain magnesium fluoride, washings and filtrate are incorporated in removes the complete methyl alcohol of unreacted under the reduced pressure, obtain methyl silicate.
Embodiment 2
The magnesium powder of 50 mL methyl alcohol and 38 microns sizes of 1.5 g is joined in the reactor, behind 40 ℃ of lower stirring 1.5 h, be that 10% silicon tetrafluoride methanol solution 32.4 g join in the reactor with massfraction, until reaction system is neutral, behind stir about 4 h, reaction system is filtered, filter cake with methanol wash again drying obtain magnesium fluoride, washings and filtrate are incorporated in removes the complete methyl alcohol of unreacted under the reduced pressure, obtain methyl silicate.
Embodiment 3
The magnesium powder of 50 mL methyl alcohol and 5 microns sizes of 1.5 g is joined in the reactor, behind 40 ℃ of lower stirring 1 h, be that 24% silicon tetrafluoride methanol solution 13.5 g join in the reactor with massfraction, until reaction system is neutral, behind stir about 0.5 h, reaction system is filtered, filter cake with methanol wash again drying obtain magnesium fluoride, washings and filtrate are incorporated in removes the complete methyl alcohol of unreacted under the reduced pressure, obtain methyl silicate.
Embodiment 4
The magnesium powder of 50 mL methyl alcohol and 5 microns sizes of 1.5 g is joined in the reactor, after stirring 2 h under the room temperature, be that 15% silicon tetrafluoride methanol solution 21.7 g join in the reactor with massfraction, until reaction system is neutral, behind stir about 0.5 h, reaction system is filtered, filter cake with methanol wash again drying obtain magnesium fluoride, washings and filtrate are incorporated in removes the complete methyl alcohol of unreacted under the reduced pressure, obtain methyl silicate.
Embodiment 5
The magnesium powder of 50 mL methyl alcohol and 18 microns sizes of 1.5 g is joined in the reactor, behind 65 ℃ of lower stirring 1 h, be that 30% silicon tetrafluoride methanol solution 10.9 g join in the reactor with massfraction, until reaction system is neutral, behind stir about 2 h, reaction system is filtered, filter cake with methanol wash again drying obtain magnesium fluoride, washings and filtrate are incorporated in removes the complete methyl alcohol of unreacted under the reduced pressure, obtain methyl silicate.
Embodiment 6
The magnesium powder of 50 mL methyl alcohol and 75 microns sizes of 1.5 g is joined in the reactor, after stirring 4 h under the room temperature, be that 15% silicon tetrafluoride methanol solution 21.7 g join in the reactor with massfraction, until reaction system is neutral, behind stir about 0.5 h, reaction system is filtered, filter cake with methanol wash again drying obtain magnesium fluoride, washings and filtrate are incorporated in removes the complete methyl alcohol of unreacted under the reduced pressure, obtain methyl silicate.
Embodiment 7
The magnesium powder of 50 mL methyl alcohol and 5 microns sizes of 1.5 g is joined in the reactor, behind 65 ℃ of lower stirring 0.5 h, be that silicon tetrafluoride methanol solution 13.5 g of 24 % join in the reactor with massfraction, until reaction system is neutral, behind stir about 0.5 h, reaction system is filtered, filter cake with methanol wash again drying obtain magnesium fluoride, washings and filtrate are incorporated in removes the complete methyl alcohol of unreacted under the reduced pressure, obtain methyl silicate.
Embodiment 8
The magnesium powder of 50 mL methyl alcohol and 5 microns sizes of 1.5 g is joined in the reactor, behind 65 ℃ of lower stirring 0.5 h, be that silicon tetrafluoride methanol solution 13.5 g of 24 % join in the reactor with massfraction, until reaction system is neutral, behind stir about 3 h, reaction system is filtered, filter cake with methanol wash again drying obtain magnesium fluoride, washings and filtrate are incorporated in removes the complete methyl alcohol of unreacted under the condition of normal pressure, obtain methyl silicate.
Claims (5)
1. a silicon tetrafluoride, methyl alcohol and magnesium prepare the method for methyl silicate and magnesium fluoride, it is characterized in that, step is:
A. methyl alcohol and magnesium powder are joined in the reactor;
B. the temperature with reaction system rises to predetermined temperature of reaction;
C. react complete after, the methanol solution of the silicon tetrafluoride that configures is joined in the reactor, until reaction system is neutral;
D. reaction product is carried out solid-liquid separation;
E. the solid that steps d is obtained with methyl alcohol clean, drying obtains the target product magnesium fluoride;
F. the filtrate that steps d is obtained is carried out distillation for removing methanol, obtains high boiling methyl silicate.
2. prepare the method for methyl silicate and magnesium fluoride by a kind of silicon tetrafluoride claimed in claim 1, methyl alcohol and magnesium, it is characterized in that, among the step a, the granular size of magnesium powder is the 5-270 micron.
3. prepare the method for methyl silicate and magnesium fluoride by a kind of silicon tetrafluoride claimed in claim 1, methyl alcohol and magnesium, it is characterized in that, among the step b, temperature of reaction is 18-65 ℃, and the reaction times is 1-4 h.
4. prepare the method for methyl silicate and magnesium fluoride by a kind of silicon tetrafluoride claimed in claim 1, methyl alcohol and magnesium, it is characterized in that, among the step c, the methanol solution mass percent of silicon tetrafluoride is 10%-30%, and the neutralization reaction time is 0.5-4 h.
5. prepare the method for methyl silicate and magnesium fluoride by a kind of silicon tetrafluoride claimed in claim 1, methyl alcohol and magnesium, it is characterized in that, among the step f, distillation pressure is 0.1-1 bar, and distillation temperature is 30-70 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210427402.0A CN103059056B (en) | 2012-11-01 | 2012-11-01 | A kind of silicon tetrafluoride, methyl alcohol and magnesium prepare the method for methyl silicate and magnesium fluoride |
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| CN201210427402.0A CN103059056B (en) | 2012-11-01 | 2012-11-01 | A kind of silicon tetrafluoride, methyl alcohol and magnesium prepare the method for methyl silicate and magnesium fluoride |
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| CN103059056A true CN103059056A (en) | 2013-04-24 |
| CN103059056B CN103059056B (en) | 2016-03-09 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB738703A (en) * | 1953-07-07 | 1955-10-19 | Kali Chemie Ag | Process for the production of esters or thioesters of inorganic acids |
| US3055927A (en) * | 1959-09-21 | 1962-09-25 | Ici Ltd | Preparation of organic orthosilicates from silicon tetrafluoride |
| CN101638415A (en) * | 2009-03-30 | 2010-02-03 | 云南省化工研究院 | Manufacturing method of silane and hydrogen fluoride |
| CN102400000A (en) * | 2011-11-30 | 2012-04-04 | 云南省化工研究院 | Method for preparing aluminium-silicon alloy and aluminium fluoride through reducing silicon tetrafluoride by utilizing aluminium |
| CN102516280A (en) * | 2011-12-08 | 2012-06-27 | 云南省化工研究院 | Method for preparing orthosilicic acid ester and fluoride through silicon tetrafluoride alcoholysis |
-
2012
- 2012-11-01 CN CN201210427402.0A patent/CN103059056B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB738703A (en) * | 1953-07-07 | 1955-10-19 | Kali Chemie Ag | Process for the production of esters or thioesters of inorganic acids |
| US3055927A (en) * | 1959-09-21 | 1962-09-25 | Ici Ltd | Preparation of organic orthosilicates from silicon tetrafluoride |
| CN101638415A (en) * | 2009-03-30 | 2010-02-03 | 云南省化工研究院 | Manufacturing method of silane and hydrogen fluoride |
| CN102400000A (en) * | 2011-11-30 | 2012-04-04 | 云南省化工研究院 | Method for preparing aluminium-silicon alloy and aluminium fluoride through reducing silicon tetrafluoride by utilizing aluminium |
| CN102516280A (en) * | 2011-12-08 | 2012-06-27 | 云南省化工研究院 | Method for preparing orthosilicic acid ester and fluoride through silicon tetrafluoride alcoholysis |
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