CN103059055A - Method for preparing methyl silicate and aluminum fluoride from silicon tetrafluoride and methanol - Google Patents
Method for preparing methyl silicate and aluminum fluoride from silicon tetrafluoride and methanol Download PDFInfo
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- CN103059055A CN103059055A CN2012104273719A CN201210427371A CN103059055A CN 103059055 A CN103059055 A CN 103059055A CN 2012104273719 A CN2012104273719 A CN 2012104273719A CN 201210427371 A CN201210427371 A CN 201210427371A CN 103059055 A CN103059055 A CN 103059055A
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- silicon tetrafluoride
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- methyl silicate
- aluminum 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 aluminum fluoride from silicon tetrafluoride and methanol, which comprises the following steps of: a, adding a prepared alcohol solution of silicon tetrafluoride and aluminum powder to a synthesis reactor; b, raising the temperature of the reactor to a predetermined temperature reaction; c, after the reaction is finished, carrying out vacuum filtration on a product to separate solid and liquid; d, cleaning the solid obtained in the step c by methanol and drying to obtain a target product, namely anhydrous aluminum fluoride; and e, carrying out distillation on the filtrate obtained in the step c to remove methanol and obtaining methyl silicate with a high boiling point. The method for preparing methyl silicate and aluminum fluoride by silicon tetrafluoride and methanol related by the invention can efficiently and comprehensively utilize fluorine and silicon resources in by-products of phosphate fertilizer enterprises.
Description
Technical field
The present invention relates to chemical technology field, particularly a kind of silicon tetrafluoride gas of utilizing is carried out the method that alcoholysis prepares methyl silicate and Anhydrous Aluminium Chloride, the method that especially fluorine, silicon resource high-level efficiency and high benefit in the phosphatic fertilizer company by product is fully utilized.
Background technology
Methyl silicate occurs mainly as the organic synthesis intermediate raw material, and the past is less as circulation of commodities, and this is with its downstream industry scale is less relevant before this.In recent years, along with the industrial development methyl silicate is being produced coating heat-resisting, the chemically-resistant effect, organic silicon solvent and precision casting launch gradually with the industrialized developing of the aspects such as insulating material, opticglass treatment agent and condensing agent of tackiness agent and electronic industry, and the future market prospect is very wide.
Aluminum fluoride is a kind of meticulous derived product of fluorine chemical industry, also is a kind of important Inorganic Chemicals, and at present about 95% aluminum fluoride is for aluminum electrolysis industry in the world, be must use in the Aluminum Electrolysis Production in order to reduce Al
2O
3One of fusing assistant of fusing point and raising electrolyte conductivity, the aluminum fluoride composition that sodium aluminum fluoride melting liquid consumes when being used for replenishing electrolysis; Partially fluorinated aluminium is used as the outer muffle painting of pottery and the fusing assistant of vitreous enamel, flux, the soldering fluid in the metal solder and catalyzer industry that non-ferrous metal is smelted.
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 the low and poor shortcoming of environmental benefit of economic benefit fails to accomplish SiF
4High benefit comprehensive utilization.Therefore extremely be necessary to look for new approach, strengthen the by product SiF to phosphoric acid by wet process and production of phosphate fertilizer
4Effectively utilize, one of approach is to produce Anhydrous Aluminium Chloride and the methyl silicate of high added value by the method for this patent.
Summary of the invention
The object of the invention is to overcome and existing silicon tetrafluoride is utilized irrational technological deficiency, provide a kind of phosphatic fertilizer company by product silicon tetrafluoride that utilizes to carry out methyl silicate and aluminium fluoride product that alcoholysis prepares high added value, 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.
The method that silicon tetrafluoride alcoholysis of the present invention prepares methyl silicate and Anhydrous Aluminium Chloride comprises that following several step: a. joins silicon tetrafluoride alcoholic solution and the metallic aluminium powder that configures in the synthesis reactor; B. the temperature with reactor is increased to the preset temperature reaction; C. react complete after, product filters solid-liquid is separated; D. the solid that step c is obtained with methyl alcohol clean, drying obtains the target product Anhydrous Aluminium Chloride; E. the filtrate that step c is obtained is carried out distillation for removing methanol, obtains high boiling methyl silicate.
Among the step a, alcohol is methyl alcohol, and the alcoholic solution concentration of silicon tetrafluoride is 10%-30%, and the granularity of the metallic aluminium powder of adding is the 6-270 micron.
Among the step b, temperature of reaction is 20-70 ℃, and the reaction times is 1-12h.
Among the step e, the temperature of distillation is 40-70 ℃, and distillation pressure is 0.3-1 bar.
Principle of the present invention is described and illustrates according to following equation:
Novelty of the present invention is to adopt simple single stage method to prepare the product of two kinds of high added values---methyl silicate and Anhydrous Aluminium Chloride, and step is simple, and economical rationality has high environmental value and economic worth.
Environmental value of the present invention is that silicon tetrafluoride and aluminium powder can react completely, and remaining alcohol can recycle, and 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.
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 alcoholysis of the present invention prepares methyl silicate and aluminum fluoride will be described in detail in following embodiment, but be not limited to embodiment.
Embodiment 1
Be that the aluminium powder 50g that 10% silicon tetrafluoride methanol solution 1040 g and granularity are 75 microns joins in the synthesis reactor with massfraction, temperature is elevated to 30 ℃ gradually after, reaction 6h.React complete after, product is carried out vacuum filtration, suction filtration obtains solid and filtrate.Solid is washed with anhydrous methanol, obtain the target product Anhydrous Aluminium Chloride.Unnecessary methyl alcohol is removed in the filtrate distillation, obtained high boiling methyl silicate.
Embodiment 2
Be that the aluminium powder 50g that 24% silicon tetrafluoride methanol solution 434 g and granularity are 13 microns joins in the synthesis reactor with massfraction, temperature is elevated to 30 ℃ gradually after, react 1 h.React complete after, product is carried out vacuum filtration, suction filtration obtains solid and filtrate.Solid is washed with anhydrous methanol, obtain the target product Anhydrous Aluminium Chloride.Unnecessary methyl alcohol is removed in the filtrate distillation, obtained high boiling methyl silicate.
Embodiment 3
Be that the aluminium powder 50g that 14% silicon tetrafluoride methanol solution 743 g and granularity are 75 microns joins in the synthesis reactor with massfraction, temperature is elevated to 30 ℃ gradually after, reaction 6h.React complete after, product is carried out vacuum filtration, suction filtration obtains solid and filtrate.Solid is washed with anhydrous methanol, obtain the target product Anhydrous Aluminium Chloride.Unnecessary methyl alcohol is removed in the filtrate distillation, obtained high boiling methyl silicate.
Embodiment 4
Be that 14% silicon tetrafluoride methanol solution 743 g and granularity are that 270 microns aluminium powder 50g join in the synthesis reactor with massfraction, temperature is elevated to 60 ℃ gradually after, reaction 6h.React complete after, product is carried out vacuum filtration, suction filtration obtains solid and filtrate.Solid is washed with anhydrous methanol, obtain the target product Anhydrous Aluminium Chloride.Unnecessary methyl alcohol is removed in the filtrate distillation, obtained high boiling methyl silicate.
Embodiment 5
Be that aluminium powder 50 g that 14% silicon tetrafluoride methanol solution 743 g and granularity are 5 microns join in the synthesis reactor with massfraction, temperature is elevated to 60 ℃ gradually after, reaction 10h.React complete after, product is carried out vacuum filtration, suction filtration obtains solid and filtrate.Solid is washed with anhydrous methanol, obtain the target product Anhydrous Aluminium Chloride.Unnecessary methyl alcohol is removed in the filtrate distillation, obtained high boiling methyl silicate.
Embodiment 6
Be that 30% silicon tetrafluoride methanol solution 367 g join in the synthesis reactor with massfraction, temperature is elevated to 60 ℃ gradually after, in 6 hours, add granularity in batches and be 10 microns aluminium powder 50 g, reaction 12h.React complete after, product is carried out vacuum filtration, suction filtration obtains solid and filtrate.Solid is washed with anhydrous methanol, obtain the target product Anhydrous Aluminium Chloride.Unnecessary methyl alcohol is removed in the filtrate distillation, obtained high boiling methyl silicate.
Embodiment 7
Be that 100 microns aluminium powder 50g aluminium powder and 300mL methyl alcohol joins in the synthesis reactor with granularity, temperature is elevated to 60 ℃ gradually after, in 6 hours, add massfraction in batches and be 14% silicon tetrafluoride methanol solution 743 g, reaction 12h.React complete after, product is carried out vacuum filtration, suction filtration obtains solid and filtrate.Solid is washed with anhydrous methanol, obtain the target product Anhydrous Aluminium Chloride.Unnecessary methyl alcohol is removed in the filtrate distillation, obtained high boiling methyl silicate.
Embodiment 8
Be that aluminium powder 50 g that 20% silicon tetrafluoride methanol solution 616g and granularity are 150 microns join in the synthesis reactor with massfraction, temperature is elevated to 60 ℃ gradually after, react 12 h.React complete after, product is carried out vacuum filtration, suction filtration obtains solid and filtrate.Solid is washed with anhydrous methanol, obtain the target product Anhydrous Aluminium Chloride.Unnecessary methyl alcohol is removed in the filtrate distillation, obtained high boiling methyl silicate.
Embodiment 9
Be that the aluminium powder 50 g aluminium powders that 20% silicon tetrafluoride methanol solution 616 g and granularity are 200 microns join in the synthesis reactor with massfraction, temperature is elevated to 60 ℃ gradually after, reaction 12h.React complete after, product is carried out vacuum filtration, suction filtration obtains solid and filtrate.Solid is washed with anhydrous methanol, obtain the target product Anhydrous Aluminium Chloride.Unnecessary methyl alcohol is removed in the filtrate distillation, obtained high boiling methyl silicate.
Claims (5)
1. a silicon tetrafluoride, methyl alcohol and metallic aluminium powder prepare the method for methyl silicate and aluminum fluoride, it is characterized in that step is:
A. silicon tetrafluoride methanol solution and the metallic aluminium powder that configures joined in the synthesis reactor;
B. the temperature with reactor rises to predetermined temperature of reaction;
C. react complete after, product carries out solid-liquid separation;
D. the solid that step c is obtained with methyl alcohol wash, to obtain target product be Anhydrous Aluminium Chloride to drying;
E. the filtrate that step c is obtained is carried out distillation for removing methanol, obtains high boiling methyl silicate.
2. by method claimed in claim 1, it is characterized in that the silicon tetrafluoride concentration in the step a silicon tetrafluoride methanol solution is 10%-30%.
3. by method claimed in claim 1, it is characterized in that adding the metallic aluminium powder granularity among the step a is the 6-270 micron.
4. by method claimed in claim 1, it is characterized in that among the step b, predetermined temperature of reaction is 20-70 ℃, the reaction times is 1-12h.
5. by method claimed in claim 1, it is characterized in that among the step e, the temperature of distillation is 40-70 ℃, distillation pressure is 0.3-1 bar.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210427371.9A CN103059055B (en) | 2012-11-01 | 2012-11-01 | A kind of silicon tetrafluoride, methyl alcohol and aluminum are for the method for methyl silicate and aluminum fluoride |
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| CN201210427371.9A CN103059055B (en) | 2012-11-01 | 2012-11-01 | A kind of silicon tetrafluoride, methyl alcohol and aluminum are for the method for methyl silicate and aluminum fluoride |
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| CN103059055A true CN103059055A (en) | 2013-04-24 |
| CN103059055B CN103059055B (en) | 2016-03-16 |
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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 CN201210427371.9A patent/CN103059055B/en active Active
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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