CN102180475A - Method for preparing boron fluoride and hydrochloric acid by using boron slurry washing liquor - Google Patents
Method for preparing boron fluoride and hydrochloric acid by using boron slurry washing liquor Download PDFInfo
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- CN102180475A CN102180475A CN 201010556435 CN201010556435A CN102180475A CN 102180475 A CN102180475 A CN 102180475A CN 201010556435 CN201010556435 CN 201010556435 CN 201010556435 A CN201010556435 A CN 201010556435A CN 102180475 A CN102180475 A CN 102180475A
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- boron
- hydrochloric acid
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- fluoride
- washing lotion
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Abstract
The invention discloses a method for preparing boron fluoride and hydrochloric acid by using boron slurry washing liquor and relates to the technical field of three wastes treatment and comprehensive utilization in inorganic chemical industry. The method comprises the steps of: reacting clarified boron slurry washing liquor with hydrochloric acid in a corrosion-resistant reactor while stirring to produce liquid boron chloride, wherein the mass ratio of boric acid in the boron slurry washing liquor to hydrochloric acid is 1:0.98-1.38 based on pure substances; reacting the liquid boron chloride with hydrogen fluoride in a closed fluorination reactor while stirring to produce boron trifluoride and hydrochloric acid mixture, and filtering to obtain hydrochloric acid aqueous solution and returning the hydrochloric acid aqueous solution for cyclic utilization, wherein the mass ratio of liquid boron chloride to hydrogen fluoride is 1:0.31-0.71 based on pure substances; and collecting the boron trifluoride gas and compressing into canned gas products. The method effectively utilizes substances separated from the boron slurry, and lays foundations for further carrying out boron slurry extraction and utilization smoothly, thus creating tremendous economic benefits.
Description
Technical field
The present invention relates to the technical field of the inorganic chemical industry disposal of three wastes and comprehensive utilization, particularly a kind of method for preparing boron fluoride and hydrochloric acid with boron mud washing lotion.
Background technology
Boron mud is with szaibelyite (2MgOB
2O
3H
2O) be raw material, by roasting, pulverizing, mix, take the carbon water law to produce borax (Na with soda ash
2B
4O
710H
2O), remaining solid waste after washing, crystallisation process extract borax.Produce one ton of borax and can produce 4 tons of boron mud, a borax plant that produces 8000 tons per year, can produce boron mud every year is 3.2 ten thousand tons.Because the quantity discharged of boron mud is bigger, the multiple comprehensive Utilization Ways of present domestic employing except that producing Magnesium Carbonate Light 41-45 and magnesium oxide and plastic and rubber filler, also has the coal of producing boron magnesium phosphorus composite fertilizer, making honeycomb briquette reinforced and do architectural borax etc.
Magnesium in the boron mud generally all is that the form with magnesiumcarbonate exists, and is sometimes also different and difference arranged along with the mineral products of szaibelyite.The component of producing the boron mud of Magnesium Carbonate Light 41-45 is such: magnesium oxide 38%, silicon-dioxide 20%, carbonic acid gas 17%, boron oxide 3%, calcium oxide 3%, manganese oxide 0.11%, other are moisture content.
Boron mud washing lotion be handle and processing boron mud before the inevitable step of carrying out, be to extract because of the characteristic that boron trioxide is dissolved in hot water.Otherwise it can bring a lot of inconvenience when other materials are extracted in processing, therefore with steam or hot water the boric anhydride dissolving is formed boric acid in advance and is very important.The material of liquid-solid like this separation two aspects extracts all very convenient, and the material of extraction is also purer.
One should improve constantly the value of output object to the utilization of boron mud, and some markets of output product in short supply, that added value is big is to improve the economic benefit that boron mud utilizes.
Its two, well-known, being widely used of boron fluoride.Being widely used in fields such as medication chemistry, petrochemical complex and light industry electronics, is the ideal catalyzer.Therefore, in the technical scheme of handling boron mud refuse, should consider the recycling of boron as far as possible, as produce boron fluoride.
Summary of the invention
The present invention is intended to the utilization and the market requirement at boron mud waste material, and a kind of method for preparing boron fluoride and hydrochloric acid with boron mud washing lotion is provided.
To achieve these goals, the technical scheme of a kind of method for preparing boron fluoride and hydrochloric acid with boron mud washing lotion of the present invention is as follows.
A kind ofly prepare the method for boron fluoride and hydrochloric acid with boron mud washing lotion, boron mud was kept 1-2 hour to 60-80 ℃ with steam heating, with drying the liquid-solid separation of whizzer, the filtrate based on boric acid that obtains is boron mud washing lotion then;
In corrosion resistant reactor, boric acid in its boron mud washing lotion and hydrochloric acid are 1 by the mass ratio of pure substance with clarifying described boron mud washing lotion and hydrochloric acid reaction: 0.98-1.38, under stirring slowly, carrying out chemical reaction, and reaction generates boron trichloride liquid; The impurity filter cake that filtration obtains minute quantity burns or is buried;
Liquid boron trichloride and hydrogen fluoride reaction are in airtight fluorinator, the mass ratio of liquid boron trichloride and ammonium acid fluoride pure substance meter is 1: 0.31-0.71, reaction generates boron trifluoride and hydrochloric acid mixture under the stirring that blows slowly, and filtration obtains aqueous hydrochloric acid and returns recycle; Boron triflouride gas collects and is compressed into jar and becomes gas products.
Chemical equation of the present invention is:
B
2O
3+3H
2O＝＝＝＝2H
3BO
3
H
3BO
3+3HCl＝＝＝＝BCl
3+3H
2O
BCl
3+3HF＝＝＝＝BF
3+3HCl
Beneficial effect of the present invention is: one, the invention provides a kind of method for preparing boron fluoride and hydrochloric acid with boron mud washing lotion, this method has effectively utilized the material that separates boron mud to form, for to next step extraction of boron mud with utilize the smooth and easy of work to lay the first stone.Its two, the purposes of preparation boron fluoride is wide, be the bigger product of a kind of economic worth, has improved the economic benefit of handling boron mud waste material, has created very big income repayment, is the model of the chemical industry comprehensive regulation and utilization.Its three, less investment, particularly suitable to the boron mud of used boron mud of process for producing Magnesium Carbonate Light 41-45 and similar components, we can say and opened up a new road.Its four, the purity height of preparation, quality is guaranteed.
Embodiment
Embodiment one
A kind ofly prepare the method for boron fluoride and hydrochloric acid with boron mud washing lotion, boron mud was kept 1-2 hour to 60-80 ℃ with steam heating, with drying the liquid-solid separation of whizzer, the filtrate based on boric acid that obtains is boron mud washing lotion then.Owing to contain boron oxide 3%, the per-cent solubility that can be calculated the boron mud washing lotion that obtains after the hydrolysis by the hydrolysis reaction formula of above-mentioned boron oxide is 5.04%.
Get 500 kilograms of boron mud washing lotions, with clarifying described boron mud washing lotion and hydrochloric acid reaction in corrosion resistant reactor, boric acid in its boron mud washing lotion and hydrochloric acid are 1: 0.98 by the mass ratio of pure substance, are carrying out chemical reaction under stirring slowly, and reaction generates boron trichloride liquid.Under this situation, generate 28 kilograms of boron trichloride liquid.The impurity filter cake that filtration obtains minute quantity burns or is buried.
With 28 kilograms of liquid boron trichlorides and hydrogen fluoride reaction in airtight fluorinator, the mass ratio of liquid boron trichloride and ammonium acid fluoride pure substance meter is 1: 0.31, reaction generates boron trifluoride and hydrochloric acid mixture under the stirring that blows slowly, wherein generate 9.84 kilograms of boron trifluorides, generate 15.84 kilograms of hydrochloric acid.Boron triflouride gas collects and is compressed into jar and becomes gas products, filters to obtain aqueous hydrochloric acid and return recycle.
Embodiment two
A kind ofly prepare the method for boron fluoride and hydrochloric acid with boron mud washing lotion, boron mud was kept 1-2 hour to 60-80 ℃ with steam heating, with drying the liquid-solid separation of whizzer, the filtrate based on boric acid that obtains is boron mud washing lotion then.Owing to contain boron oxide 3%, but be 5.04% by the per-cent solubility that the hydrolysis reaction formula reckoner of above-mentioned boron oxide goes out the boron mud washing lotion that obtains after the hydrolysis.
Get 500 kilograms of boron mud washing lotions, with clarifying described boron mud washing lotion and hydrochloric acid reaction in corrosion resistant reactor, boric acid in its boron mud washing lotion and hydrochloric acid are 1: 1.18 by the mass ratio of pure substance, are carrying out chemical reaction under stirring slowly, and reaction generates boron trichloride liquid.Under this situation, generate 33.70 kilograms of boron trichloride liquid.The impurity filter cake that filtration obtains minute quantity burns or is buried.
With 33.70 kilograms of liquid boron trichlorides and hydrogen fluoride reaction in airtight fluorinator, the mass ratio of liquid boron trichloride and ammonium acid fluoride pure substance meter is 1: 0.51, reaction generates boron trifluoride and hydrochloric acid mixture under the stirring that blows slowly, wherein generate 19.48 kilograms of boron trifluorides, generate 31.37 kilograms of hydrochloric acid.Boron triflouride gas collects and is compressed into jar and becomes gas products, filters to obtain aqueous hydrochloric acid and return recycle.
Embodiment three
A kind ofly prepare the method for boron fluoride and hydrochloric acid with boron mud washing lotion, boron mud was kept 1-2 hour to 60-80 ℃ with steam heating, with drying the liquid-solid separation of whizzer, the filtrate based on boric acid that obtains is boron mud washing lotion then.Owing to contain boron oxide 3%, but be 5.04% by the per-cent solubility that the hydrolysis reaction formula reckoner of above-mentioned boron oxide goes out the boron mud washing lotion that obtains after the hydrolysis.
Get 500 kilograms of boron mud washing lotions, with clarifying described boron mud washing lotion and hydrochloric acid reaction in corrosion resistant reactor, boric acid in its boron mud washing lotion and hydrochloric acid are 1: 1.38 by the mass ratio of pure substance, are carrying out chemical reaction under stirring slowly, and reaction generates boron trichloride liquid.Under this situation, generate 39.39 kilograms of boron trichloride liquid.The impurity filter cake that filtration obtains minute quantity burns or is buried.
With 39.39 kilograms of liquid boron trichlorides and hydrogen fluoride reaction in airtight fluorinator, the mass ratio of liquid boron trichloride and ammonium acid fluoride pure substance meter is 1: 0.71, reaction generates boron trifluoride and hydrochloric acid mixture under the stirring that blows slowly, wherein generate 31.70 kilograms of boron trifluorides, generate 51.05 kilograms of hydrochloric acid.Boron triflouride gas collects and is compressed into jar and becomes gas products, filters to obtain aqueous hydrochloric acid and return recycle.
Claims (1)
1. one kind prepares the method for boron fluoride and hydrochloric acid with boron mud washing lotion, it is characterized in that: boron mud was kept 1-2 hour to 60-80 ℃ with steam heating, and with drying the liquid-solid separation of whizzer, the filtrate based on boric acid that obtains is boron mud washing lotion then;
In corrosion resistant reactor, boric acid in its boron mud washing lotion and hydrochloric acid are 1 by the mass ratio of pure substance with clarifying described boron mud washing lotion and hydrochloric acid reaction: 0.98-1.38, under agitation carrying out chemical reaction, and reaction generates boron trichloride liquid; The impurity filter cake that filtration obtains minute quantity burns or is buried;
Liquid boron trichloride and hydrogen fluoride reaction are in airtight fluorinator, the mass ratio of liquid boron trichloride and ammonium acid fluoride pure substance meter is 1: 0.31-0.71, reaction under agitation generates boron trifluoride and hydrochloric acid mixture, and filtration obtains aqueous hydrochloric acid and returns recycle; Boron triflouride gas collects and is compressed into jar and becomes gas products.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010556435 CN102180475A (en) | 2010-11-23 | 2010-11-23 | Method for preparing boron fluoride and hydrochloric acid by using boron slurry washing liquor |
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|---|---|---|---|
| CN 201010556435 CN102180475A (en) | 2010-11-23 | 2010-11-23 | Method for preparing boron fluoride and hydrochloric acid by using boron slurry washing liquor |
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|---|---|
| CN102180475A true CN102180475A (en) | 2011-09-14 |
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| CN 201010556435 Pending CN102180475A (en) | 2010-11-23 | 2010-11-23 | Method for preparing boron fluoride and hydrochloric acid by using boron slurry washing liquor |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105803480A (en) * | 2016-05-09 | 2016-07-27 | 上海应用技术学院 | Preparation method of boron trifluoride gas |
-
2010
- 2010-11-23 CN CN 201010556435 patent/CN102180475A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 《化学化工大辞典》 20030131 《化学化工大辞典》编委会 硼酸、三氯化硼 第1757、第1983页 , * |
| 《实验化学》 20051130 刘约权等 实验五十四 高等教育出版社 第278-279页 , * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105803480A (en) * | 2016-05-09 | 2016-07-27 | 上海应用技术学院 | Preparation method of boron trifluoride gas |
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Application publication date: 20110914 |