CN105883840A - Method for producing boron fluoride and hydrochloric acid from boron mud waste liquid - Google Patents
Method for producing boron fluoride and hydrochloric acid from boron mud waste liquid Download PDFInfo
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- CN105883840A CN105883840A CN201410477945.2A CN201410477945A CN105883840A CN 105883840 A CN105883840 A CN 105883840A CN 201410477945 A CN201410477945 A CN 201410477945A CN 105883840 A CN105883840 A CN 105883840A
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- boron
- hydrochloric acid
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- boron mud
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Abstract
The invention discloses a method for producing boron fluoride and hydrochloric acid from a boron mud waste liquid and relates to the technical field of inorganic chemical three-waste treatment and integrated utilization. The method comprises that a clear boron mud washing liquid and hydrochloric acid undergo a reaction in a corrosion-resistant reactor along with stirring to produce a boron trichloride liquid, wherein a pure substance mass ratio of boric acid in the boron mud washing liquid to hydrochloric acid is 1: 0.95-1.39, the liquid boron trichloride and hydrogen fluoride undergo a reaction in an enclosed fluorinator along with stirring to produce a boron trichloride-hydrochloric acid mixture, wherein a pure substance mass ratio of the liquid boron trichloride to hydrogen fluoride is 1: 0.29-0.73, the mixture is filtered, the hydrochloric acid water solution is returned and recycled and the boron trichloride gas is collected and compressed to form a gas product. The method effectively utilizes separated boron mud composition, lays a basis for smooth boron mud later extraction and utilization and creates large 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 one utilizes boron mud waste liquid to produce fluorine
Change boron and the method for hydrochloric acid.
Background technology
Boron mud is with boromagnesite (2MgO B2O3·H2O) it is raw material, is mixed with soda ash by roasting, pulverizing, take carbon water law
Produce borax (Na2B4O7·10H2O), remaining solid waste after washing, crystallization process extract borax.Producing one ton of borax can
Producing 4 tons of boron mud, a borax plant producing 8000 tons per year, can produce boron mud every year is 3.2 ten thousand tons.Owing to the discharge capacity of boron mud is relatively big,
The current multiple comprehensive Utilization Ways of domestic employing, in addition to producing light magnesium carbonate and magnesia and plastic and rubber filler, also produces boron
Mei Lin composite fertilizer, make honeycomb briquette coal charging and do architectural borax etc..
Magnesium in boron mud is typically all presented in magnesium carbonate, sometimes has difference also with the mineral products difference of boromagnesite.
The component of production light magnesium carbonate boron mud is such that magnesia and accounts for 38%, and silica accounts for 20%, and carbon dioxide accounts for 17%,
Boron oxide accounts for 3%, and calcium oxide accounts for 3%, and manganese oxide accounts for 0.11%, and other is moisture content.
Boron mud washing lotion is the inevitable step processing and carrying out before processing boron mud, is because diboron trioxide is dissolved in the characteristic of hot water
Carry out extracting.Otherwise it can bring a lot of inconvenience, the most in advance with steam or hot water other materials are extracted in processing when
Boric anhydride is dissolved formation boric acid be very important.So material of both solid-liquor separation extracts all very convenient, the material of extraction
Also compare pure.
One, should improve constantly the value of output object to the utilization of boron mud, product that some markets of output are in short supply, that added value is big,
To improve the economic benefit that boron mud utilizes.
They are two years old, it is well known that being widely used of boron fluoride.Boron fluoride is widely used in medication chemistry, petrochemical industry and light industry electricity
The fields such as son, it is preferable catalyst.Therefore, in the technical scheme processing boron mud refuse, the recovery of boron should be considered as far as possible
Utilize, as produced boron fluoride.
Summary of the invention
It is contemplated that for the utilization of boric sludge waste and the market demand, it is provided that one utilizes boron mud waste liquid to produce boron fluoride and hydrochloric acid
Method.
To achieve these goals, the technical scheme of a kind of method utilizing boron mud waste liquid to produce boron fluoride and hydrochloric acid of the present invention is as follows.
A kind of utilize boron mud waste liquid to produce boron fluoride and the method for hydrochloric acid, boron mud steam is heated to 59~81 DEG C maintain 1.1~
2.1 hours, then with drying centrifuge solid-liquor separation, the filtrate based on boric acid obtained i.e. boron mud washing lotion;
By described boron mud washing lotion and the hydrochloric acid reaction of clarification in corrosion resistant reactor, the boric acid in its boron mud washing lotion is pressed with hydrochloric acid
The mass ratio of pure material meter is 1: 0.95~1.39, carries out chemical reaction under stirring slowly, and reaction generates boron chloride liquid
Body;It is filtrated to get minimal amount of impurity filter cake to burn or buried;
Liquid boron chloride and hydrogen fluoride reaction in airtight fluorination reaction, liquid boron chloride and the hydrogen fluoride matter based on pure material
Amount ratio is 1: 0.29~0.73, and under stirring slowly, reaction generates boron trifluoride and hydrochloric acid mixture, is filtrated to get hydrochloric acid water
Solution returns to recycle;Boron triflouride gas collects and is compressed into tank and becomes gas products.
The chemical equation of the present invention is:
B2O3+3H2O=2H3BO3
H3BO3+ 3HCl=BCl3+3H2O
BCl3+ 3HF=BF3+3HCl
The beneficial effects of the present invention is: one, the invention provides and a kind of utilize boron mud waste liquid to produce boron fluoride and the side of hydrochloric acid
Method, the method effectively make use of the material composition separating boron mud, for boron mud, next step extracts and utilizes the smooth and easy of work to carry out
Lay the first stone.Its two, the purposes of preparation boron fluoride is wide, is the product that a kind of economic worth is bigger, improves process boron mud and gives up
The economic benefit of material, creates the biggest profit return, is the model of the chemical industry comprehensive regulation and utilization.Its three, small investment,
Especially suitable to the boron mud of boron mud and similar components used by process for producing light magnesium carbonate, it may be said that to open a Tiao Xin road.Its four,
The purity of preparation is high, and quality is guaranteed.
Detailed description of the invention
Embodiment one
A kind of utilize boron mud waste liquid to produce boron fluoride and the method for hydrochloric acid, boron mud steam is heated to 59~81 DEG C maintain 1.1~
2.1 hours, then with drying centrifuge solid-liquor separation, the filtrate based on boric acid obtained i.e. boron mud washing lotion.Due to containing oxidation
Boron 3%, the hydrolysis formula of above-mentioned boron oxide the percentage solubility of the boron mud washing lotion obtained after can calculating hydrolysis is 5.04%.
Take 500 kilograms of boron mud washing lotions, by described boron mud washing lotion and the hydrochloric acid reaction of clarification in corrosion resistant reactor, its boron mud
Boric acid in washing lotion and the hydrochloric acid mass ratio based on pure material is 1: 0.98, carries out chemical reaction, reaction under stirring slowly
Generate boron chloride liquid.Under this situation, generate boron chloride liquid 28 kilograms.It is filtrated to get minimal amount of impurity filter cake to burn
Or it is buried.
By 28 kg liquid boron chlorides and hydrogen fluoride reaction in airtight fluorination reaction, liquid boron chloride and hydrogen fluoride are by pure thing
The mass ratio of matter meter is 1: 0.31, and under stirring slowly, reaction generates boron trifluoride and hydrochloric acid mixture, wherein generates trifluoro
Change boron 9.84 kilograms, generate hydrochloric acid 15.84 kilograms.Boron triflouride gas collects and is compressed into tank and becomes gas products, filters
Obtain aqueous hydrochloric acid solution to return to recycle.
Embodiment two
A kind of utilize boron mud waste liquid to produce boron fluoride and the method for hydrochloric acid, boron mud steam is heated to 59~81 DEG C maintain 1.1~
2.1 hours, then with drying centrifuge solid-liquor separation, the filtrate based on boric acid obtained i.e. boron mud washing lotion.Due to containing oxidation
Boron 3%, by the hydrolysis formula of above-mentioned boron oxide can computational chart go out hydrolysis after the percentage solubility of boron mud washing lotion that obtains be 5.04
%.
Take 500 kilograms of boron mud washing lotions, by described boron mud washing lotion and the hydrochloric acid reaction of clarification in corrosion resistant reactor, its boron mud
Boric acid in washing lotion and the hydrochloric acid mass ratio based on pure material is 1: 1.18, carries out chemical reaction, reaction under stirring slowly
Generate boron chloride liquid.Under this situation, generate boron chloride liquid 33.70 kilograms.It is filtrated to get minimal amount of impurity filter cake
Burn or buried.
By 33.70 kg liquid boron chlorides and hydrogen fluoride reaction in airtight fluorination reaction, liquid boron chloride is pressed with hydrogen fluoride
The mass ratio of pure material meter is 1: 0.51, and under stirring slowly, reaction generates boron trifluoride and hydrochloric acid mixture, wherein generates
Boron trifluoride 19.48 kilograms, generates hydrochloric acid 31.37 kilograms.Boron triflouride gas collects and is compressed into tank and becomes gas products,
It is filtrated to get aqueous hydrochloric acid solution to return to recycle.
Embodiment three
A kind of utilize boron mud waste liquid to produce boron fluoride and the method for hydrochloric acid, boron mud steam is heated to 59~81 DEG C maintain 1.1~
2.1 hours, then with drying centrifuge solid-liquor separation, the filtrate based on boric acid obtained i.e. boron mud washing lotion.Due to containing oxidation
Boron 3%, by the hydrolysis formula of above-mentioned boron oxide can computational chart go out hydrolysis after the percentage solubility of boron mud washing lotion that obtains be 5.04
%.
Take 500 kilograms of boron mud washing lotions, by described boron mud washing lotion and the hydrochloric acid reaction of clarification in corrosion resistant reactor, its boron mud
Boric acid in washing lotion and the hydrochloric acid mass ratio based on pure material is 1: 1.38, carries out chemical reaction, reaction under stirring slowly
Generate boron chloride liquid.Under this situation, generate boron chloride liquid 39.39 kilograms.It is filtrated to get minimal amount of impurity filter cake
Burn or buried.
By 39.39 kg liquid boron chlorides and hydrogen fluoride reaction in airtight fluorination reaction, liquid boron chloride is pressed with hydrogen fluoride
The mass ratio of pure material meter is 1: 0.71, and under stirring slowly, reaction generates boron trifluoride and hydrochloric acid mixture, wherein generates
Boron trifluoride 31.70 kilograms, generates hydrochloric acid 51.05 kilograms.Boron triflouride gas collects and is compressed into tank and becomes gas products,
It is filtrated to get aqueous hydrochloric acid solution to return to recycle.
Claims (1)
1. one kind utilizes boron mud waste liquid to produce boron fluoride and the method for hydrochloric acid, it is characterised in that: boron mud steam is heated to 59~
81 DEG C maintain 1.1~2.1 hours, then with drying centrifuge solid-liquor separation, the filtrate based on boric acid obtained i.e. boron mud washing lotion;
By described boron mud washing lotion and the hydrochloric acid reaction of clarification in corrosion resistant reactor, the boric acid in its boron mud washing lotion and hydrochloric acid are by pure thing
The mass ratio of matter meter is 1: 0.95~1.39, under agitation carries out chemical reaction, and reaction generates boron chloride liquid;Filter
Obtain minimal amount of impurity filter cake to burn or buried;Liquid boron chloride and hydrogen fluoride reaction in airtight fluorination reaction, liquid
Boron chloride and the hydrogen fluoride mass ratio based on pure material is 1: 0.29~0.73, and under agitation reaction generates boron trifluoride and salt
Acid blend, is filtrated to get aqueous hydrochloric acid solution and returns to recycle;Boron triflouride gas collects and is compressed into tank and becomes gas
Product.
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CN201410477945.2A CN105883840A (en) | 2014-09-10 | 2014-09-10 | Method for producing boron fluoride and hydrochloric acid from boron mud waste liquid |
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CN201410477945.2A CN105883840A (en) | 2014-09-10 | 2014-09-10 | Method for producing boron fluoride and hydrochloric acid from boron mud waste liquid |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107585776A (en) * | 2017-10-13 | 2018-01-16 | 湖北省宏源药业科技股份有限公司 | A kind of method of Rheological Phase Method synthesis LiBF4 |
CN114797754A (en) * | 2022-03-29 | 2022-07-29 | 常熟理工学院 | Method for preparing efficient wastewater adsorbent by using boron mud |
-
2014
- 2014-09-10 CN CN201410477945.2A patent/CN105883840A/en active Pending
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107585776A (en) * | 2017-10-13 | 2018-01-16 | 湖北省宏源药业科技股份有限公司 | A kind of method of Rheological Phase Method synthesis LiBF4 |
CN114797754A (en) * | 2022-03-29 | 2022-07-29 | 常熟理工学院 | Method for preparing efficient wastewater adsorbent by using boron mud |
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Application publication date: 20160824 |
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