CN101565188B - Technique for preparing borax from brine - Google Patents
Technique for preparing borax from brine Download PDFInfo
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- CN101565188B CN101565188B CN2009100594916A CN200910059491A CN101565188B CN 101565188 B CN101565188 B CN 101565188B CN 2009100594916 A CN2009100594916 A CN 2009100594916A CN 200910059491 A CN200910059491 A CN 200910059491A CN 101565188 B CN101565188 B CN 101565188B
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Abstract
The invention discloses a technique for preparing borax from brine, which relates to the technical field of inorganic salt production and aims at solving the technical problems of low total yield, high cost, high energy consumption, serious environmental pollution, decreasing raw material and the like in the traditional borax production technique. The method comprises the following steps of: mixing the raw material, namely brine, with a mixed alcohol extracting agent according to the mass ratio of 1:1 to 3; extracting the raw material, namely, the brine, by a continuous countercurrent method, thus obtaining a raffinate phase and an extraction phase; mixing the extraction phase with water according to the mass ratio of 1:0.1 to 3 and using the continuous countercurrent method for back extraction, thus obtaining a back extraction solution; adjusting the pH of the back extraction solution to be 8 to 10 and then stirring and cooling the back extraction solution to form borax sediment whichis then filtered, thus obtaining solid borax decahydrate. The method is applicable to preparing borax by taking brine as the raw material.
Description
Technical field
The present invention relates to a kind of technical field of inorganic salt production, particularly a kind ofly utilize rich potassium boron bittern to produce the processing method of borax for raw material.
Background technology
Borax is a sodium tetraborate decahydrate, and molecular formula is Na
2B
4O
710H
2O.Being colourless translucent crystal or white crystalline powder, is the most important compound of boron.Borax is important chemical, metallurgical raw material, is the raw material of making opticglass, enamel and enamel in glass-ceramic industry; In metallurgical industry, be used to produce the special steel of high-strength boron steel, high hard heat-resisting alloy steel and anti-three acid corrosions; In agricultural, promptly can be used as trace element fertilizer, can make sterilant again; Aspect fine chemistry industry, be the important batching of producing washing composition, tamanori, makeup.
The traditional boron utilization of resources of China is mainly derived from China northeast and Tibet based on the solid boron rock.Through the commercial minings of decades, China's solid boron resource is exhaustion closely, can develop only surplus in the of 300 ten thousand tons of boron rock reserves, can not satisfy growing industrial requirement.
In the prior art, application number 85102759, denomination of invention " alkaline decomposition of boric ore ", though this method adopts normal pressure alkaline hydrolysis method to be better than pressure alkali decomposition and carbon alkaline process, this method temperature of reaction is had relatively high expectations; Application number 87101578, denomination of invention " preparation method of borax " is a raw material with ludwigite stone, handles making borax by smelting, melt separation and rich boron slag charge sodium, and this method processing step is longer, and it is bigger to consume energy; Application number 89105720.X, denomination of invention " a kind of technology of the producing borax from boron ore with calcic height (CaO is 32～38%) ", this method is with after the boron ore powder high-temperature roasting, replace caustic soda to carry out the causticization alkaline hydrolysis with soda ash, this method is roasting under 850 ℃ of left and right sides high temperature, shortcomings such as exist service temperature higher, the reaction times is longer, and the alkaline hydrolysis rate is low.
Present technology with bittern production borax is after bittern evaporation is concentrated, to add sulfuric acid acidation and extract boric acid, then with boric acid and alkali reaction generation borax.The yield of this method complex process, boron is 50-70% only, and the raw and auxiliary material consumption is big, the production cost height.
Generally speaking, the main drawback of borax production technology existence at present is:
1, adopt the solid boron rock as raw material, cost height, energy consumption height, China's solid boron resource is closely exhausted simultaneously;
Need the pressurized high-temperature alkaline hydrolysis when 2, being raw material, cause bigger energy expenditure and environmental pollution, count total recovery from starting material flotation, treating process simultaneously and be not higher than 40% with boron magnesium ore deposit;
3, be that raw material system borax total recovery is low with the salt lake brine, obtain thick boric acid by sulfuric acid acidation, yield is generally 70%, and in further alkalization process system borax process, yield is 65～70%, and total recovery generally is not higher than 50%.
Summary of the invention
The present invention is intended to solve that existing total recovery is low in traditional borax production technique, cost is high, energy consumption is high, environmental pollution is serious and raw material resources technical problem such as scarcity day by day, and to provide a kind of be raw material, yield height with bittern, cost is low, energy consumption is little, the technology of the low in the pollution of the environment and preparing borax from brine that raw material resources are abundant.
The objective of the invention is to be achieved through the following technical solutions.
The technology of preparing borax from brine of the present invention, comprising following steps:
A) raw brine is mixed by mass ratio 1: 1～3 with the alcohol mixture extraction agent,, get extracting phase and extraction phase by continuous countercurrent technique extraction feed bittern;
B) above-mentioned extraction phase is mixed by mass ratio 1: 0.1～3 with water, strip, get anti-stripping agent by continuous countercurrent technique;
C) adjust above-mentioned anti-stripping agent pH8～10, stir cooling, form the borax throw out, filter, obtain solid-state borax decahydrate.
The technology of preparing borax from brine of the present invention, the continuous countercurrent technique extraction progression in the wherein said step a) is 5～15 grades, and extraction temperature is 25～70 ℃, and the single-stage extraction time is 2～10 minutes.
The technology of preparing borax from brine of the present invention, the continuous countercurrent technique reextraction progression in the wherein said step b) is 3～10 grades, and the reextraction temperature is 25～70 ℃, and the single-stage back-extraction time is 2～10 minutes.
The technology of preparing borax from brine of the present invention, alcohol mixture is any one or any two kinds by volume 1～20 in the C8～C12 band branched fatty alcohol in the wherein said alcohol mixture extraction agent: 1 mixes.
The technology of preparing borax from brine of the present invention, alcohol mixture is any one or any two kinds by volume 1～20 in octanol, primary isoamyl alcohol, Pentyl alcohol, n-Heptyl alcohol, hexalin, nonyl alcohol, nonylcarbinol, the dibutyl card benzylalcohol in the wherein said alcohol mixture extraction agent: 1 mixes.
The technology of preparing borax from brine of the present invention, wherein said alcohol mixture extraction agent are by alcohol mixture and varsol by volume 1～3: 1 mixes.
The technology of preparing borax from brine of the present invention, wherein said varsol are aviation kerosene, solvent oil.
The technology of preparing borax from brine of the present invention, B2O3 content is 15～35 grams per liters in the wherein said raw brine, Ca2+ content is that 3～100 grams per liters, Mg2+ content are 3～100 grams per liters.
The technology of preparing borax from brine of the present invention under 15～40 ℃ of conditions of temperature, adds sodium hydroxide in the wherein said step c), adjusts anti-stripping agent pH, churning time 0.5～2.5 hour, and it is 10～35 ℃ that cooling forms the sedimentary temperature condition of borax.
The beneficial effect of the technology of preparing borax from brine of the present invention:
1, the present invention is a raw material with the traditional solid boron rock of subsurface brine replacement, and raw material resources are abundant, and energy consumption is little, reduces production costs;
2, in the extraction process, adopt alcohol mixture, have the selectivity height, impurity separates advantage completely, has significantly improved the borax yield as extraction agent;
3, in the back extraction process, adopt water as anti-stripping agent, it is low to have a cost, the advantage that environmental pollution is little;
4, in the borax production process, adopt sodium hydroxide to regulate pH, it is few to have a consumption, does not produce by product;
5, the present invention has filled up a big blank of domestic preparation borax technology, has bigger economic benefit and social benefit.
Description of drawings
Fig. 1 is the process flow diagram of preparing borax from brine of the present invention
Embodiment
Application principle of the present invention, effect and effect are illustrated by following embodiment with reference to accompanying drawing 1.
Embodiment 1
The fall to normal price bittern of 4 wells of Qionglai, Sichuan is picked up from use, the bittern mother liquor behind evaporation 35%～40% moisture, and the bittern composition sees Table 1.
Table 1 evaporation bittern mother liquor composition
| Element | K + | Na + | Ca 2+ | Mg 2+ | Cl - | B 2O 3 | Br - |
| Content (g/L) | 81.32 | 78.52 | 5.423 | 6.097 | 223.7 | 27.89 | 4.583 |
Get the evaporation bittern mother liquor 500mL that table 1 is formed, constant temperature is poured in the separating funnel under 60 ℃, and the alcohol mixture that adds 1000mL is as extraction agent, and alcohol mixture is octanol and dibutyl carbitol mixture, blending ratio is an octanol: Trivalin SF=20: 1, adopt continuous countercurrent technique extraction feed bittern.Be about to aforementioned mixing solutions and shake up, extracted 5 minutes, separatory gets extracting phase and load organic phases.Extracting phase carries out the next stage extraction, carries out 12 grades of extractions altogether, and extraction agent recycles.
Above-mentioned load organic phases 1000mL is poured in the separating funnel under 60 ℃, and the water that adds 0.3 times of volume adopts continuous countercurrent technique to strip as strip liquor.Be about to aforementioned mixing solutions and shake up, constant temperature was stripped 5 minutes, and separatory carries out 5 grades of reextraction altogether.
Strip liquor adds certain amount of industrial one sodium hydroxide under 20 ℃, add-on one control pH value of solution=9 of sodium hydroxide are as the criterion, and constant temperature stirred after 1 hour, cooled to 15 ℃ again, and the boron in the solution is separated out with the borax decahydrate form at this moment.
After the filtration, the borax that obtains is after 60 ℃ of oven dry, and borax purity reaches 99.7%, reaches national premium grads standard, borax single yield 70%, cyclic yield 96%.
Example 2
The fall to normal price bittern of 4 wells of Qionglai, Sichuan is picked up from use, the bittern mother liquor behind evaporation 35%～40% moisture, and the bittern composition is referring to table 1.
Get the evaporation bittern mother liquor 500mL that table 1 is formed, constant temperature is poured in the separating funnel under 60 ℃, and the alcohol mixture that adds 1000mL is as extraction agent, alcohol mixture is octanol and dibutyl carbitol mixture, and blending ratio is an octanol: dibutyl carbitol=20: 1 shakes up, extracted separatory 5 minutes.Extracting phase carries out the next stage extraction, carries out 12 grades of extractions altogether, and extraction agent recycles, and load organic phases is stripped.Above-mentioned load organic phases 1000mL is poured in the separating funnel under 60 ℃, the water that adds 0.3 times of volume is as strip liquor, shake up, constant temperature was stripped 2 minutes, separatory carries out 5 grades of reextraction altogether, and strip liquor adds certain amount of industrial one sodium hydroxide under 20 ℃, add-on one control pH value of solution=8 of sodium hydroxide are as the criterion, constant temperature stirred after 0.5 hour, cooled to 15 ℃ again, and the boron in the solution is separated out with the borax decahydrate form at this moment, after the filtration, the borax that obtains is after 60 ℃ of oven dry, and borax purity reaches 99.5%, reaches national premium grads standard, borax single yield 72%, cyclic yield 98%.
Example 3
The fall to normal price bittern of 4 wells of Qionglai, Sichuan is picked up from use, the bittern mother liquor behind evaporation 35%～40% moisture, and the bittern composition is referring to table 1.
Get the evaporation bittern mother liquor 500mL that table 1 is formed, constant temperature is poured in the separating funnel under 25 ℃, and the octanol that adds 1500mL shakes up as extraction agent, extracts separatory 3 minutes.Extracting phase carries out the next stage extraction, carries out 15 grades of extractions altogether, and extraction agent recycles, and load organic phases is stripped.Above-mentioned load organic phases 1000mL is poured in the separating funnel under 25 ℃, the water that adds 0.1 times of volume is as strip liquor, shake up, constant temperature was stripped 2 minutes, separatory carries out 3 grades of reextraction altogether, and strip liquor adds certain amount of industrial one sodium hydroxide under 15 ℃, add-on one control pH value of solution=8 of sodium hydroxide are as the criterion, constant temperature stirred after 1 hour, cooled to 20 ℃ again, and the boron in the solution is separated out with the borax decahydrate form at this moment, after the filtration, the borax that obtains is after 50 ℃ of oven dry, and borax purity reaches 99.5%, reaches national premium grads standard, borax single yield 70%, cyclic yield 95%.
Example 4
The fall to normal price bittern of 4 wells of Qionglai, Sichuan is picked up from use, the bittern mother liquor behind evaporation 35%～40% moisture, and the bittern composition is referring to table 1.
Get the evaporation bittern mother liquor 500mL that table 1 is formed, constant temperature is poured in the separating funnel under 70 ℃, and the alcohol mixture that adds 1200mL is as extraction agent, alcohol mixture is octanol and aviation kerosene mixture, and blending ratio is an octanol: aviation kerosene=1: 2 shakes up as extraction agent, extracted separatory 3 minutes.Extracting phase carries out the next stage extraction, carries out 5 grades of extractions altogether, and extraction agent recycles, and load organic phases is stripped.Above-mentioned load organic phases 1000mL is poured in the separating funnel under 70 ℃, the water that adds 3 times of volumes is as strip liquor, shake up, constant temperature was stripped 10 minutes, separatory carries out 10 grades of reextraction altogether, and strip liquor adds certain amount of industrial one sodium hydroxide under 40 ℃, add-on one control pH value of solution=8 of sodium hydroxide are as the criterion, constant temperature stirred after 2.5 hours, cooled to 35 ℃ again, and the boron in the solution is separated out with the borax decahydrate form at this moment, after the filtration, the borax that obtains is after 65 ℃ of oven dry, and borax purity reaches 99.3%, reaches national premium grads standard, borax single yield 71%, cyclic yield 96%.
From the above, the technology of preparing borax from brine of the present invention, replacing traditional solid boron rock with subsurface brine is raw material, and raw material resources are abundant, and energy consumption is little, reduces production costs; In the extraction process, adopt alcohol mixture, have the selectivity height, impurity separates advantage completely, has significantly improved the borax yield as extraction agent; In the back extraction process, adopt water as anti-stripping agent, it is low to have a cost, the advantage that environmental pollution is little; Simultaneously, the present invention adopts sodium hydroxide to regulate pH in the borax production process, and not only consumption is few, also has plurality of advantages such as not producing by product.
Claims (5)
1. the technology of a preparing borax from brine is characterized in that comprising the steps:
A) raw brine is mixed by mass ratio 1: 1～3 with the alcohol mixture extraction agent,, get extracting phase and extraction phase, B in the raw brine wherein by continuous countercurrent technique extraction feed bittern
2O
3Content is 15～35 grams per liters, Ca
2+Content is 3～100 grams per liters, Mg
2+Content is 3～100 grams per liters, and wherein the alcohol mixture extraction agent is mixed by volume by alcohol mixture and varsol at 1～3: 1, and wherein continuous countercurrent technique extraction progression is 5～15 grades, and extraction temperature is 25～70 ℃, and the single-stage extraction time is 2～10 minutes;
B) above-mentioned extraction phase is mixed by mass ratio 1: 0.1～3 with water, strip by continuous countercurrent technique, get anti-stripping agent, wherein continuous countercurrent technique reextraction progression is 3～10 grades, and the reextraction temperature is 25～70 ℃, and the single-stage back-extraction time is 2～10 minutes;
C) adjust above-mentioned anti-stripping agent pH8～10, stir cooling, form the borax throw out, filter, obtain solid-state borax decahydrate.
2. the technology of preparing borax from brine as claimed in claim 1 is characterized in that: alcohol mixture is any one or any two kinds by volume 1～20 in C8～C12 band branched fatty alcohol in the described alcohol mixture extraction agent: 1 mixes.
3. the technology of preparing borax from brine as claimed in claim 1 is characterized in that: alcohol mixture is any one or any two kinds by volume 1～20 in octanol, primary isoamyl alcohol, Pentyl alcohol, n-Heptyl alcohol, hexalin, nonyl alcohol, nonylcarbinol, the dibutyl card benzylalcohol in the described alcohol mixture extraction agent: 1 mixes.
4. the technology of preparing borax from brine as claimed in claim 1, it is characterized in that: described varsol is aviation kerosene or solvent oil.
5. the technology of preparing borax from brine as claimed in claim 1, it is characterized in that: under 15～40 ℃ of conditions of temperature, add sodium hydroxide in the described step c), adjust anti-stripping agent pH, churning time 0.5～2.5 hour, it is 10～35 ℃ that cooling forms the sedimentary temperature condition of borax.
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| CN101565188B true CN101565188B (en) | 2011-07-27 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| BR102013023697B1 (en) * | 2013-09-16 | 2019-09-10 | Vale Sa | process used for the production of lithium carbonate from a brine rich in ca and mg |
| CN104860326B (en) * | 2015-05-08 | 2017-07-25 | 国家海洋局天津海水淡化与综合利用研究所 | A kind of boracic material liquid back extraction analysis boron method |
| CN105347352B (en) * | 2015-12-09 | 2019-03-08 | 李洪岭 | A kind of high-efficiency energy-saving heat reverse-extraction method production boric acid new process |
| CN105905917B (en) * | 2016-04-07 | 2018-02-16 | 中国科学院青海盐湖研究所 | The method that native borax is prepared from the carbonate type bittern of plateau |
| CN106587090B (en) * | 2016-12-23 | 2018-11-13 | 江西合纵锂业科技有限公司 | A method of synthesizing four water eight borate two sodium using liquid boron rock |
| CN108046283A (en) * | 2017-12-08 | 2018-05-18 | 中国科学院青海盐湖研究所 | The process of boron is extracted from salt lake bittern based on centrifugal extractor |
| CN114044523B (en) * | 2021-12-14 | 2022-09-30 | 内蒙古工业大学 | Process for preparing borax from blast furnace boron-rich slag through low-temperature sodium treatment |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1810643A (en) * | 2006-02-21 | 2006-08-02 | 西藏奇发矿业有限公司 | Process of extracting borax decahydrate from salt lake sediment |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1810643A (en) * | 2006-02-21 | 2006-08-02 | 西藏奇发矿业有限公司 | Process of extracting borax decahydrate from salt lake sediment |
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