CN105347352B - A kind of high-efficiency energy-saving heat reverse-extraction method production boric acid new process - Google Patents

A kind of high-efficiency energy-saving heat reverse-extraction method production boric acid new process Download PDF

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CN105347352B
CN105347352B CN201510899036.2A CN201510899036A CN105347352B CN 105347352 B CN105347352 B CN 105347352B CN 201510899036 A CN201510899036 A CN 201510899036A CN 105347352 B CN105347352 B CN 105347352B
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boric acid
strip liquor
liquor
temperature
strip
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CN105347352A (en
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李洪岭
曹闽生
张宁红
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Qinghai liyada Chemical Co.,Ltd.
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李洪岭
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Abstract

A kind of high-efficiency energy-saving heat reverse-extraction method production boric acid new process, polyalcohol extractant is used to extract boric acid at normal temperature boric acid liquid mine, obtain extract liquor, it is 2 that process water acid, which is adjusted pH value, obtain strip liquor, strip liquor is mixed with extract liquor, it is stripped under stirring, it is characterized in that back extraction temperature is 35 ~ 100 DEG C, according to temperature, the usage amount of strip liquor is adjusted, makes 49.9 ~ 184.8 g/L of boric acid mass-volume concentration in strip liquor, the strip liquor of obtained high concentration, direct crystallisation by cooling obtain boric acid.The characteristics of present invention has significant energy-saving effect, and process route is short, high production efficiency, and production capacity is high, and superior product quality is environmental-friendly, product cost.

Description

A kind of high-efficiency energy-saving heat reverse-extraction method production boric acid new process
One, technical field
The present invention relates to chemical production technology, in particular to a kind of high-efficiency energy-saving heat reverse-extraction method produces boric acid new process.
Two, background technique
Boric acid, molecular formula H3BO3, it is a kind of important chemical products, is widely used in medicine, chemical industry, building materials, optical fiber etc. Industry.In nature, boron is present in solid boron rock and liquid boron rock.Boric acid production is most to utilize solid boron rock, production technology There are acid system and alkaline process etc..Liquid boron rock using evaporation or acidizing crystal, is recycled after forming solid mineral, is directly utilized not mostly More, the method directly utilized at present is mainly extraction.
The chemical substances such as extraction technology utilization polyalcohol as extractant, by the boric acid in liquid boron rock extract into Enter in extractant (polyalcohol), realize the separation of boric acid and other materials, the extractant (polyalcohol) after extracting boric acid is again with acid The aqueous solution of change is stripped at normal temperature, will be entered the back extraction of the boric acid in extractant (polyalcohol) and be entered in the aqueous solution of acidification, and obtain The boric acid aqueous solution few to the higher impurity of purity.Boric acid is crystallized out using the method for evaporating, concentrating and crystallizing again, separates drying After obtain boric acid product.
The boric acid back extraction to appear in the newspapers at present is all to carry out at normal temperature, and concentration of the boric acid in the aqueous solution of acidification is maximum only 40g/L can be reached, can not direct crystallization go out boric acid, also need using be concentrated by evaporation method crystallize to obtain boric acid product, this work The major defect of skill is energy consumption height, and the production cycle is long, and low efficiency, production capacity are low, and product quality is not high, and machine utilization is big.
Three, summary of the invention
The present invention proposes a kind of high-efficiency energy-saving heat reverse-extraction method aiming at the deficiency of extraction production boric acid prior art Produce boric acid new process.The quasi- technical solution taken of the present invention are as follows: a kind of high-efficiency energy-saving heat reverse-extraction method production boric acid new process, it will Boric acid liquid mine uses polyalcohol extractant to extract boric acid at normal temperature, obtains extract liquor, and it is 2 that process water acid, which is adjusted pH value, Strip liquor is obtained, strip liquor is mixed with extract liquor, is stripped under stirring, it is characterised in that back extraction temperature is 35 ~ 100 DEG C, root According to temperature, the usage amount of strip liquor is adjusted, makes 49.9 ~ 184.8 g/L of boric acid mass-volume concentration in strip liquor, obtains High concentration strip liquor, direct crystallisation by cooling obtains boric acid.
For a better understanding of the present invention, it is described further below.Polyalcohol 25L is taken, is added in 1L kerosene, extraction is made The total 26L of agent is taken, the liquid boron rock (H in advance with hydrochloric acid tune PH to 3 is added to3BO3Content 20g/L) in 60L, liquid boron rock is day Right boracic lake water, brine and industrial boracic low concentration aqueous solution extract under room temperature, obtain the extract liquor 26L of boronic acid containing 37g/L; Good extract liquor 5L made above is added in the 15L reaction kettle with stirring, while preparing 950 ml of pure water of PH to 2 with hydrochloric acid It is added into reaction kettle, is heated to 35 DEG C, extraction is stirred under heat preservation, extracts stratification after boric acid out, separate, obtain strip liquor 950ml analyzes strip liquor and extract liquor boric acid concentration, and obtaining boric acid concentration in 35 DEG C of strip liquors is 49.9g/L, extraction Remaining boric acid concentration is 27.3g/L in liquid.Same method does above-mentioned experiment under 60 DEG C, 80 DEG C, 100 DEG C and room temperature (25 DEG C), Obtain the result of table 1.
Table 1
Table 1 using different temperatures gradient the experiment results show that be stripped, the boric acid concentration in strip liquor and back extraction temperature Directly proportional, i.e. back extraction temperature is higher, and the boric acid concentration in strip liquor is also higher, and remaining boric acid concentration is lower after extract liquor back extraction. The present invention is exactly to utilize this characteristic, during extraction preparing boracic acid, improves back extraction temperature, omits evaporization process, drop Low energy consumption;Purpose is exactly according to back extraction temperature, and reasonable use of water reduces water consumption and energy consumption;In traditional handicraft, the mother liquor of boric acid and Cleaning solution will return to evaporization process, increase energy consumption, and in the present invention, mother liquor, cleaning solution return in strip liquor as process water again It reuses, the water consumption in production substantially reduces;Since evaporization process is omitted, energy consumption and equipment corrosion are reduced, is saved Equipment investment and maintenance cost;
The present invention has significant energy-saving effect, and process route is short, high production efficiency, and production capacity is high, superior product quality, environment Close friend, the low feature of product cost.
Four, Detailed description of the invention
Fig. 1 is process flow chart of the invention
Fig. 2 is conventional process flow figure.
Five, specific embodiment
Preferably to describe the present invention, below with reference to process flow chart of the invention to being originally described in further details.
Polyalcohol 25L is taken, is added in 1L kerosene, the total 26L of extractant is made, is added in advance with the liquid of hydrochloric acid tune PH to 3 Body boron rock (H3BO3Content 20g/L) in 60L, liquid boron rock is natural boracic lake water, brine and industrial boracic low concentration aqueous solution, It is extracted under room temperature, obtains the extract liquor 26L of boronic acid containing 36.8g/L;
Embodiment 1: good extract liquor 5L made above is added in the 15L reaction kettle with stirring, while will be pure with hydrochloric acid Water is prepared the strip liquor 3.5L that pH value is 2 and is added into reaction kettle, and the boric acid mass-volume concentration 49.9g/ in strip liquor is made L is heated to 35 DEG C, and extraction is stirred under heat preservation, extracts stratification after boric acid out, separates, obtains strip liquor 3.5L, wherein boric acid Mass-volume concentration is 49.9g/L, and remaining boric acid concentration is 1.81g/L in polyalcohol extract liquor.Add in obtained strip liquor Enter 4g decolorising agent and carry out decoloration deodorization, after the direct crystallisation by cooling of isolated clear liquid, separation, washing, drying, obtains 49g boron Acid product, mother liquor, washing water return to strip liquor process as process water and reuse.Product is through analyzing: H3BO3100.27% Cl- 0.02% SO4 2-0.01% Fe0.005%。
Embodiment 2: good extract liquor 5L made above is added in the 15L reaction kettle with stirring, while will be pure with hydrochloric acid Water is prepared the strip liquor 1.6L that pH value is 2 and is added into reaction kettle, and the boric acid mass-volume concentration 110g/L in strip liquor is made, 60 DEG C are heated to, extraction is stirred under heat preservation, extracts stratification after boric acid out, separates, obtains strip liquor 1.6L, wherein boric acid matter Amount volumetric concentration is 109g/L, and remaining boric acid concentration is 1.8g/L in polyalcohol extract liquor.4g is added in obtained strip liquor Decolorising agent carries out decoloration deodorization, after the direct crystallisation by cooling of isolated clear liquid, separation, washing, drying, obtains the production of 115g boric acid Product, mother liquor, washing water return to strip liquor process as process water and reuse.Product is through analyzing: H3BO3100.3% Cl- 0.017% SO4 2-0.009% Fe0.0003%。
Embodiment 3: good extract liquor 5L made above is added in the 15L reaction kettle with stirring, while will be pure with hydrochloric acid Water is prepared the strip liquor 1.1L that pH value is 2 and is added into reaction kettle, and the boric acid mass-volume concentration 160g/L in strip liquor is made, 80 DEG C are heated to, extraction is stirred under heat preservation, extracts stratification after boric acid out, separates, obtains strip liquor 1.1L, wherein boric acid matter Amount volumetric concentration is 158.8g/L, and remaining boric acid concentration is 1.8g/L in polyalcohol extract liquor.It is added in obtained strip liquor 4g decolorising agent carries out decoloration deodorization, after the direct crystallisation by cooling of isolated clear liquid, separation, washing, drying, obtains 133g boric acid Product, mother liquor, washing water return to strip liquor process as process water and reuse.Product is through analyzing: H3BO3100.21% Cl- 0.01% SO4 2-0.008% Fe0.0003%。
Embodiment 4: good extract liquor 5L made above is added in the 15L reaction kettle with stirring, while will be pure with hydrochloric acid Water is prepared the strip liquor 0.95L that pH value is 2 and is added into reaction kettle, and the boric acid mass-volume concentration in strip liquor is made 184.8g/L is heated to 100 DEG C, and extraction is stirred under heat preservation, extracts stratification after boric acid out, separates, obtains strip liquor 0.95L, wherein boric acid mass-volume concentration is 183.2g/L, and remaining boric acid concentration is 1.8g/L in polyalcohol extract liquor.? To strip liquor in 4g decolorising agent be added carry out decoloration deodorization, by the isolated direct crystallisation by cooling of clear liquid, separation, washing, dry After dry, 142g boric acid product is obtained, mother liquor, washing water return to strip liquor process as process water and reuse.Product is through analyzing: H3BO3100.09% Cl-0.01% SO4 2-0.009% Fe0.00035%。
It is tested using traditional handicraft experimental control
1) good extract liquor 5L made above is added in the 15L reaction kettle with stirring, while is prepared pure water with hydrochloric acid The strip liquor 5.1L that pH value is 2 is added into reaction kettle, and stirring extraction 1 hour is stripped out stratification after boric acid, separates, obtain To strip liquor 5.1L, wherein boric acid concentration 34.1g/L, remaining boric acid concentration is 1.805g/L in polyalcohol extract liquor.
2) strip liquor is evaporated to about 1.1L, the evaporation capacity 3.9L concentrate of water contains H3BO3160.5g/L Cl-0.05g/L SO2-0.04g/L Fe0.018g/L after crystallisation by cooling, separation, washing, drying, obtains 133.3g boric acid product, this product is through dividing Analyse H3BO399.725% Cl-0.05% SO4 2-0.03% Fe0.012%。
By Examples 1 to 4 and the list of traditional handicraft experimental data, it is shown in Table 2
From being shown in Table 2 it can be seen that traditional handicraft has the disadvantage in that
1, boric acid product must could be made through being concentrated by evaporation in the strip liquor obtained.According to embodiment 3, energy consumption data and biography System process energy consumption data, which compare to calculate conventionally produced 1 ton of boric acid and consume thermal energy more than new process and about consume, marks 4.3 tons of coal, The carbon for providing the fuel discharge of thermal energy causes pollution to environment simultaneously.
2, it is concentrated by evaporation the impurity content increased in strip liquor, boric acid product impurity is caused to increase.
3, evaporation process solution acidity constantly increases, and equipment corrosion is caused to increase.
The present invention overcomes above disadvantage, the present invention has significant energy-saving effect, and process route is short, production efficiency Height, production capacity is high, and superior product quality is environmental-friendly, the low feature of product cost.

Claims (3)

1. a kind of high-efficiency energy-saving heat reverse-extraction method produces boric acid new process, boric acid liquid mine is used into polyalcohol extractant at normal temperature Boric acid is extracted, extract liquor is obtained, it is 2 that process water acid, which is adjusted pH value, obtains strip liquor, and strip liquor is mixed with extract liquor, stirring Under be stripped, it is characterised in that back extraction temperature be 80~100 DEG C, according to temperature, adjust the usage amount of strip liquor, make strip liquor In boric acid mass-volume concentration be 160~184.8g/L, obtained high concentration strip liquor, direct crystallisation by cooling obtains boric acid;
The polyalcohol extractant is that polyalcohol 25L is added in 1L kerosene.
2. a kind of high-efficiency energy-saving heat reverse-extraction method according to claim 1 produces boric acid new process, which is characterized in that back extraction temperature Degree is 80 DEG C, according to temperature, adjusts the usage amount of strip liquor, makes the boric acid mass-volume concentration 160g/L in strip liquor, obtain The high concentration strip liquor arrived, direct crystallisation by cooling obtain boric acid.
3. a kind of high-efficiency energy-saving heat reverse-extraction method according to claim 1 produces boric acid new process, which is characterized in that back extraction temperature Degree is 100 DEG C, according to temperature, adjusts the usage amount of strip liquor, makes the boric acid mass-volume concentration 184.8g/L in strip liquor, Obtained high concentration strip liquor, direct crystallisation by cooling obtain boric acid.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101538048A (en) * 2009-04-29 2009-09-23 青海中信国安科技发展有限公司 Method for extracting boric acid from boron-containing magnesium chloride solution by using an acidification-extraction method
CN101544378A (en) * 2009-04-03 2009-09-30 河北工业大学 Process method for extracting low-concentration boracic acid in magnesium-containing brine
CN101565188A (en) * 2009-06-03 2009-10-28 邛崃市鸿丰钾矿肥有限责任公司 Technique for preparing borax from brine
CN103482640A (en) * 2013-09-27 2014-01-01 中国科学院青海盐湖研究所 Method for separating boron from boron-containing bittern

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101544378A (en) * 2009-04-03 2009-09-30 河北工业大学 Process method for extracting low-concentration boracic acid in magnesium-containing brine
CN101538048A (en) * 2009-04-29 2009-09-23 青海中信国安科技发展有限公司 Method for extracting boric acid from boron-containing magnesium chloride solution by using an acidification-extraction method
CN101565188A (en) * 2009-06-03 2009-10-28 邛崃市鸿丰钾矿肥有限责任公司 Technique for preparing borax from brine
CN103482640A (en) * 2013-09-27 2014-01-01 中国科学院青海盐湖研究所 Method for separating boron from boron-containing bittern

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