CN117163968A - Method for preparing boric acid and borax from MVR boron concentrate in lithium extraction process of salt lake - Google Patents

Method for preparing boric acid and borax from MVR boron concentrate in lithium extraction process of salt lake Download PDF

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Publication number
CN117163968A
CN117163968A CN202311168278.5A CN202311168278A CN117163968A CN 117163968 A CN117163968 A CN 117163968A CN 202311168278 A CN202311168278 A CN 202311168278A CN 117163968 A CN117163968 A CN 117163968A
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boron
boric acid
mvr
borax
washing
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Inventor
李陇岗
吴小王
秦佳政
余明祥
苏建军
权彩兄
李清鸿
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Qinghai Zhongxin Guoan Lithium Development Co ltd
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Qinghai Zhongxin Guoan Lithium Development Co ltd
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Abstract

The application provides a method for preparing boric acid and borax from MVR boron concentrate in a salt lake lithium extraction process, which relates to the field of inorganic salt chemical industry and comprises the following steps: step 1, MVR forced evaporation to obtain boron concentrate; step 2, acid regulation and boric acid precipitation; step 3, boric acid primary washing and secondary countercurrent washing; and 4, drying and separating. According to the process method, the multi-step treatment flows such as MVR technology and secondary countercurrent washing are introduced, and the boron element is comprehensively and efficiently separated and concentrated from the salt lake old brine, so that the boric acid is prepared, the recovery rate of the boron is high, the salt lake resource can be effectively utilized, and the process has a wide market prospect.

Description

Method for preparing boric acid and borax from MVR boron concentrate in lithium extraction process of salt lake
Technical Field
The application relates to the technical field of inorganic salt chemical industry, in particular to a method for preparing boric acid and borax from MVR boron concentrate in a lithium extraction process of a salt lake.
Background
Boric acid is white powdery crystal or triclinic plane scaly luster crystal, has a greasy hand feeling, and the aqueous solution is weak acid. It is used in glass, enamel, ceramic, medicine, metallurgy, leather, dye, pesticide, fertilizer, textile and other industry. Boric acid has antiseptic property, and can be used as antiseptic, such as wood antiseptic, pH regulator, and antibacterial antiseptic. It is used in the fields of metal welding, leather, photography, etc. and in the manufacture of dye, heat-resistant and fireproof fabric, artificial jewel, capacitor and cosmetics. Can also be used as pesticide and catalyst. The agricultural boron-containing trace element fertilizer has fertilizer efficiency for a plurality of crops, and can improve the quality of the crops and the yield.
The West Ji-Nel salt lake brine contains a large amount of boron elements besides elements such as lithium and magnesium, and the existing method for extracting boron from raw material brine comprises the following steps: acidifying precipitation, floatation, ion exchange, solvent extraction, etc. The process for extracting boron by the acidification precipitation method has the advantages of simple process route and small equipment investment, and has wider industrial application, but the method is applicable to raw material brine with higher boron content. The existing comprehensive utilization process route of salt lake brine is generally a traditional lithium extraction process such as a calcination method, and the old brine is directly acidified to extract boric acid before extracting lithium, but the boron concentration in the old brine of the salt lake is not high (B) 2 O 3 The content is 3-35 g/L), the boron yield of the method is lower, and meanwhile, other unwanted substances besides the target boric acid can be precipitated together in the precipitation process, so that the purity of the boric acid is influenced, and the extracted boric acid product contains impurities. Therefore, the low-cost, stable and efficient boron extraction process is particularly important for the comprehensive utilization of the magnesium sulfate subtype salt lake brine.
Disclosure of Invention
Aiming at the defects existing in the prior art, the application provides a method for preparing boric acid from MVR boron concentrate in the process of extracting lithium from a salt lake, which comprises the following steps:
step 1, taking a boron-rich solution as a raw material, and forcedly evaporating and concentrating by an MVR evaporator to obtain a boron concentrate, wherein B is the boron concentrate 2 O 3 The concentration is 100-150 g/L, wherein the boron-rich solution is B obtained by separating lithium and magnesium from the old brine of the salt lake through a membrane process, separating boron by a reverse osmosis membrane after dilution, adding NaOH to change the form of the boron, and continuing concentrating by the reverse osmosis membrane 2 O 3 A concentrate having a concentration of about 17 g/L;
step 2, adding acid into the boron concentrated solution obtained in the step 1 to adjust the pH value to 1.5-4.5, then cooling the boron concentrated solution to normal temperature, separating out boric acid, and separating solid and liquid phases to obtain crude boric acid and boric acid mother liquor, wherein the acid adding amount of each 1L of the boron concentrated solution is 205-292 ml;
and 3, performing primary washing and secondary washing on the crude boric acid obtained in the step 2 to obtain wet boric acid. Firstly, pure water is mixed with crude boric acid according to the proportion of 1:1-1:1.5, and the washing is carried out for about 0.5 hour. Then, adopting countercurrent washing, mixing pure water and crude boric acid according to the proportion of 1:1, and washing for 0.5 hour, wherein the obtained secondary washing liquid is taken as washing liquid to enter primary washing;
and 4, drying the wet boric acid obtained in the step 3 at a drying temperature of 85 ℃ for 2-2.5 hours to obtain the refined boric acid.
Preferably, B of the boron concentrate in step 1 above 2 O 3 The concentration is 140-145 g/L.
Preferably, the acid added in the step 2 is any one of concentrated hydrochloric acid with the mass fraction of 37% or sulfuric acid solution prepared by preparing concentrated sulfuric acid into a ratio of 1:1, and the pH value of the boron concentrated solution is adjusted to be 1.5 after the acid is added.
Preferably, the volume ratio of pure water to crude boric acid in the first washing in the step 3 is 1:1.
On the other hand, the application also provides a method for preparing borax from MVR boron concentrate in the lithium extraction process of salt lake, which comprises the following steps:
step 1, taking a boron-rich solution as a raw material, and forcedly evaporating and concentrating through MVR to obtain a boron concentrated solution, wherein the boron isB of concentrate 2 O 3 The concentration is 159g/L, the boron-rich solution is B obtained by separating lithium and magnesium from the old brine of the salt lake by a membrane process, diluting, separating boron by a reverse osmosis membrane, adding sodium hydroxide to change the form of boron, and continuing concentrating by the reverse osmosis membrane 2 O 3 A concentrated solution having a concentration of not less than 17 g/L;
step 2, adding concentrated hydrochloric acid into the boron concentrated solution obtained in the step 1 to adjust the pH value to 9.45, then cooling the boron concentrated solution to normal temperature, separating out borax, and separating a solid-liquid phase to obtain crude borax and borax mother solution;
step 3, performing primary washing on the crude borax obtained in the step 2 to obtain borax, wherein the primary washing is that pure water and the crude borax are added according to a ratio of 1:1-1:2, and stirring is performed for 0.5h;
and 4, drying the borax obtained in the step 3 at the drying temperature of 50-80 ℃ for 0.5-2 hours to obtain dry borax.
In summary, the present application includes at least one of the following beneficial technical effects:
1. the application provides a method for preparing boric acid and borax from MVR boron concentrate in the process of extracting lithium from a salt lake, which is characterized in that the process comprises the steps of introducing MVR technology, secondary countercurrent washing and the like, comprehensively and efficiently separating and concentrating boron element from old brine of the salt lake, thereby preparing boric acid, and the recovery rate of boron is high, and the process can effectively utilize salt lake resources and has wide market prospect;
2. in the application, in the process of extracting lithium by adopting a membrane process, mother liquor obtained by magnesium-lithium separation is diluted and enters a reverse osmosis membrane to separate boron element, the form of boron is changed by NaOH treatment, then the solution rich in boron is obtained by reverse osmosis membrane concentration, and the solution is forcedly evaporated and concentrated by MVR technology, so that the boron content of boron concentrate is improved, the efficiency of adding acid for crystallization and extracting boron is improved, and the boron recovery rate is higher;
3. the method can remarkably remove the chlorate and sulfate content in the crude boric acid obtained by acid crystallization by adopting a washing mode of secondary countercurrent washing, so that the purity of the obtained boric acid product is higher;
4. the application also provides a method for preparing borax from MVR boron concentrate in the lithium extraction process of salt lake, which adopts the same technological method for preparing boric acid, only needs to add acid to adjust the pH value to about 9.45, then cooling to normal temperature and separating to obtain borax products, and the crude borax can basically reach the standard of first grade after primary washing and drying.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing boric acid and borax from MVR boron concentrate in a lithium extraction process of a salt lake;
fig. 2 is a schematic flow chart of a method for preparing borax from MVR boron concentrate.
Detailed Description
Hereinafter, techniques in the embodiments of the present application will be clearly and completely described with reference to the drawings in the embodiments of the present application; it is apparent that the described embodiments are only some, but not all, embodiments of the application; all other embodiments, which can be made by a person skilled in the art without any inventive effort, are intended to fall within the scope of the present application.
Example 1:
step 1, taking B 2 O 3 The boron-rich solution with the concentration of 17.312g/L is forcedly evaporated and concentrated by an MVR evaporator to obtain B 2 O 3 A boron concentrate having a concentration of 143.275 g/L;
and 2, adding 292ml of concentrated hydrochloric acid with the mass fraction of 37% into 1L of boron concentrate, adjusting the pH value of the boron concentrate to 1.5, cooling to normal temperature, and carrying out solid-liquid separation to obtain 264.41g of crude boric acid and 1.098L of boric acid mother liquor. The data of the chemical composition of the materials and the like of each step in the embodiment are shown in table 1.
TABLE 1
In this example, the boron yield of the crude boric acid reaches 89.65%.
Comparative example 1:
step 1, taking the boron-rich solution same as in the example 1, and forcedly evaporating and concentrating by an MVR evaporator to obtain B 2 O 3 A boron concentrate having a concentration of 127.924 g/L;
step 2, adding 240ml of concentrated hydrochloric acid with the mass fraction of 37% into 1L of boron concentrated solution to adjust the pH value of the boron concentrated solution to 1.4, cooling to normal temperature, and carrying out solid-liquid separation to obtain 227.42g of crude boric acid and 1.08L of boric acid mother solution, wherein the data of the chemical composition and the like of the materials in each step in the comparative example are shown
Table 2.
TABLE 2
In this comparative example, the boron yield of the crude boric acid reached 86.38%.
Comparative example 2:
step 1, taking the boron-rich solution same as in the example 1, and forcedly evaporating and concentrating by an MVR evaporator to obtain B 2 O 3 A boron concentrate having a concentration of 104.116 g/L;
step 2, adding 248ml of concentrated hydrochloric acid with mass fraction of 37% into 1.2L of boron concentrate to adjust the pH value of the boron concentrate to 2.5, cooling to normal temperature, and carrying out solid-liquid separation to obtain 172.98g of crude boric acid and 1.34L of boric acid mother liquor, wherein the data of chemical composition and the like of materials in each step in the comparative example are shown
Table 3.
TABLE 3 Table 3
In this comparative example, the boron yield of the crude boric acid reached 70.12%.
Comparative example 3:
step 1, step 1 of this comparative example is the same as step 1 of comparative example 2;
step 2, adding 247ml of concentrated hydrochloric acid with the mass fraction of 37% into 1.2L of boron concentrated solution to adjust the pH value of the boron concentrated solution to 3.5, cooling to normal temperature, and carrying out solid-liquid separation to obtain 168.46g of crude boric acid and 1.33L of boric acid mother solution, wherein the data of chemical compositions and the like of materials in each step in the comparative example are shown
Table 4.
TABLE 4 Table 4
In this comparative example, the boron yield of the crude boric acid reached 68.04%.
Comparative example 4:
step 1, step 1 of this comparative example is the same as step 1 of comparative example 2;
step 2, adding 239ml of concentrated hydrochloric acid with the mass fraction of 37% into 1.2L of boron concentrated solution to adjust the pH value of the boron concentrated solution to 4.5, cooling to normal temperature, and carrying out solid-liquid separation to obtain 139.37g of crude boric acid and 1.35L of boric acid mother solution, wherein the data of chemical compositions and the like of materials in each step in the comparative example are shown
Table 5.
TABLE 5
In this comparative example, the boron yield of the crude boric acid reached 56.75%.
Example 2:
the implementation process of this embodiment is the same as steps 1 and 2 in embodiment 1;
and step 3, taking 100g of crude boric acid, adding pure water according to the proportion of 1:1 for primary washing and secondary countercurrent washing, wherein the washing time is 0.5h, and returning the obtained secondary washing liquid to be used for primary washing according to the proportion of 1:1, so as to finally obtain 71.46g of wet boric acid and 0.108L of mother liquor. The data of the chemical composition of the materials and the like of each step in the embodiment are shown in Table 6.
TABLE 6
In the embodiment, the chlorine radical content in the wet boric acid is less than 0.050, and the standard of industrial boric acid first-class products is achieved.
Comparative example 5:
the procedure of this comparative example was the same as steps 1 and 2 in comparative example 1;
step 3, taking 152g of crude boric acid, adding pure water according to the proportion of 1:1 for washing for 0.5h to obtain 131.33g of wet boric acid and 0.195L of mother liquor;
and step 4, drying the wet boric acid at 85 ℃ for 2.5 hours to finally obtain 120.01g of refined boric acid. The data of the chemical composition of the materials and the like of each step in the comparative example are shown in Table 7.
TABLE 7
In the comparative example, the chlorine radical content in the refined boric acid is more than 0.10, and the standard of the industrial boric acid qualified product is not met.
Example 3:
step 1, taking B 2 O 3 The boron-rich solution with the concentration of 17.312g/L is forcedly evaporated and concentrated by an MVR evaporator to obtain B 2 O 3 A boron concentrate having a concentration of 177.685 g/L;
step 2, adding 329mg of 1:1 sulfuric acid into 2L of boron concentrate, adjusting the pH value of the boron concentrate to 1.5, cooling to normal temperature, and carrying out solid-liquid separation to obtain 470.87g of crude boric acid and 2L of boric acid mother liquor;
step 3 was the same as step 3 in example 2, and 78.41g of wet boric acid and 0.091L of a mother liquor were finally obtained. The data of the chemical composition of the materials and the like of each step in the embodiment are shown in Table 8.
TABLE 8
In the embodiment, the boron yield of the wet boric acid reaches 93.93%, the chloride content in the wet boric acid is less than 0.050, and the sulfate content is less than 0.60, so that the standard of industrial boric acid qualified products is achieved.
Comparative example 6:
the procedure of this comparative example was the same as steps 1 and 2 in example 3;
and step 3, taking 200g of crude boric acid, adding pure water according to the ratio of 1:1 for primary washing and secondary washing, wherein the washing time is 0.5h, and finally obtaining 152.55g of wet boric acid and 0.19L of mother liquor. The data of the chemical composition of the materials and the like of each step in this example are shown in Table 9.
TABLE 9
In the comparative example, the boron yield of the wet boric acid reaches 94.20 percent, and meanwhile, the chloride content in the wet boric acid is less than 0.050, but the sulfate content is more than 0.60, and the standard of the industrial boric acid qualified product is not reached.
Example 4:
step 1, taking B 2 O 3 The boron-rich solution with the concentration of 23.490g/L is forcedly evaporated and concentrated by an MVR evaporator to obtain B 2 O 3 A boron concentrate having a concentration of 159.010 g/L;
step 2, adding 175mg of concentrated hydrochloric acid with the mass fraction of 37% into 2.85L of boron concentrate, adjusting the pH value of the boron concentrate to 9.45, cooling to normal temperature, and carrying out solid-liquid separation to obtain 1136.1g of crude borax and 2.18L of borax mother solution;
step 3, adding pure water into 100g of crude borax according to the proportion of 1:1 for one-time washing, wherein the washing time is 0.5h, and 68.38g of wet borax and 0.107L of mother solution are obtained;
and 4, drying the wet borax at 80 ℃ for 2 hours to finally obtain 68.38g of dry borax. The data of the chemical composition of the materials and the like of each step in the comparative example are shown in Table 10.
Table 10
The boron yield of the embodiment reaches 80.63 percent and simultaneously reaches the industrial sodium tetraborate decahydrate standard.
In connection with examples 1 to 4, comparative examples 1 to 6, the following points can be seen:
(1) According to the process for preparing boric acid by combining the MVR boron concentrate provided by the application with the embodiments 1-3, the boron concentrate is obtained by forcibly evaporating the boron-rich solution through the MVR evaporator, the boron yield reaches more than 80% in the refined boric acid obtained through the processes of acid adding crystallization, countercurrent washing and separation drying, and the quality can meet the national standard of industrial boric acid, so that the boron extraction efficiency in magnesium sulfate subtype salt lake brine is improved.
(2) In the boron concentrate obtained by forced evaporation by the MVR evaporator, B in the boron concentrate of example 1 was obtained by comparing example 1 with comparative example 1 2 O 3 When the concentration is controlled between 140 and 145g/L, the yield of crude boron borate obtained by acid crystallization is highest; comparative example 1 boron concentrate B 2 O 3 The concentration is 127.924g/L, and the boron yield is relatively low, so that the concentration is higher, and the yield are higher when the concentration is higher, so that concentrated solutions with different concentrations are obtained through forced evaporation.
(3) By comparing example 1 with comparative examples 2 to 4, the pH value of the boron concentrate is adjusted to 1.5, 2.5, 3.5 and 4.5 by adding acid, and the lower the pH value is, the higher the yield of crude boron borate obtained by crystallization by adding acid is.
(4) By comparing the example 2 with the comparative example 5, the chlorine radical in the boric acid exceeds standard of qualified products after the crude boric acid is washed once; when the coarse boric acid is subjected to secondary countercurrent washing, the qualified chlorine borate can reach the standard of first grade.
(5) By comparing example 3 with comparative example 6, when boric acid is produced by adding sulfuric acid, the chloride in the crude boric acid can reach the standard of qualified products, but the sulfate radical exceeds the standard; the crude boric acid produced by adding sulfuric acid is washed twice by pure water, and the sulfate radical in the obtained wet boric acid has little change and is a defective product and a first grade product of chloride radical; when pure water is used for countercurrent secondary washing, sulfate radical can reach qualified products and chloride radical reaches first grade products.
(6) According to the process for preparing borax from the MVR boron concentrate, disclosed by the application, the boron concentrate is obtained by forcibly evaporating the boron-rich solution through the MVR evaporator, the PH value is regulated to about 9.45 by hydrochloric acid, and then the borax product is obtained by cooling to normal temperature and then separating, the boron yield reaches more than 80%, and the boron extraction efficiency in magnesium sulfate subtype salt lake brine is improved; the crude borax can basically reach the standard of the first grade sodium tetraborate decahydrate of the industry specified in the state after being washed and dried once.
The above embodiments are not intended to limit the scope of the present application, so: all equivalent changes in structure, shape and principle of the application should be covered in the scope of protection of the application.

Claims (8)

1. The method for preparing boric acid from MVR boron concentrate in the process of extracting lithium from salt lake is characterized by comprising the following steps:
step 1, taking a boron-rich solution as a raw material, and forcedly evaporating and concentrating by an MVR evaporator to obtain a boron concentrate, wherein B is the boron concentrate 2 O 3 The concentration is 100-150 g/L, wherein the boron-rich solution is mother solution obtained by separating lithium and magnesium from salt lake old brine through a membrane process, the mother solution enters a reverse osmosis membrane after being diluted so as to separate boron elements, the form of boron is changed through NaOH treatment, and then the solution is concentrated through the reverse osmosis membrane so as to obtain the boron-rich solution;
step 2, adding acid into the boron concentrated solution obtained in the step 1 to adjust the pH value to 1.5-4.5, then cooling the boron concentrated solution to normal temperature, and then performing solid-liquid separation to obtain crude boric acid and boric acid mother liquor, wherein the acid adding amount of each 1L of the boron concentrated solution is 205-292 ml;
step 3, performing primary washing and secondary washing on the crude boric acid obtained in the step 2 to obtain wet boric acid, wherein the primary washing mode is that washing liquid and the crude boric acid are added according to the proportion of 1:1-1:1.5, the washing time is 0.5h, the secondary washing mode is that countercurrent washing is performed, pure water and the crude boric acid are added according to the proportion of 1:1, and the washing time is 0.5h, and the obtained secondary washing liquid enters the primary washing as washing liquid;
and 4, the washed wet boric acid enters a drying treatment link. The wet boric acid is dried at a temperature of 85 ℃ for 2 to 2.5 hours to obtain the refined boric acid.
2. The method for preparing boric acid from MVR boron concentrate in a salt lake lithium extraction process according to claim 1, wherein the boron concentrate in the step 1 is B 2 O 3 The concentration is preferably 140 to 145g/L.
3. The method for preparing boric acid from MVR boron concentrate in a salt lake lithium extraction process according to any one of claims 1 or 2, wherein the acid added in step 2 is preferably any one of hydrochloric acid and sulfuric acid, and the pH value of the boron concentrate is preferably 1.5.
4. A method for preparing boric acid and borax from MVR boron concentrate in a salt lake lithium extraction process according to claim 3, wherein the hydrochloric acid is preferably concentrated hydrochloric acid with a mass fraction of 37%.
5. A method for producing boric acid from a concentrated solution of MVR boron in a salt lake according to claim 3 wherein the sulfuric acid is preferably a 1:1 sulfuric acid solution prepared with concentrated sulfuric acid.
6. The method for preparing boric acid from the concentrated solution of MVR boron in the lithium extraction process of salt lake according to any one of claims 1 to 5, wherein the ratio of the primary washing pure water to the crude boric acid in the step 3 is preferably 1:1.
7. The method for preparing boric acid from MVR boron concentrate in a salt lake lithium extraction process according to claim 6, wherein the crude boric acid in the step 3 is subjected to a secondary washing to obtain a secondary washing liquid, and the secondary washing liquid can be used for primary washing of the crude boric acid.
8. The method for preparing borax from MVR boron concentrate in the process of extracting lithium from salt lake is characterized by comprising the following steps:
step 1, taking a boron-rich solution as a raw material, and forcedly evaporating and concentrating through MVR to obtain a boron concentrate, wherein B of the boron concentrate 2 O 3 The concentration is 159g/L, the boron-rich solution is B obtained by separating lithium and magnesium from the old brine of the salt lake by a membrane process, diluting, separating boron by a reverse osmosis membrane, adding sodium hydroxide to change the form of boron, and continuing concentrating by the reverse osmosis membrane 2 O 3 A concentrate having a concentration of 17 g/L;
step 2, adding concentrated hydrochloric acid into the boron concentrated solution obtained in the step 1 to adjust the pH value to 9.45, then cooling the boron concentrated solution to normal temperature, separating out borax, and separating a solid-liquid phase to obtain crude borax and borax mother solution;
step 3, washing the crude borax obtained in the step 2 to obtain wet borax, wherein the washing mode is that pure water and the crude borax are added according to the proportion of 1:1-1:2, and washing is carried out for 0.5h;
and 4, drying the wet borax obtained in the step 3 at the drying temperature of 50-80 ℃ for 0.5-2 hours to obtain dry borax.
CN202311168278.5A 2023-09-12 2023-09-12 Method for preparing boric acid and borax from MVR boron concentrate in lithium extraction process of salt lake Pending CN117163968A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114917600A (en) * 2022-06-01 2022-08-19 启东神农机械有限公司 Evaporative crystallization process and device for producing borax from salt lake lithium extraction discharge liquid

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114917600A (en) * 2022-06-01 2022-08-19 启东神农机械有限公司 Evaporative crystallization process and device for producing borax from salt lake lithium extraction discharge liquid

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