CN111943229A - Method for preparing ultra-high-purity sodium hydroxide reagent by industrial caustic soda flake electrodialysis method - Google Patents
Method for preparing ultra-high-purity sodium hydroxide reagent by industrial caustic soda flake electrodialysis method Download PDFInfo
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- CN111943229A CN111943229A CN202010805447.1A CN202010805447A CN111943229A CN 111943229 A CN111943229 A CN 111943229A CN 202010805447 A CN202010805447 A CN 202010805447A CN 111943229 A CN111943229 A CN 111943229A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D1/00—Oxides or hydroxides of sodium, potassium or alkali metals in general
- C01D1/04—Hydroxides
- C01D1/28—Purification; Separation
- C01D1/38—Purification; Separation by dialysis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/42—Electrodialysis; Electro-osmosis ; Electro-ultrafiltration; Membrane capacitive deionization
- B01D61/422—Electrodialysis
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Abstract
The invention discloses a method for preparing an ultra-high-purity sodium hydroxide reagent by an industrial caustic soda flake electrodialysis method, which comprises the following steps of dissolving industrial caustic soda flakes in water to prepare high-concentration liquid caustic soda; the invention adopts the industrial caustic soda flakes as the raw material, and takes the ionic membrane as the separation membrane to carry out electrodialysis to produce the ultra-high-purity sodium hydroxide reagent, and the method for producing the ultra-high-purity sodium hydroxide reagent by carrying out electrodialysis by taking the ionic membrane as the separation membrane and adopting the industrial caustic soda flakes as the raw material is theoretically and practically feasible by referring to the production process of the sodium chloride solution ionic membrane electrolysis method for industrially producing the high-purity sodium hydroxide reagent. Compared with the absolute ethyl alcohol method, the method only releases hydrogen and oxygen, the separation and collection technology and equipment are mature, the production device is small, the safety coefficient and the production efficiency in the production of the ultra-high-purity sodium hydroxide reagent are increased, and meanwhile, the waste anolyte can be used for preparing a dissolving agent of high-concentration liquid caustic soda, so that the green and pollution-free production in the whole process is ensured.
Description
Technical Field
The invention relates to the technical field of chemical production, in particular to a method for preparing an ultra-high-purity sodium hydroxide reagent by an industrial caustic soda flake electrodialysis method.
Background
The ultra-pure sodium hydroxide is rare in the market, mainly Weke Germany is abroad, and only a small amount of Tianjin Kemiou is produced in China, so the price is high and the purchase is difficult. Can meet the requirements of a small amount of applications and can not provide enough supply for mass use. In order to meet the requirement of a large amount of ultra-high-purity sodium hydroxide required by the production of a certain special chemical product, the development of a novel method for preparing the ultra-high-purity sodium hydroxide at low cost is imperative.
At present, the absolute ethanol method is mainly used for purifying industrial caustic soda flakes to prepare the ultrahigh-purity sodium hydroxide, and the absolute ethanol method is used for purifying the industrial caustic soda flakes to effectively remove impurities and produce the ultrahigh-purity sodium hydroxide reagent. This method is not suitable for mass production of ultra-high purity sodium hydroxide.
Disclosure of Invention
In view of the problems in the prior art, the invention discloses a method which adopts the technical scheme that firstly, industrial caustic soda flakes are dissolved in water to prepare high-concentration liquid caustic soda; filtering the high-concentration liquid caustic soda, wherein the filtrate is purified liquid caustic soda; purifying the purified liquid caustic soda by electrodialysis to prepare an electrodialysis product, namely an ultra-high-purity sodium hydroxide reagent; and fourthly, filtering the low-concentration liquid caustic soda serving as the anolyte after electrodialysis, and returning the anolyte serving as the dissolving liquid for preparing the high-concentration liquid caustic soda.
As a preferred technical scheme of the invention, the first step is that firstly, industrial tablet alkali is dissolved in water to prepare high-concentration liquid alkali; the second step is that high-concentration liquid caustic soda is filtered, and the filtrate is purified liquid caustic soda; purifying the purified caustic soda liquid by electrodialysis to prepare an electrodialysis product, namely an ultra-high-purity sodium hydroxide reagent; and fourthly, filtering the low-concentration liquid caustic soda serving as the anolyte after the electrodialysis, and returning the anolyte serving as the dissolving liquid for preparing the high-concentration liquid caustic soda.
As a preferred technical scheme of the invention, the industrial tablet alkali is dissolved in water to prepare high-concentration liquid alkali, wherein the high-concentration liquid alkali comprises the following components: weighing the industrial caustic soda flakes and water according to the mass ratio of (1: 2-1: 4), and completely dissolving the industrial caustic soda flakes and the water under stirring to prepare high-concentration liquid caustic soda, wherein the mass concentration of the high-concentration liquid caustic soda is 20-33%.
As a preferred technical scheme of the present invention, the purified caustic soda liquid is purified by electrodialysis to prepare an electrodialysis product, that is, an ultra-high purity sodium hydroxide reagent is: filtering the high-concentration liquid caustic soda, wherein the filter medium is made of different materials, and comprises an alumina ceramic core, a quartz ceramic core and common filter paper, and the filtrate is purified high-concentration liquid caustic soda.
As a preferred technical scheme of the present invention, the anolyte after the electrodialysis is low-concentration caustic soda liquid, and is returned as a dissolving solution for preparing high-concentration caustic soda liquid after being filtered: and (3) taking the purified high-concentration liquid caustic soda as an anolyte, performing electrodialysis for 2.0-6.0 h at the temperature of 20-60 ℃, controlling the current to be 2.0-4.5A in the electrodialysis process, filtering the low-concentration liquid caustic soda serving as the anolyte after the electrodialysis, wherein the concentration of the low-concentration liquid caustic soda is 5-10%, and returning the low-concentration liquid caustic soda serving as a dissolving solution for preparing the high-concentration liquid caustic soda by using industrial caustic soda flakes.
As a preferable technical scheme of the invention, in the electrodialysis product, namely the high-purity sodium hydroxide reagent, the mass concentration of sodium hydroxide is between 15% and 25%, wherein the mass fractions of aluminum oxide, iron oxide, calcium oxide (wherein magnesium oxide is calculated by calcium oxide) and the like are all less than the requirements of the first-class products in GB/T1119-2006, and the first-class products are met.
The invention has the beneficial effects that: the invention adopts the industrial caustic soda flakes as the raw material, and takes the ionic membrane as the separation membrane to carry out electrodialysis to produce the ultra-high-purity sodium hydroxide reagent, and the method for producing the ultra-high-purity sodium hydroxide reagent by carrying out electrodialysis by taking the ionic membrane as the separation membrane and adopting the industrial caustic soda flakes as the raw material is theoretically and practically feasible by referring to the production process of the sodium chloride solution ionic membrane electrolysis method for industrially producing the high-purity sodium hydroxide reagent. Compared with the absolute ethyl alcohol method, the method only releases hydrogen and oxygen, the separation and collection technology and equipment are mature, the production device is small, the safety coefficient and the production efficiency in the production of the ultra-high-purity sodium hydroxide reagent are increased, and meanwhile, the waste anolyte can be used for preparing a dissolving agent of high-concentration liquid caustic soda, so that the green and pollution-free production in the whole process is ensured.
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FIG. 1 is a schematic view of the structure of the present invention.
Detailed Description
Example 1
As shown in figure 1, the invention discloses a method for preparing an ultra-high-purity sodium hydroxide reagent by an industrial caustic soda flake electrodialysis method, which adopts the technical scheme that the method comprises the following steps of (1) dissolving industrial caustic soda flake in water to prepare high-concentration caustic soda liquid; filtering the high-concentration liquid caustic soda, wherein the filtrate is purified liquid caustic soda; purifying the purified liquid caustic soda by electrodialysis to prepare an electrodialysis product, namely an ultra-high-purity sodium hydroxide reagent; and fourthly, filtering the low-concentration liquid caustic soda serving as the anolyte after electrodialysis, and returning the anolyte serving as the dissolving liquid for preparing the high-concentration liquid caustic soda.
As a preferred technical scheme of the invention, the first step is that firstly, industrial tablet alkali is dissolved in water to prepare high-concentration liquid alkali; the second step is that high-concentration liquid caustic soda is filtered, and the filtrate is purified liquid caustic soda; purifying the purified caustic soda liquid by electrodialysis to prepare an electrodialysis product, namely an ultra-high-purity sodium hydroxide reagent; and fourthly, filtering the low-concentration liquid caustic soda serving as the anolyte after the electrodialysis, and returning the anolyte serving as the dissolving liquid for preparing the high-concentration liquid caustic soda.
As a preferred technical scheme of the invention, the industrial tablet alkali is dissolved in water to prepare high-concentration liquid alkali, wherein the high-concentration liquid alkali comprises the following components: weighing industrial caustic soda flakes and water according to the mass ratio (1:2) and completely dissolving the industrial caustic soda flakes and the water under stirring to prepare high-concentration liquid caustic soda, wherein the mass concentration of the high-concentration liquid caustic soda is 20%.
As a preferred technical scheme of the present invention, the purified caustic soda liquid is purified by electrodialysis to prepare an electrodialysis product, that is, an ultra-high purity sodium hydroxide reagent is: filtering the high-concentration liquid caustic soda, wherein the filter medium is made of different materials, and comprises an alumina ceramic core, a quartz ceramic core and common filter paper, and the filtrate is purified high-concentration liquid caustic soda.
As a preferred technical scheme of the present invention, the anolyte after the electrodialysis is low-concentration caustic soda liquid, and is returned as a dissolving solution for preparing high-concentration caustic soda liquid after being filtered: and (3) taking the purified high-concentration liquid caustic soda as an anolyte, performing electrodialysis for 2.0h at 20 ℃, controlling the current to be 2.0A in the electrodialysis process, filtering the anolyte which is low-concentration liquid caustic soda with the concentration of 5 percent after the electrodialysis, and returning the anolyte to be used as a dissolving solution for preparing the high-concentration liquid caustic soda by using industrial caustic soda flakes.
As a preferable technical scheme of the invention, in the electrodialysis product, namely the high-purity sodium hydroxide reagent, the mass concentration of sodium hydroxide is 15%, wherein the mass fractions of aluminum oxide, iron oxide, calcium oxide (wherein magnesium oxide is calculated as calcium oxide) and the like are all less than the requirements of first-class products in GB/T1119-2006, and the first-class products are met.
Example 2
As shown in figure 1, the invention discloses a method for preparing an ultra-high-purity sodium hydroxide reagent by an industrial caustic soda flake electrodialysis method, which adopts the technical scheme that the method comprises the following steps of (1) dissolving industrial caustic soda flake in water to prepare high-concentration caustic soda liquid; filtering the high-concentration liquid caustic soda, wherein the filtrate is purified liquid caustic soda; purifying the purified liquid caustic soda by electrodialysis to prepare an electrodialysis product, namely an ultra-high-purity sodium hydroxide reagent; and fourthly, filtering the low-concentration liquid caustic soda serving as the anolyte after electrodialysis, and returning the anolyte serving as the dissolving liquid for preparing the high-concentration liquid caustic soda.
As a preferred technical scheme of the invention, the first step is that firstly, industrial tablet alkali is dissolved in water to prepare high-concentration liquid alkali; the second step is that high-concentration liquid caustic soda is filtered, and the filtrate is purified liquid caustic soda; purifying the purified caustic soda liquid by electrodialysis to prepare an electrodialysis product, namely an ultra-high-purity sodium hydroxide reagent; and fourthly, filtering the low-concentration liquid caustic soda serving as the anolyte after the electrodialysis, and returning the anolyte serving as the dissolving liquid for preparing the high-concentration liquid caustic soda.
As a preferred technical scheme of the invention, the industrial tablet alkali is dissolved in water to prepare high-concentration liquid alkali, wherein the high-concentration liquid alkali comprises the following components: weighing industrial caustic soda flakes and water according to the mass ratio (1: 4) and completely dissolving the industrial caustic soda flakes and the water under stirring to prepare high-concentration liquid caustic soda, wherein the mass concentration of the high-concentration liquid caustic soda is 33%.
As a preferred technical scheme of the present invention, the purified caustic soda liquid is purified by electrodialysis to prepare an electrodialysis product, that is, an ultra-high purity sodium hydroxide reagent is: filtering the high-concentration liquid caustic soda, wherein the filter medium is made of different materials, and comprises an alumina ceramic core, a quartz ceramic core and common filter paper, and the filtrate is purified high-concentration liquid caustic soda.
As a preferred technical scheme of the present invention, the anolyte after the electrodialysis is low-concentration caustic soda liquid, and is returned as a dissolving solution for preparing high-concentration caustic soda liquid after being filtered: and (3) taking the purified high-concentration liquid caustic soda as an anolyte, performing electrodialysis for 6.0h at 60 ℃, controlling the current to be 4.5A in the electrodialysis process, taking the anolyte after electrodialysis as low-concentration liquid caustic soda with the concentration of 10%, filtering, and returning to be used as a dissolving solution for preparing the high-concentration liquid caustic soda by using industrial caustic soda flakes.
As a preferable technical scheme of the invention, in the electrodialysis product, namely the high-purity sodium hydroxide reagent, the mass concentration of sodium hydroxide is 25%, wherein the mass fractions of aluminum oxide, iron oxide, calcium oxide (wherein the magnesium oxide is calculated as calcium oxide) and the like are all less than the requirements of the first-class product in GB/T1119-2006, and the first-class product requirement is met.
Components not described in detail herein are prior art.
Although the present invention has been described in detail with reference to the specific embodiments, the present invention is not limited to the above embodiments, and various changes and modifications without inventive changes may be made within the knowledge of those skilled in the art without departing from the spirit of the present invention.
Claims (6)
1. A method for preparing an ultra-high-purity sodium hydroxide reagent by an industrial caustic soda flake electrodialysis method is characterized by comprising the following steps of dissolving industrial caustic soda flakes in water to prepare high-concentration liquid caustic soda; filtering the high-concentration liquid caustic soda, wherein the filtrate is purified liquid caustic soda; purifying the purified liquid caustic soda by electrodialysis to prepare an electrodialysis product, namely an ultra-high-purity sodium hydroxide reagent; and fourthly, filtering the low-concentration liquid caustic soda serving as the anolyte after electrodialysis, and returning the anolyte serving as the dissolving liquid for preparing the high-concentration liquid caustic soda.
2. The method for preparing the ultra-high purity sodium hydroxide reagent by the industrial caustic soda flake electrodialysis method according to claim 1, wherein the method comprises the following steps: dissolving industrial tablet alkali in water to prepare high-concentration liquid alkali; the second step is that high-concentration liquid caustic soda is filtered, and the filtrate is purified liquid caustic soda; purifying the purified caustic soda liquid by electrodialysis to prepare an electrodialysis product, namely an ultra-high-purity sodium hydroxide reagent; and fourthly, filtering the low-concentration liquid caustic soda serving as the anolyte after the electrodialysis, and returning the anolyte serving as the dissolving liquid for preparing the high-concentration liquid caustic soda.
3. The method for preparing the ultra-high purity sodium hydroxide reagent by the industrial caustic soda flake electrodialysis method according to claim 1, wherein the method comprises the following steps: dissolving industrial tablets in alkali water to prepare high-concentration liquid alkali: weighing the industrial caustic soda flakes and water according to the mass ratio of (1: 2-1: 4), and completely dissolving the industrial caustic soda flakes and the water under stirring to prepare high-concentration liquid caustic soda, wherein the mass concentration of the high-concentration liquid caustic soda is 20-33%.
4. The method for preparing the ultra-high purity sodium hydroxide reagent by the industrial caustic soda flake electrodialysis method according to claim 1, wherein the method comprises the following steps: purifying the purified liquid caustic soda by adopting electrodialysis to prepare an electrodialysis product, wherein the ultra-pure sodium hydroxide reagent is as follows: filtering the high-concentration liquid caustic soda, wherein the filter medium is made of different materials, and comprises an alumina ceramic core, a quartz ceramic core and common filter paper, and the filtrate is purified high-concentration liquid caustic soda.
5. The method for preparing the ultra-high purity sodium hydroxide reagent by the industrial caustic soda flake electrodialysis method according to claim 1, wherein the method comprises the following steps: and fourthly, filtering the electrodialysis anode liquor which is low-concentration caustic soda liquid and returning the filtered anolyte to be used as a dissolving liquor for preparing high-concentration caustic soda liquid: and (3) taking the purified high-concentration liquid caustic soda as an anolyte, performing electrodialysis for 2.0-6.0 h at the temperature of 20-60 ℃, controlling the current to be 2.0-4.5A in the electrodialysis process, filtering the low-concentration liquid caustic soda serving as the anolyte after the electrodialysis, wherein the concentration of the low-concentration liquid caustic soda is 5-10%, and returning the low-concentration liquid caustic soda serving as a dissolving solution for preparing the high-concentration liquid caustic soda by using industrial caustic soda flakes.
6. The method for preparing the ultra-high purity sodium hydroxide reagent by the industrial caustic soda flake electrodialysis method according to claim 1, wherein the method comprises the following steps: in the electrodialysis product, namely the high-purity sodium hydroxide reagent, the mass concentration of sodium hydroxide is between 15% and 25%, wherein the mass fractions of aluminum oxide, ferric oxide, calcium oxide (wherein magnesium oxide is calculated by calcium oxide) and the like are all less than the requirements of first-class products in GB/T1119-2006, and the requirements of first-class products are met.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112758957A (en) * | 2020-12-28 | 2021-05-07 | 宜宾丝丽雅股份有限公司 | Process for purifying sodium hydroxide concentration by electrodialysis |
CN112853550A (en) * | 2020-12-28 | 2021-05-28 | 宜宾丝丽雅股份有限公司 | Treatment method for recycling alkali liquor |
CN113044863A (en) * | 2021-04-25 | 2021-06-29 | 百色学院 | Method for improving decomposition rate of seed precipitation in alumina production |
CN113045066A (en) * | 2021-03-26 | 2021-06-29 | 石增芹 | Preparation method of transparent negative ion liquid |
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CN104016388A (en) * | 2014-06-12 | 2014-09-03 | 合肥工业大学 | Separation method of alkaline liquid in production of alumina |
CN104016376A (en) * | 2014-06-25 | 2014-09-03 | 苏州晶瑞化学有限公司 | Continuous production method of high-purity potassium hydroxide water solution |
CN106890573A (en) * | 2015-12-21 | 2017-06-27 | 杭州水处理技术研究开发中心有限公司 | NaOH electrodialysis concentrates film group device |
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US5141610A (en) * | 1988-04-19 | 1992-08-25 | Vaughan Daniel J | Electrodialytic process for restoring sodium hydroxide etchants for aluminum |
CN104016388A (en) * | 2014-06-12 | 2014-09-03 | 合肥工业大学 | Separation method of alkaline liquid in production of alumina |
CN104016376A (en) * | 2014-06-25 | 2014-09-03 | 苏州晶瑞化学有限公司 | Continuous production method of high-purity potassium hydroxide water solution |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112758957A (en) * | 2020-12-28 | 2021-05-07 | 宜宾丝丽雅股份有限公司 | Process for purifying sodium hydroxide concentration by electrodialysis |
CN112853550A (en) * | 2020-12-28 | 2021-05-28 | 宜宾丝丽雅股份有限公司 | Treatment method for recycling alkali liquor |
CN113045066A (en) * | 2021-03-26 | 2021-06-29 | 石增芹 | Preparation method of transparent negative ion liquid |
CN113044863A (en) * | 2021-04-25 | 2021-06-29 | 百色学院 | Method for improving decomposition rate of seed precipitation in alumina production |
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