CN113666390A - Method for preparing ionic membrane caustic soda raw material brine by using fused salt chlorination residues - Google Patents
Method for preparing ionic membrane caustic soda raw material brine by using fused salt chlorination residues Download PDFInfo
- Publication number
- CN113666390A CN113666390A CN202111008807.6A CN202111008807A CN113666390A CN 113666390 A CN113666390 A CN 113666390A CN 202111008807 A CN202111008807 A CN 202111008807A CN 113666390 A CN113666390 A CN 113666390A
- Authority
- CN
- China
- Prior art keywords
- brine
- caustic soda
- preparing
- raw
- ionic membrane
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 title claims abstract description 117
- 239000012267 brine Substances 0.000 title claims abstract description 99
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 title claims abstract description 88
- 150000003839 salts Chemical class 0.000 title claims abstract description 62
- 235000011121 sodium hydroxide Nutrition 0.000 title claims abstract description 39
- 238000005660 chlorination reaction Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000012528 membrane Substances 0.000 title claims abstract description 27
- 239000002994 raw material Substances 0.000 title claims abstract description 14
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 54
- 239000000243 solution Substances 0.000 claims abstract description 34
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 28
- 239000011780 sodium chloride Substances 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000002893 slag Substances 0.000 claims abstract description 21
- 239000003513 alkali Substances 0.000 claims abstract description 19
- 238000001914 filtration Methods 0.000 claims abstract description 18
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 15
- 239000000706 filtrate Substances 0.000 claims abstract description 14
- 239000007800 oxidant agent Substances 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 230000001590 oxidative effect Effects 0.000 claims abstract description 12
- 238000002386 leaching Methods 0.000 claims abstract description 11
- 239000008267 milk Substances 0.000 claims abstract description 10
- 235000013336 milk Nutrition 0.000 claims abstract description 10
- 210000004080 milk Anatomy 0.000 claims abstract description 10
- 238000001556 precipitation Methods 0.000 claims abstract description 8
- 239000006228 supernatant Substances 0.000 claims abstract description 8
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 5
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 5
- 235000011116 calcium hydroxide Nutrition 0.000 claims abstract description 5
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000011575 calcium Substances 0.000 claims description 13
- 229910052749 magnesium Inorganic materials 0.000 claims description 10
- 239000004571 lime Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 7
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 7
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 7
- 229910052791 calcium Inorganic materials 0.000 claims description 7
- 239000000460 chlorine Substances 0.000 claims description 7
- 229910052801 chlorine Inorganic materials 0.000 claims description 7
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical group [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000012047 saturated solution Substances 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 150000002500 ions Chemical class 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 4
- 238000004064 recycling Methods 0.000 abstract description 3
- -1 salt chloride Chemical class 0.000 abstract description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 abstract description 2
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 239000011777 magnesium Substances 0.000 description 12
- 239000000203 mixture Substances 0.000 description 7
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000010936 titanium Substances 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000008399 tap water Substances 0.000 description 2
- 235000020679 tap water Nutrition 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910006130 SO4 Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910003074 TiCl4 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000003841 chloride salts Chemical class 0.000 description 1
- 230000009194 climbing Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 235000010215 titanium dioxide Nutrition 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
- C01D3/16—Purification by precipitation or adsorption
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a method for preparing ionic membrane caustic soda raw material brine by using molten salt chlorination residues, and belongs to the technical field of waste salt treatment and resource recycling in the titanium tetrachloride production field. The method comprises the following steps: a. leaching the fused salt chloride slag to obtain crude salt water; b. adding mixed alkali and an oxidant, precipitating and filtering after complete reaction to obtain mixed brine; c. heating to 90-95 ℃, adding a sodium carbonate solution in time, standing after complete reaction, and filtering to obtain NaCl brine; d. adding slaked lime milk or Ca (OH) to NaCl brine2Standing for precipitation and filtering after reaction; adding raw salt into the filtrate, or increasing the NaCl content in the brine to 305-315 g/l by adopting a concentration method, settling and clarifying, wherein the supernatant is the raw brine produced by the ion membrane caustic soda. The method provides an effective way for treating the molten salt chlorination slag, and also provides a new qualified source for the ionic membrane caustic soda raw material brine.
Description
Technical Field
The invention belongs to the technical field of waste salt treatment and resource recycling in the titanium tetrachloride production field, and particularly relates to a method for preparing ionic membrane caustic soda raw material brine by using molten salt chlorination residues.
Background
About 80 percent of global titanium resources are primary titanium ores, 95 percent of the national titanium resources are primary titanium ores, and the primary titanium ores (such as Panxi vanadium titano-magnetite) are used asTitanium slag smelted from initial resources is generally high in calcium and magnesium (MgO + CaO is more than or equal to 7 percent) and TiO2Low grade (74-76 percent), can not be used as raw materials for boiling chlorination production, and only can adopt a molten salt chlorination method to produce TiCl4Further producing sponge titanium and titanium white chloride. Years of production practice of climbing steel group shows that TiCl produced by molten salt chlorination4The cost of the method is 30 percent lower than that of boiling chlorination. But the production amount of the waste salt and the molten salt chlorination slag of the molten salt chlorination is large, the components are complex, and the treatment and the utilization are difficult. At present, the treatment is generally carried out at home and abroad by adopting a filling cooling-crushing-lime mixing special slag yard landfill mode, and more than 80 percent of components of the treatment are soluble metal chlorides, so that the risk of pollution to soil and underground water is great. Once the country prohibits landfills, the enterprise is at risk of a shutdown. Therefore, the recycling treatment of the fused salt chlorination residues becomes a 'bottleneck' technical problem for the survival and development of the fused salt chlorination process, and needs to be solved urgently.
Disclosure of Invention
The invention aims to solve the technical problem that the existing molten salt chlorination slag treatment mode pollutes the environment, provides a method for directly preparing brine meeting the ionic membrane caustic soda primary brine standard by using molten salt chlorination slag, and relieves the problem of molten salt chlorination slag treatment.
The technical scheme adopted by the invention for solving the technical problems is as follows: a method for preparing ionic membrane caustic soda raw material brine by using fused salt chlorination residues comprises the following steps:
a. leaching: leaching the fused salt chlorination residues with water, and filtering after complete leaching to obtain crude salt water;
b. preparing mixed brine: adding mixed alkali and oxidant into the crude brine under stirring, wherein the mixed alkali is Na2CO3And NaOH, wherein the oxidant is NaClO solution, and after complete reaction, the mixed salt water is obtained through precipitation and filtration;
c. preparing NaCl brine: heating the mixed brine to 90-95 ℃, adding a sodium carbonate solution in time, stirring at a constant temperature, standing after complete reaction, and filtering to obtain NaCl brine;
d. preparing raw material brine of ionic membrane caustic soda: adding slaked lime milk or Ca (OH) to NaCl brine2Standing for precipitation and filtering after reaction; filter with filter elementAdding raw salt into the solution, increasing the NaCl content in the brine to 305-315 g/l, settling and clarifying, wherein the supernatant is the raw brine produced by the ionic membrane caustic soda; or increasing the NaCl concentration of the filtrate to 305-315 g/l by adopting a concentration method.
Wherein, in the step b of the method, the content of active chlorine in the oxidant>6 g/l; the mixed alkali is a solution with the mass concentration of 30 percent, and Na is contained in the mixed alkali2CO3The mass ratio of the NaOH solution to the NaOH solution is 1: 1-5.
Furthermore, the volume ratio of the crude brine to the mixed alkali to the oxidant is 1: 0.2-1.2: 0.1-0.2.
And further, in the step b, the reaction time is more than or equal to 10 hours.
Wherein, in the method, the sodium carbonate solution is saturated solution, and the adding amount is according to the ratio of sodium carbonate in the solution to Mg in the mixed brine2+The molar ratio of the raw materials is 1.0-1.2: 1.0.
In the step a of the method, the mass ratio of the molten salt chlorination residues to the water is 1: 1-5.
In the step d of the method, the mass concentration of the lime milk is 10-21%.
Wherein in the step d of the method, lime milk or Ca (OH)2The dosage of the water is according to the CO in the brine3 2-The content is determined, and the molar ratio of the added calcium to the carbonate in the salt water is 0.95-1.0: 1.0.
Wherein, in the step d of the method, the precipitation time is more than or equal to 2 hours.
Wherein in the step d of the method, the used raw salt comprises more than or equal to 95 percent of NaCl, less than or equal to 1.0 percent of Ca and Mg, and SO4 2-Not more than 0.5 percent, and the dissolution temperature is 55 +/-2 ℃, which are mass contents.
The invention has the beneficial effects that: the method comprises the steps of firstly, leaching the fused salt chloride slag, adding mixed alkali and an oxidant, and deeply removing ammonium, F, Fe, Mn and other ions in crude brine, wherein the ammonium is<0.1mg/l、F<0.1mg/l、Fe<1mg/l、Mn<1 mg/l; adding saturated sodium carbonate solution to make Mg2+Less than 60 mg/l; adding lime milk or slaked lime to make CO in salt water3 2-Less than or equal to 0.5 g/l. The purified brine is supplemented with original salt or concentrated to prepare composite saltThe starting material for the biofilm caustic soda requirement is virgin (saturated brine).
Detailed Description
The process of the invention can be carried out in particular in the following manner.
A method for preparing ionic membrane caustic soda raw material brine by using fused salt chlorination residues comprises the following steps:
a. leaching: dissolving and leaching the fused salt chlorination residues with water according to the mass ratio of 1: 1-5, and filtering after complete dissolution and leaching to obtain crude salt water;
b. preparing mixed brine: adding a mixed alkali solution with the mass concentration of 30 percent and an oxidant into the crude brine under stirring, wherein the mixed alkali solution is Na2CO3And NaOH solution, Na2CO3The mass ratio of the active chlorine to NaOH is 1: 1-5, and the oxidant is active chlorine content>6g/l of NaClO solution, the volume ratio of the crude salt water to the mixed alkali solution to the oxidant is 1: 0.2-1.2: 0.1-0.2, and after the reaction is over 10 hours, the mixed salt water is precipitated and filtered to obtain the mixed salt water;
c. preparing NaCl brine: heating the mixed salt water to 90-95 ℃, adding saturated sodium carbonate solution in time, wherein the adding amount is according to the ratio of sodium carbonate in the solution to Mg in the mixed salt water2+Adding the materials according to the molar ratio of 1.0-1.2: 1.0, stirring at constant temperature, standing after complete reaction, and filtering to obtain NaCl brine;
d. preparing raw material brine of ionic membrane caustic soda: adding slaked lime milk or Ca (OH) to NaCl brine2The dosage is according to CO in the brine3 2-The content is determined, and the molar ratio of the added calcium to the carbonate in the salt water is 0.95-1.0: 1.0; standing for more than 2h, and filtering; adding raw salt into the filtrate (brine), increasing the NaCl content in the brine to 305-315 g/l, settling and clarifying, wherein the supernatant is the raw brine produced by the ion membrane caustic soda; concentration may also be used to increase the NaCl concentration of the brine to 315 g/l.
The present invention will be further described with reference to the following examples, but the scope of the present invention is not limited thereto.
Example one
Taking 1 kg of fused salt chlorination slag, crushing (the diameter of the slag is less than or equal to 2.5cm), adding2.5L of tap water was added, stirred and dissolved. After the molten salt chlorination residues are completely dissolved, filtering to obtain 2.22L crude salt water, wherein the specific components are shown in Table 1. Slowly adding 1.198L of 30% mixed alkali solution containing Na2CO3The solution was mixed with NaOH at a mass ratio of 1: 2, and 200mL of NaClO solution having an active chlorine content of 16g/L was added thereto to effect a complete reaction for 48 hours, followed by precipitation and filtration to obtain 2.94L of mixed brine (water quality shown in Table 2). Adding Mg into mixed brine2+Reacting saturated sodium carbonate solution with a molar ratio of 1.1 at 95 ℃ for 40min, settling, clarifying, and filtering supernatant to obtain 2.82L filtrate, namely magnesium-removed NaCl brine (see Table 3). 73g of digested lime milk with a concentration of 20% was added to the magnesium-removed brine, stirred well, reacted for 4h, and 2.79L of the filtrate was filtered, the filtrate composition being shown in Table 4. And (3) keeping the temperature of the filtrate at 55 ℃, adding 314.4g of industrial salt with the purity of 98.5% into the filtrate under the stirring condition, fully stirring the mixture to completely dissolve the salt, standing the mixture for 4 hours to obtain a supernatant, namely NaCl315g/l saturated saline meeting the requirements of the ionic membrane caustic soda production process, wherein the analysis results are shown in Table 5.
Table 1 example a crude brine analysis result
Table 2 example-mixed brine analysis results
Table 3 example a result of analysis of a magnesium-depleted NaCl brine
Table 4 example a further purified NaCl brine analysis results
Table 5 analysis results of saturated brine prepared in example one
Example two
1 kg of waste molten chloride salt was similarly quenched with 2.2L of tap water, and filtered to obtain 2.02L of crude brine (see Table 6). Slowly adding 1.30L of 30% mixed alkali solution containing Na2CO3The mass ratio of the solution to NaOH was 1: 2, 270mL of NaClO solution having an active chlorine content of 12g/L was added thereto, the mixture was allowed to react for 24 hours, and the precipitate was filtered to obtain 3.12L of mixed brine (water quality shown in Table 7). Adding Mg into mixed brine2+Reacting saturated sodium carbonate solution with a molar ratio of 1.09 at 92 ℃ for 40min, clarifying the precipitate, and filtering the supernatant to obtain filtrate, namely the magnesium-removed NaCl brine (see Table 8). 103g of digested lime cream with a concentration of 16% was added to the magnesium-removed brine, stirred well, reacted for 4 hours, and 2.68L of filtrate was filtered, the filtrate composition being shown in Table 9. The filtrate was evaporated until a small amount of crystals appeared and cooled to room temperature, and the supernatant was saturated NaCl brine (see table 10 for analytical results).
TABLE 6 example II crude brine analysis results
Table 7 example two mixed brine analysis results
TABLE 8 example two magnesium removal NaCl brine analysis results
Table 9 analysis of NaCl brine from example two further purification
Table 10 analysis results of saturated brine prepared in example two
Comparative example 1
Crude brine is prepared by the same method as the example one, mixed alkali is not added when the crude brine is prepared into mixed brine, only NaOH is added, the adding ratio of alkali liquor to crude brine is (V/V is 0.65:1), and Ca in the prepared mixed brine is added2+、Mg2+Almost all enter the solution, the slag phase is difficult to filter due to low content of Mg and Ca salts, and the composition is shown in Table 11.
Table 11 comparative example-mixed brine analysis results
Comparative example No. two
Crude brine and mixed brine were prepared in the same manner as in example one, except that if the active chlorine in the oxidizing agent was too low, e.g., 2g/l, NH was added to the prepared mixed brine4 +、F-And the contents of TFe and Mn are too high, and TFe and NH in the prepared brine are obtained after the mixed brine is continuously subjected to magnesium and carbonate removal4 +、F-The content of the active carbon is less than 1 mg/l. The brine composition is shown in table 12.
Table 12 analysis results of mixed brine of comparative example
Comparative example three:
crude brine and mixed brine were prepared in the same manner as in example one, except that the mixed brine had a magnesium removal temperature of 70 ℃ and Mg was contained in the magnesium removal brine2+682Mg/l higher than Mg in ion membrane caustic soda saturated brine2+Less than or equal to 500 mg/l.
TABLE 13 analysis results of the triple magnesium-removed brine of comparative example
Claims (10)
1. A method for preparing ionic membrane caustic soda raw material brine by using fused salt chlorination residues is characterized by comprising the following steps:
a. leaching: leaching the fused salt chlorination residues with water, and filtering after complete leaching to obtain crude salt water;
b. preparing mixed brine: adding mixed alkali and oxidant into the crude brine under stirring, wherein the mixed alkali is Na2CO3And NaOH, wherein the oxidant is NaClO solution, and after complete reaction, the mixed salt water is obtained through precipitation and filtration;
c. preparing NaCl brine: heating the mixed brine to 90-95 ℃, adding a sodium carbonate solution in time, stirring at a constant temperature, standing after complete reaction, and filtering to obtain NaCl brine;
d. preparing raw material brine of ionic membrane caustic soda: adding slaked lime milk or Ca (OH) to NaCl brine2Standing for precipitation and filtering after reaction; adding raw salt into the filtrate, increasing the NaCl content in the brine to 305-315 g/l, settling and clarifying, wherein the supernatant is the raw brine produced by the ionic membrane caustic soda; or increasing the NaCl concentration of the filtrate to 305-315 g/l by adopting a concentration method.
2. The method for preparing the raw brine of the ionic membrane caustic soda by using the molten salt chlorination slag as claimed in claim 1, is characterized in that: in step b, the content of active chlorine in the oxidizing agent>6 g/l; the mixed alkali is a solution with the mass concentration of 30 percent, and Na is contained in the mixed alkali2CO3The mass ratio of the NaOH solution to the NaOH solution is 1: 1-5.
3. The method for preparing the raw brine of the ionic membrane caustic soda by using the molten salt chlorination slag as claimed in claim 2, is characterized in that: the volume ratio of the crude brine to the mixed alkali to the oxidant is 1: 0.2-1.2: 0.1-0.2.
4. The method for preparing the raw brine of the ionic membrane caustic soda by using the molten salt chlorination slag as claimed in claim 3, is characterized in that: in the step b, the reaction time is more than or equal to 10 hours.
5. The method for preparing the raw brine of the ionic membrane caustic soda by using the molten salt chlorination slag as claimed in claim 1, is characterized in that: the sodium carbonate solution is saturated solution, and the adding amount of the sodium carbonate solution and Mg in the mixed brine are according to the ratio of sodium carbonate in the solution to Mg in the mixed brine2+The molar ratio of the raw materials is 1.0-1.2: 1.0.
6. The method for preparing the raw brine of the ionic membrane caustic soda by using the molten salt chlorination slag as claimed in claim 1, is characterized in that: in the step a, the mass ratio of the molten salt chlorination residues to the water is 1: 1-5.
7. The method for preparing the raw brine of the ionic membrane caustic soda by using the molten salt chlorination slag as claimed in claim 1, is characterized in that: in the step d, the mass concentration of the lime milk is 10-21%.
8. The method for preparing the raw brine of the ionic membrane caustic soda by using the molten salt chlorination slag as claimed in claim 1, is characterized in that: in step d, lime milk or Ca (OH)2The dosage of the water is according to the CO in the brine3 2-The content is determined, and the molar ratio of the added calcium to the carbonate in the salt water is 0.95-1.0: 1.0.
9. The method for preparing the raw brine of the ionic membrane caustic soda by using the molten salt chlorination slag as claimed in claim 8, is characterized in that: in the step d, the precipitation time is more than or equal to 2 hours.
10. The method for preparing the raw brine of the ionic membrane caustic soda by using the molten salt chlorination slag as claimed in claim 1, is characterized in that: the raw salt used in the step d is that the NaCl content is more than or equal to 95 percent, the total content of Ca and Mg is less than or equal to 1.0 percent,SO4 2-Less than or equal to 0.5 percent and the dissolution temperature is 55 +/-2 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111008807.6A CN113666390A (en) | 2021-08-31 | 2021-08-31 | Method for preparing ionic membrane caustic soda raw material brine by using fused salt chlorination residues |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111008807.6A CN113666390A (en) | 2021-08-31 | 2021-08-31 | Method for preparing ionic membrane caustic soda raw material brine by using fused salt chlorination residues |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113666390A true CN113666390A (en) | 2021-11-19 |
Family
ID=78547766
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111008807.6A Pending CN113666390A (en) | 2021-08-31 | 2021-08-31 | Method for preparing ionic membrane caustic soda raw material brine by using fused salt chlorination residues |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113666390A (en) |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2096507C1 (en) * | 1996-04-11 | 1997-11-20 | Акционерное общество "Иргиредмет" | Method of processing chloride slag containing precious metals |
| FR2866870A1 (en) * | 2004-02-26 | 2005-09-02 | Goux Jean Yves Le | Preparation of crystallized sodium chloride (NaCl) from brines, used in conditioning salts, comprises eliminating magnesium; producing sodium carbonate; crystallizing-evaporating NaCl; precipitating sulfates; and eliminating excess calcium |
| CN101343070A (en) * | 2008-08-28 | 2009-01-14 | 攀钢集团钛业有限责任公司 | Waste molten salt treatment method |
| CN102718233A (en) * | 2011-12-15 | 2012-10-10 | 沈阳化工大学 | Method for combined treatment on chlorinated waste molten salts and Cl-containing waste water |
| CN102923736A (en) * | 2012-10-22 | 2013-02-13 | 戈尔工业品贸易（上海）有限公司 | Processing method for refining industrial brine |
| CN103011203A (en) * | 2012-12-07 | 2013-04-03 | 沈阳化工大学 | Method for treatment of chlorinated waste molten salt generated in TiCl4 production process |
| CN103566719A (en) * | 2013-10-28 | 2014-02-12 | 沈阳化工大学 | Method for preparing raw material of desulfurizing agent by using waste chlorination molten salt generated in production of TiCl4 |
| CN105883911A (en) * | 2016-04-07 | 2016-08-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Resourceful treatment method for fused salt chlorination residues |
| CN107164637A (en) * | 2017-06-30 | 2017-09-15 | 江苏省冶金设计院有限公司 | The system and method for handling titanium dioxide fused salt chlorimation abraum salt |
| CN110372017A (en) * | 2019-08-30 | 2019-10-25 | 河北工业大学 | Bittern mixes the separation method that alkaline process prepares basic magnesium carbonate and its natrium potassium salt |
| CN113213510A (en) * | 2021-04-26 | 2021-08-06 | 攀钢集团攀枝花钛材有限公司 | Method for treating waste salt generated by chlorination of molten salt |
-
2021
- 2021-08-31 CN CN202111008807.6A patent/CN113666390A/en active Pending
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2096507C1 (en) * | 1996-04-11 | 1997-11-20 | Акционерное общество "Иргиредмет" | Method of processing chloride slag containing precious metals |
| FR2866870A1 (en) * | 2004-02-26 | 2005-09-02 | Goux Jean Yves Le | Preparation of crystallized sodium chloride (NaCl) from brines, used in conditioning salts, comprises eliminating magnesium; producing sodium carbonate; crystallizing-evaporating NaCl; precipitating sulfates; and eliminating excess calcium |
| CN101343070A (en) * | 2008-08-28 | 2009-01-14 | 攀钢集团钛业有限责任公司 | Waste molten salt treatment method |
| CN102718233A (en) * | 2011-12-15 | 2012-10-10 | 沈阳化工大学 | Method for combined treatment on chlorinated waste molten salts and Cl-containing waste water |
| CN102923736A (en) * | 2012-10-22 | 2013-02-13 | 戈尔工业品贸易（上海）有限公司 | Processing method for refining industrial brine |
| CN103011203A (en) * | 2012-12-07 | 2013-04-03 | 沈阳化工大学 | Method for treatment of chlorinated waste molten salt generated in TiCl4 production process |
| CN103566719A (en) * | 2013-10-28 | 2014-02-12 | 沈阳化工大学 | Method for preparing raw material of desulfurizing agent by using waste chlorination molten salt generated in production of TiCl4 |
| CN105883911A (en) * | 2016-04-07 | 2016-08-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Resourceful treatment method for fused salt chlorination residues |
| WO2017174012A1 (en) * | 2016-04-07 | 2017-10-12 | 攀钢集团攀枝花钢铁研究院有限公司 | Molten-salt chlorinated-slag resource processing method |
| CN107164637A (en) * | 2017-06-30 | 2017-09-15 | 江苏省冶金设计院有限公司 | The system and method for handling titanium dioxide fused salt chlorimation abraum salt |
| CN110372017A (en) * | 2019-08-30 | 2019-10-25 | 河北工业大学 | Bittern mixes the separation method that alkaline process prepares basic magnesium carbonate and its natrium potassium salt |
| CN113213510A (en) * | 2021-04-26 | 2021-08-06 | 攀钢集团攀枝花钛材有限公司 | Method for treating waste salt generated by chlorination of molten salt |
Non-Patent Citations (1)
| Title |
|---|
| 刘够生等: "察尔汗盐湖尾盐氯化钠"二段除铵"工艺研究", 《盐业与化工》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105883911B (en) | Fused salt chlorimation slag recycling processing method | |
| CN105129822B (en) | System and method for treating chlor-alkali production byproduct salt mud | |
| CN106044799B (en) | Titanium chloride slag and its method for comprehensive utilization of filtrate in chloride process titanium dioxide powder craft | |
| US6143260A (en) | Method for removing magnesium from brine to yield lithium carbonate | |
| CN113582224B (en) | Resource utilization method for titanium white waste acid leaching fused salt chlorination slag | |
| US7462337B2 (en) | Recovery of titanium dioxide from titanium oxide bearing materials like steelmaking slags | |
| CN113816399A (en) | Method for recycling NaCl and recycling Fe, Mn and Mg resources in titanium slag | |
| CN107500352A (en) | A kind of method that low-temperature precipitation produces high-purity ammonium vanadate | |
| CN108911237A (en) | The method of sodium vanadium extracting waste water resource utilization | |
| CN110304703A (en) | A kind of preparation method with aluminium ash production polyaluminium chloride water purification agent | |
| CN101760637B (en) | Leaching technology of magnesium-containing ore | |
| CN109694092B (en) | Comprehensive treatment method for chlorine-containing solid waste | |
| CN111620481B (en) | Recycling treatment method of industrial wastewater containing chlorine and arsenic | |
| CN105883884A (en) | Method for preparing industrial calcium chloride from thiourea waste residues | |
| CN106746402B (en) | Method for treating arsenic-removing sludge | |
| CN112299448A (en) | Method for recovering sodium chloride from titanium white molten salt slag by chlorination process | |
| CN113800549A (en) | Method for extracting barium chloride from precipitated barium sulfate waste residue | |
| CN113666390A (en) | Method for preparing ionic membrane caustic soda raw material brine by using fused salt chlorination residues | |
| JP2003105457A (en) | Method for separating and recovering titanium oxide and iron oxide from titanium-containing concentrate | |
| US4200618A (en) | Preparation of magnesium chloride | |
| CN113336244A (en) | Method for removing ammonium from brine prepared from waste chlorination residues for ionic membrane caustic soda | |
| WO2005068358A1 (en) | Production of 'useful material(s)' from waste acid issued from the production of titanium dioxyde | |
| CN111498870A (en) | Method for treating sintering machine head ash in steel mill by using chemical production byproduct potassium carbonate | |
| WO2024040703A1 (en) | Resource utilization method for crude sodium sulfate | |
| JP2021008385A (en) | Method for producing zinc carbonate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20211119 |