CN117019086A - Adsorbent suitable for purifying thionyl chloride and purification method - Google Patents
Adsorbent suitable for purifying thionyl chloride and purification method Download PDFInfo
- Publication number
- CN117019086A CN117019086A CN202311003732.1A CN202311003732A CN117019086A CN 117019086 A CN117019086 A CN 117019086A CN 202311003732 A CN202311003732 A CN 202311003732A CN 117019086 A CN117019086 A CN 117019086A
- Authority
- CN
- China
- Prior art keywords
- adsorbent
- thionyl chloride
- purifying
- boehmite
- powder
- 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
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 239000003463 adsorbent Substances 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims description 16
- 238000000746 purification Methods 0.000 title description 3
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 52
- 239000000843 powder Substances 0.000 claims abstract description 49
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims abstract description 44
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000007789 gas Substances 0.000 claims abstract description 30
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 26
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000010457 zeolite Substances 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910001593 boehmite Inorganic materials 0.000 claims abstract description 23
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims abstract description 23
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims abstract description 19
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000001125 extrusion Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- 238000002791 soaking Methods 0.000 claims abstract description 3
- 239000000047 product Substances 0.000 claims description 14
- 239000012043 crude product Substances 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 claims description 2
- -1 sulfone chloride Chemical class 0.000 abstract description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052742 iron Inorganic materials 0.000 abstract description 9
- 238000002360 preparation method Methods 0.000 abstract description 8
- 230000000052 comparative effect Effects 0.000 description 7
- YBBRCQOCSYXUOC-UHFFFAOYSA-N sulfuryl dichloride Chemical compound ClS(Cl)(=O)=O YBBRCQOCSYXUOC-UHFFFAOYSA-N 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 229910052717 sulfur Inorganic materials 0.000 description 6
- 239000011593 sulfur Substances 0.000 description 6
- 238000009423 ventilation Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- RFZUPEMRDGRJCR-UHFFFAOYSA-K [Al](Cl)(Cl)Cl.[S] Chemical compound [Al](Cl)(Cl)Cl.[S] RFZUPEMRDGRJCR-UHFFFAOYSA-K 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000012798 spherical particle Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 150000001263 acyl chlorides Chemical class 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- PXJJSXABGXMUSU-UHFFFAOYSA-N disulfur dichloride Chemical compound ClSSCl PXJJSXABGXMUSU-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000011555 saturated liquid Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
- FWMUJAIKEJWSSY-UHFFFAOYSA-N sulfur dichloride Chemical compound ClSCl FWMUJAIKEJWSSY-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/165—Natural alumino-silicates, e.g. zeolites
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The application provides an adsorbent suitable for purifying thionyl chloride. The preparation method of the adsorbent comprises dispersing boehmite powder in water, adding citric acid, heating and stirring, filtering, and vacuum drying; soaking zeolite powder in an aluminum chloride solution, filtering, and introducing sulfur dioxide and hydrogen sulfide gas at 35-40 ℃; mixing the treated boehmite powder, zeolite powder, pseudo-boehmite and water, and performing extrusion molding to obtain the adsorbent. The adsorbent of the application can conveniently reduce the content of sulfone chloride and the content of iron ions in the thionyl chloride product, and is easy to separate from the product.
Description
Technical Field
The application relates to the field of thionyl chloride production, in particular to an adsorbent suitable for purifying thionyl chloride and a purification method.
Background
The sulfoxide chloride is a colorless or yellow liquid inorganic compound, has strong pungent smell, can be mixed in benzene, chloroform, carbon tetrachloride and other organic solvents, is hydrolyzed by water and is decomposed by heating, and is mainly used for preparing acyl chloride and also used for producing pesticides, medicines, dyes and the like. In recent years, with the development of new energy automobile technology, it is found that thionyl chloride can be used as a raw material of electrolyte solute of a power lithium battery, so that the production of thionyl chloride is highly focused by mass enterprises, and people want to obtain bonus in new energy batteries and new energy automobile industries.
At present, domestic enterprises generally adopt a sulfur dioxide gas phase method to produce thionyl chloride, sulfuryl chloride cannot be avoided in the production process of the method, the boiling point of thionyl chloride (78.8 ℃) is very close to that of sulfuryl chloride (69 ℃), the thionyl chloride and the sulfuryl chloride are difficult to be thoroughly separated in a conventional rectification mode, and the content of the sulfuryl chloride in the product is high. Patent US4337235a decomposes sulfuryl chloride by adding sulfur and a catalyst aluminum trichloride, the method comprising fractionating the mixture in the presence of sulfur to distill a mixture of thionyl chloride, sulfuryl chloride, sulfur dichloride and sulfur, the distillate converting sulfuryl chloride to sulfur dioxide, chlorine and sulfur monochloride in the vapor state by sulfur-aluminum chloride particles and reflux vapor containing sulfur-aluminum chloride. However, the method of this patent requires the addition of sulfur and aluminum trichloride catalyst at different steps, which is troublesome, and the sulfur is very slow to dissolve, and the separation effect after use is also unsatisfactory.
Patent CN103172031B provides a method for refining thionyl chloride by using special equipment, in which saturated steam raw material enters a heater, is heated into superheated gas in the heater, the superheated gas enters a fixed bed reactor, contacts an activated carbon bed layer in the fixed bed reactor to undergo decomposition reaction, the gas after reaction enters a cooler to be cooled into saturated liquid, enters a rectifying tower, carries out gas-liquid mass transfer in the tower, and the top of the tower is provided with sulfone chloride, sulfur dioxide and chlorine, and the bottom of the tower is provided with a high-purity thionyl chloride product. The purity of the thionyl chloride is above 99.7%, and the content of the sulfone chloride is lower than 0.3%. However, if the method is to be used, new equipment must be replaced or added, and the method is inconvenient for enterprises with insufficient investment of equipment to directly match with the original device for use, and has poor universal applicability.
Besides high content of sulfone chloride, the content of iron ions is far higher than that of foreign imported products because the synthetic system is generally made of stainless steel, so that the difference between the quality of the domestic sulfoxide chloride and the foreign imported products is remarkable, and the domestic sulfoxide chloride is difficult to replace and is applied to the field of new energy batteries.
There is no convenient solution disclosed to simultaneously and conveniently reduce the sulfone chloride content and the iron ion content in the thionyl chloride product. In view of this, the present application has been made.
Disclosure of Invention
In order to solve the technical problems, the application provides an adsorbent suitable for purifying thionyl chloride.
The embodiment of the application provides an adsorbent suitable for purifying thionyl chloride, and the preparation method of the adsorbent comprises the following steps:
(1) Dispersing boehmite powder in water, adding citric acid, heating and stirring, filtering, and vacuum drying;
(2) Soaking zeolite powder in aluminum chloride solution, filtering, and introducing sulfur dioxide and hydrogen sulfide gas at 35-40 ℃;
(3) Mixing and extrusion molding the boehmite powder treated in the step (1) and the zeolite powder treated in the step (2) with pseudo-boehmite and water to obtain the adsorbent.
As an example, in step (1), the molar ratio of boehmite powder to citric acid is 1:0.4-1.2.
As an example, in the step (1), the temperature of heating and stirring is 80-95 ℃ and the time is 15-32 h.
As an example, in step (2), the mass of aluminum chloride in the aluminum chloride solution is 0.05% to 2.8% of the mass of zeolite powder.
As an example, in step (2), the molar ratio of sulfur dioxide to hydrogen sulfide gas is 1:2.0-2.2.
As an example, the rate of introducing sulfur dioxide and hydrogen sulfide gas is 2 to 6L/h for 0.5 to 5.5 hours per 1000g of zeolite powder.
As an example, the mass ratio of boehmite powder, zeolite powder and pseudo-boehmite is 3-5:5-7:0.5-1.5.
The application also provides a method for purifying thionyl chloride, which comprises the steps of carrying out adsorption treatment on a crude product of thionyl chloride by adopting the adsorbent according to any one of the above steps, and then carrying out distillation to obtain a purified thionyl chloride product.
Compared with the prior art, the application has the following advantages:
1. the application provides an adsorbent which can simultaneously reduce the content of sulfone chloride and the content of iron ions in a crude product of thionyl chloride, and is easy to separate from the product after being used.
2. The adsorbent of the application is beneficial to popularization and application in industry, and no extra equipment is needed for thionyl chloride production enterprises.
3. The adsorbent of the application does not introduce other impurities into the thionyl chloride product.
4. The adsorbent is prepared from cheap and easily available raw materials, and has low cost.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions of the embodiments of the present application are clearly and completely described below. It will be apparent that the described embodiments are some, but not all, embodiments of the application. All other embodiments, which can be made by a person skilled in the art without creative efforts, based on the described embodiments of the present application fall within the protection scope of the present application.
The raw materials adopted in the following embodiments are all common products purchased in the market, and manufacturers or batches do not influence the basic beneficial effects of realizing the technical scheme of the application.
In the specific implementation process, the adsorbent suitable for purifying thionyl chloride can be formed into the shapes of common solid adsorbents such as spherical particles, long strips and the like.
As a specific example, spherical particles having an average particle diameter of 2.5 to 4mm are used in the following cases.
In the application, the vacuum drying can be carried out by adopting the conventional vacuum drying equipment. The temperature of vacuum drying is controlled between 64 and 68 ℃ and the vacuum degree is controlled between 0.07 and 0.08MPa.
Example 1
An adsorbent suitable for purifying thionyl chloride, the preparation method comprises the following steps:
(1) Dispersing 1000g of boehmite powder in 3L of water, adding 1281.1g of citric acid, heating to 85 ℃, stirring for 20h, filtering and drying in vacuum;
(2) Dissolving 0.5g of aluminum chloride in 2L of water to obtain an aluminum chloride solution; 1000g of zeolite powder is immersed in aluminum chloride solution, then filtered, and sulfur dioxide and hydrogen sulfide gas are introduced at 40 ℃; wherein the volume ratio of the sulfur dioxide gas to the hydrogen sulfide gas is 1:2, the ventilation rate is 2L/h, and the time is 5.5h;
(3) Mixing boehmite powder treated in the step (1), zeolite powder treated in the step (2), 100g pseudo-boehmite and water (a proper amount, not limited to a specific amount, is convenient to mold) and extruding and molding to obtain the adsorbent.
Example 2
An adsorbent suitable for purifying thionyl chloride, the preparation method comprises the following steps:
(1) 428.6g of boehmite powder is dispersed in 3L of water, 1674.2g of citric acid is added, the mixture is heated to 95 ℃ and stirred for 15h, filtered and dried in vacuum;
(2) Dissolving 28g of aluminum chloride in 2L of water to obtain an aluminum chloride solution; 1000g of zeolite powder is immersed in aluminum chloride solution, then filtered, and sulfur dioxide and hydrogen sulfide gas are introduced at 35 ℃; wherein the volume ratio of the sulfur dioxide gas to the hydrogen sulfide gas is 1:2.1, the ventilation rate is 6L/h, and the time is 0.5h;
(3) Mixing boehmite powder treated in the step (1), zeolite powder treated in the step (2), 214.3g pseudo-boehmite and water (right amount) and extruding and forming to obtain the adsorbent.
Example 3
An adsorbent suitable for purifying thionyl chloride, the preparation method comprises the following steps:
(1) 666.7g of boehmite powder is dispersed in 3L of water, 1423.7g of citric acid is added, the mixture is heated to 90 ℃ and stirred for 25h, filtered and dried in vacuum;
(2) Dissolving 1g of aluminum chloride in 2L of water to obtain an aluminum chloride solution; 1000g of zeolite powder is immersed in aluminum chloride solution, then filtered, and sulfur dioxide and hydrogen sulfide gas are introduced at 38 ℃; wherein the volume ratio of the sulfur dioxide gas to the hydrogen sulfide gas is 1:2.2, the ventilation rate is 5L/h, and the time is 4h;
(3) Mixing and extrusion molding the boehmite powder treated in the step (1), the zeolite powder treated in the step (2), 166.7g of pseudo-boehmite and water (right amount) to obtain the adsorbent.
Example 4
An adsorbent suitable for purifying thionyl chloride, the preparation method comprises the following steps:
(1) Dispersing 1000g of boehmite powder in 3L of water, adding 2668.7g of citric acid, heating to 80 ℃ and stirring for 20h, filtering and drying in vacuum;
(2) Dissolving 10g of aluminum chloride in 2L of water to obtain an aluminum chloride solution; 1000g of zeolite powder is immersed in aluminum chloride solution, and then filtered, and sulfur dioxide and hydrogen sulfide gas are introduced at the temperature of 35-40 ℃; wherein the volume ratio of the sulfur dioxide gas to the hydrogen sulfide gas is 1:2, the ventilation rate is 4L/h, and the time is 5h;
(3) Mixing and extrusion molding the boehmite powder treated in the step (1), the zeolite powder treated in the step (2), 240g of pseudo-boehmite and water (right amount) to obtain the adsorbent.
Example 5
An adsorbent suitable for purifying thionyl chloride, the preparation method comprises the following steps:
(1) 666.7g of boehmite powder is dispersed in 3L of water, 2562.2g of citric acid is added, the mixture is heated to 90 ℃ and stirred for 18h, filtered and dried in vacuum;
(2) Dissolving 20g of aluminum chloride in 2L of water to obtain an aluminum chloride solution; 1000g of zeolite powder is immersed in aluminum chloride solution, then filtered, and sulfur dioxide and hydrogen sulfide gas are introduced at 40 ℃; wherein the volume ratio of the sulfur dioxide gas to the hydrogen sulfide gas is 1:2.1, the ventilation rate is 6L/h, and the time is 2h;
(3) Mixing and extrusion molding the boehmite powder treated in the step (1), the zeolite powder treated in the step (2), 250g of pseudo-boehmite and water (right amount) to obtain the adsorbent.
Example 6
An adsorbent suitable for purifying thionyl chloride, the preparation method comprises the following steps:
(1) 428.6g of boehmite powder is dispersed in 3L of water, 1464.2g of citric acid is added, the mixture is heated to 80 ℃ and stirred for 28 hours, filtered and dried in vacuum;
(2) Dissolving 25g of aluminum chloride in 2L of water to obtain an aluminum chloride solution; 1000g of zeolite powder is immersed in aluminum chloride solution, then filtered, and sulfur dioxide and hydrogen sulfide gas are introduced at 37 ℃; wherein the volume ratio of the sulfur dioxide gas to the hydrogen sulfide gas is 1:2, the ventilation rate is 3L/h, and the time is 3.5h;
(3) Mixing and extrusion molding the boehmite powder treated in the step (1), the zeolite powder treated in the step (2), 142.9g of pseudo-boehmite and water (right amount) to obtain the adsorbent.
Comparative example 1
The difference from example 1 is that zeolite powder was replaced with activated carbon of equal mass, and the others were kept the same.
Comparative example 2
The difference from example 1 is that boehmite powder was changed to zeolite powder + activated carbon of equal mass (mass ratio 1:1), the others remained the same.
Comparative example 3
The difference from example 1 is that in step (2) the mixing is carried out directly with the solid sulfur which is theoretically equivalent to what can be produced by the gas introduced, the others remaining the same.
Effect example
The adsorbents obtained in examples 1 to 6 and comparative examples 1 to 3 were used to pretreat crude thionyl chloride in the same batch in a certain factory, respectively, and the prepurification properties were examined.
The crude product of thionyl chloride to be treated is slightly yellow, the content of thionyl chloride is 95w%, the content of sulfone chloride is 4w%, and the rest is other impurities, wherein the content of iron ions is 15.62 multiplied by 10 -6 。
The adsorbent comprises the following components: the crude thionyl chloride is put into use with the mass ratio of 1:5, stirred for 12 hours at 40 ℃, and filtered to remove the adsorbent, thus obtaining the treated thionyl chloride. The color of the crude thionyl chloride product after pretreatment, the content of sulfone chloride and iron ions are shown in the following table 1.
In this embodiment, the method for testing the components of the crude product and the pretreated crude product is a conventional method in the industry (refer to HG/T3788-2005) under the same testing conditions, which is only used to assist in embodying the advantages of the present application, and is not an innovative gist of the present application, and will not be described in detail.
TABLE 1
| Using adsorbents | Color of | Thionyl chloride (%) | Chlorination sulfone (%) | Iron ion content |
| Example 1 | Colorless and colorless | 96.49 | 2.73 | 10.42×10 -6 |
| Example 2 | Colorless and colorless | 96.58 | 2.56 | 9.81×10 -6 |
| Example 3 | Colorless and colorless | 96.70 | 2.41 | 9.29×10 -6 |
| Example 4 | Colorless and colorless | 96.62 | 2.53 | 9.75×10 -6 |
| Example 5 | Colorless and colorless | 96.68 | 2.40 | 9.33×10 -6 |
| Example 6 | Colorless and colorless | 96.77 | 2.32 | 9.26×10 -6 |
| Comparative example 1 | The yellow color is slightly light | 95.11 | 3.95 | 15.58×10 -6 |
| Comparative example 2 | The yellow color is slightly light | 95.09 | 3.98 | 15.63×10 -6 |
| Comparative example 3 | Almost colorless | 95.74 | 3.47 | 13.74×10 -6 |
From the experimental results in the table, the adsorbent disclosed by the application is favorable for pre-purifying the crude thionyl chloride product, reduces the content of the sulfone chloride and the iron ions, and reduces the burden for the subsequent rectification procedure.
In addition, according to the feedback of a certain enterprise using the adsorbent of the application, after the adsorbent of the application is matched in advance on the existing thionyl chloride production line for treatment, the purity of the thionyl chloride of the obtained refined and purified thionyl chloride product can reach 99.81 percent, the content of the thionyl chloride is lower than 0.22 percent, and the content of the iron ions can be as low as 3.15x10 -6 The application possibility of the distance substitution imported products in the battery field is further increased.
Although the embodiments of the present application are described above, the embodiments are only used for facilitating understanding of the present application, and are not intended to limit the present application. Any person skilled in the art can make any modification and variation in form and detail without departing from the spirit and scope of the present disclosure, but the scope of the present disclosure is to be determined by the appended claims.
Claims (8)
1. An adsorbent suitable for purifying thionyl chloride, the adsorbent being prepared by a process comprising the steps of:
(1) Dispersing boehmite powder in water, adding citric acid, heating and stirring, filtering, and vacuum drying;
(2) Soaking zeolite powder in an aluminum chloride solution, filtering, and introducing sulfur dioxide and hydrogen sulfide gas at 35-40 ℃;
(3) Mixing and extrusion molding the boehmite powder treated in the step (1) and the zeolite powder treated in the step (2) with pseudo-boehmite and water to obtain the adsorbent.
2. The adsorbent of claim 1, wherein in step (1), the molar ratio of boehmite powder to citric acid is 1:0.4-1.2.
3. The adsorbent for purifying thionyl chloride according to claim 1, wherein in the step (1), the temperature of heating and stirring is 80-95 ℃ for 15-32 hours.
4. The adsorbent for purifying thionyl chloride according to claim 1, wherein in the step (2), the mass of aluminum chloride in the aluminum chloride solution is 0.05% -2.8% of the mass of zeolite powder.
5. The adsorbent suitable for purifying thionyl chloride according to claim 1, wherein in step (2), the molar ratio of sulfur dioxide to hydrogen sulfide gas is 1:2.0 to 2.2.
6. The adsorbent for purifying thionyl chloride according to claim 5, wherein the rate of introducing sulfur dioxide and hydrogen sulfide gas per 1000g zeolite powder is 2 to 6L/h for 0.5 to 5.5 hours.
7. The adsorbent suitable for purifying thionyl chloride according to claim 1, wherein the mass ratio of boehmite powder, zeolite powder and pseudo-boehmite is 3-5: 5-7: 0.5 to 1.5.
8. A method for purifying thionyl chloride, characterized in that the purified thionyl chloride product is obtained by subjecting a crude product of thionyl chloride to adsorption treatment by the adsorbent according to any one of claims 1 to 7 and then distillation or rectification.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311003732.1A CN117019086A (en) | 2023-08-09 | 2023-08-09 | Adsorbent suitable for purifying thionyl chloride and purification method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311003732.1A CN117019086A (en) | 2023-08-09 | 2023-08-09 | Adsorbent suitable for purifying thionyl chloride and purification method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117019086A true CN117019086A (en) | 2023-11-10 |
Family
ID=88636755
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311003732.1A Pending CN117019086A (en) | 2023-08-09 | 2023-08-09 | Adsorbent suitable for purifying thionyl chloride and purification method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117019086A (en) |
-
2023
- 2023-08-09 CN CN202311003732.1A patent/CN117019086A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CA1079679A (en) | Process for purifying halogenosilanes and halogenogermanes | |
| NZ527110A (en) | Low energy carbonylation process | |
| KR970701166A (en) | PROCESS FOR THE PRODUCTION OF CYCLOHEXYLADIPATES AND ADIPIC ACID | |
| CN1986390A (en) | Process of purifying and recovering waste sulfuric acid containing organic impurity | |
| CN109868180A (en) | A kind of pretreating process of the waste lubricating oil cyclic regeneration of environmental protection | |
| US2067985A (en) | Treatment of waste sulphuric acid and manufacture of sulphate and carbonaceous compositions therefrom | |
| CN117019086A (en) | Adsorbent suitable for purifying thionyl chloride and purification method | |
| CN109535425A (en) | A kind of polyphenylene sulfide resin production process | |
| CN110759838A (en) | Treatment method of thiourea feed liquid | |
| CN114853580B (en) | Process for separating and purifying 2-butoxychloroethane as byproduct in production process of tri (butoxyethyl) phosphate | |
| CN114853646A (en) | Method for synthesizing dimethyl dithiodipropionate based on continuous vulcanization reaction | |
| US3992442A (en) | Process for the continuous production of sorbic acid | |
| EP0106445B2 (en) | Process for modifying and stabilising the colour of carboxylic acids or their mixtures | |
| US1765688A (en) | Process of making sulphuryl chloride | |
| CA1060632A (en) | Purification of sulfuric acid containing acetic acid | |
| KR20230022033A (en) | Recovery method of dimethylformamide from the waste solution of polyimide production process | |
| US2704296A (en) | Treatment of maleic acid liquors with chlorine | |
| JPH06298720A (en) | Purification of fluoroalkyl sulfonic acid | |
| JPH0434537B2 (en) | ||
| US2615786A (en) | High boiling mercaptan production | |
| CN113474327B (en) | Method for treating acesulfame potassium waste liquid | |
| CN111747839A (en) | Synthetic method of 2- (4' -ethylbenzoyl) benzoic acid | |
| US2914559A (en) | Manufacture of fumaric acid | |
| WO2024101848A1 (en) | Synthesis method of carbonyl sulfide and apparatus therefor | |
| CN108311102B (en) | Method for removing peculiar smell of sodium hydrosulfide solution |
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 |