CN114349688A - High-purity pyridinium propanesulfonate solution and preparation method thereof - Google Patents
High-purity pyridinium propanesulfonate solution and preparation method thereof Download PDFInfo
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- XSUMSESCSPMNPN-UHFFFAOYSA-N propane-1-sulfonate;pyridin-1-ium Chemical compound C1=CC=NC=C1.CCCS(O)(=O)=O XSUMSESCSPMNPN-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- 238000000909 electrodialysis Methods 0.000 claims abstract description 23
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims abstract description 21
- CSKVLUWCGPWCQR-UHFFFAOYSA-M sodium;3-hydroxypropane-1-sulfonate Chemical compound [Na+].OCCCS([O-])(=O)=O CSKVLUWCGPWCQR-UHFFFAOYSA-M 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000009713 electroplating Methods 0.000 claims abstract description 5
- 229910052751 metal Inorganic materials 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims abstract description 5
- 150000003839 salts Chemical class 0.000 claims abstract description 5
- 239000008346 aqueous phase Substances 0.000 claims abstract description 3
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 26
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical group Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 14
- 239000011592 zinc chloride Substances 0.000 claims description 13
- 235000005074 zinc chloride Nutrition 0.000 claims description 13
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims 12
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000012266 salt solution Substances 0.000 claims 1
- 229910021645 metal ion Inorganic materials 0.000 abstract description 11
- ZTWXTOUATKTCQF-UHFFFAOYSA-N 3-hydroxypropane-1-sulfonic acid;sodium Chemical compound [Na].OCCCS(O)(=O)=O ZTWXTOUATKTCQF-UHFFFAOYSA-N 0.000 abstract description 3
- 230000008676 import Effects 0.000 abstract description 2
- 159000000000 sodium salts Chemical class 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 32
- REEBJQTUIJTGAL-UHFFFAOYSA-N 3-pyridin-1-ium-1-ylpropane-1-sulfonate Chemical compound [O-]S(=O)(=O)CCC[N+]1=CC=CC=C1 REEBJQTUIJTGAL-UHFFFAOYSA-N 0.000 description 18
- 238000012360 testing method Methods 0.000 description 8
- 238000004128 high performance liquid chromatography Methods 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- KWIUHFFTVRNATP-UHFFFAOYSA-N glycine betaine Chemical compound C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 4
- 238000007747 plating Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 3
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- RZBSVYZMOJXQJU-UHFFFAOYSA-N [Na].CCCO Chemical compound [Na].CCCO RZBSVYZMOJXQJU-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 229960003237 betaine Drugs 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000012847 fine chemical Substances 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- CLHYKAZPWIRRRD-UHFFFAOYSA-N 1-hydroxypropane-1-sulfonic acid Chemical compound CCC(O)S(O)(=O)=O CLHYKAZPWIRRRD-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical group OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002168 alkylating agent Substances 0.000 description 1
- 229940100198 alkylating agent Drugs 0.000 description 1
- 239000002280 amphoteric surfactant Substances 0.000 description 1
- 238000005282 brightening Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 239000012450 pharmaceutical intermediate Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- KCXFHTAICRTXLI-UHFFFAOYSA-N propane-1-sulfonic acid Chemical compound CCCS(O)(=O)=O KCXFHTAICRTXLI-UHFFFAOYSA-N 0.000 description 1
- 238000013094 purity test Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/06—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom
- C07D213/16—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom containing only one pyridine ring
- C07D213/20—Quaternary compounds thereof
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/138—Halogens; Compounds thereof with alkaline earth metals, magnesium, beryllium, zinc, cadmium or mercury
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/06—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom
- C07D213/127—Preparation from compounds containing pyridine rings
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
- C25D3/14—Electroplating: Baths therefor from solutions of nickel or cobalt from baths containing acetylenic or heterocyclic compounds
- C25D3/18—Heterocyclic compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Pyridine Compounds (AREA)
Abstract
The invention discloses a high-purity pyridinium propanesulfonate solution and a preparation method thereof, wherein 3-hydroxypropanesulfonic acid sodium salt and pyridine are used as raw materials and react in water under the catalysis of metal salt; and after the reaction is finished, carrying out electrodialysis treatment on the reaction solution to obtain a high-purity pyridinium propanesulfonate solution. For many years, high-quality and high-purity products (the purity is more than 99.0%) are in a blank state in China for a long time and completely depend on import, the purity of domestic PPS is low (about 95%), and a large amount of sodium salt and other metal ions are contained in the middle of the products to influence the electroplating function of the products. The invention adopts a micro-technique to react 3-hydroxypropanesulfonic acid sodium with pyridine by an aqueous phase catalysis method for the first time, and then removes metal ions by an electrodialysis technique to obtain a pyridinium propanesulfonate solution with the purity of more than 99.5 percent.
Description
Technical Field
The invention belongs to the fine chemical technology, and particularly relates to a high-purity pyridinium propanesulfonate solution and a preparation method thereof.
Background
Pyridinium propanesulfonate (PPS for short) is a fine chemical functional product and is mainly used in the field of surface treatment, such as high-speed electroplating, chemical plating, electroplating of printed circuit boards and the like. PPS also belongs to betaine type betaine, is an amphoteric surfactant, and can be used as a pigment accelerator, a steel corrosion inhibitor, an alkylating agent, an electronic cleaning agent, a positron inhibitor, a pharmaceutical intermediate and the like. For many years, high-quality and high-purity products (the purity is more than 99.0%) are in a blank state in China for a long time and completely depend on import, the purity of domestic PPS is low (about 95%), and a large amount of sodium salt and other metal ions are contained in the middle of the products to influence the electroplating function of the products.
Disclosure of Invention
The invention discloses a novel preparation method for preparing a high-purity pyridinium propanesulfonate solution.
The invention adopts the following technical scheme:
a preparation method of a high-purity pyridinium propanesulfonate solution comprises the steps of firstly, taking 3-hydroxypropanesulfonic acid sodium salt and pyridine as raw materials, and reacting in water under the catalysis of metal salt; and after the reaction is finished, carrying out electrodialysis treatment on the reaction solution to obtain a high-purity pyridinium propanesulfonate solution.
The invention discloses application of aluminum trichloride and zinc chloride in preparation of a high-purity pyridinium propane sulfonate solution, and preferably, the high-purity pyridinium propane sulfonate solution is prepared by carrying out aqueous phase catalytic reaction on 3-hydroxypropanesulfonic acid sodium salt and pyridine serving as raw materials.
In the invention, the metal salt is aluminum trichloride and zinc chloride; preferably, the mass ratio of the 3-sodium hydroxypropanesulfonate to the pyridine to the aluminum trichloride to the zinc chloride is (80-100) to (0.01-2); preferably, the mass usage of the 3-hydroxypropanesulfonic acid sodium salt and the pyridine is the same, and the mass usage of the aluminum trichloride and the zinc chloride is the same; further preferably, the dosage of the aluminum trichloride is 1 per mill of the mass of the 3-hydroxypropanesulfonic acid sodium sulfonate.
In the invention, the amount of water is 1-5 times, preferably 3 times of the mass of the 3-hydroxypropanesulfonic acid sodium salt.
In the invention, the reaction is carried out in a microchannel reactor, the reaction temperature is 60-100 ℃, the reaction time is 0.2-2 h, and the reaction pressure is 2-7 MPa; preferably, the reaction temperature is 70-90 ℃, the reaction time is 0.5-1.5 h, and the reaction pressure is 4-6 MPa.
In the invention, the parameters of electrodialysis are voltage of 10-20V, current of 0.5-4A and flow rate of 50-200L/h.
PPS is one of main products of a nickel plating intermediate, has excellent brightening and leveling effects, is most commonly and widely applied to a nickel plating process, and can provide a plating layer with certain smoothness and luster for devices, but a high-quality and high-purity pyridinium propanesulfonate solution is difficult to obtain in the prior art. The invention adopts a micro-technique to react 3-hydroxypropanesulfonic acid sodium with pyridine by a water phase catalysis method for the first time, and then removes metal ions by an electrodialysis technique to obtain a pyridinium propanesulfonate solution with the purity of more than 99.5 percent (calculated by absolute dry weight).
Drawings
FIG. 1 is an infrared spectrum of PPS prepared in example one;
FIG. 2 is an HPLC (high Performance liquid chromatography) of PPS prepared in example one.
Detailed Description
The raw materials of the invention are all the existing products, and the specific operation method and the test method are the conventional techniques in the field. Product characterization (such as infrared and the like), HPLC (Shimadzu high performance liquid chromatograph (LC-20A)) purity test and pyridine residue test, and metal ion content test is carried out by adopting an atomic absorption spectrometer (Ohwes AA6300) which is a conventional technology.
The quality of the PPS product is the solid quality of the high-purity pyridinium propanesulfonate solution after drying water, and the PPS purity is tested by performing conventional HPLC.
The reaction formula of the invention is as follows:
example one
According to the parts by weight:
1. dissolving 100 parts of 3-hydroxypropanesulfonic acid sodium salt (CAS 3542-44-7) in 300 parts of water, and adding 0.1 part of aluminum trichloride and 0.1 part of zinc chloride to obtain a material 1;
2. preparing 100 parts of pyridine as a material 2;
3. conveying the material 1 and the material 2 to a micro-channel reactor, and reacting at 80 ℃ and 5Mpa for 1 h; after the reaction is finished, removing metal ions from the solution (reaction solution) obtained by the microchannel reactor through an electrodialysis technology to obtain a pyridinium propanesulfonate solution (CAS 15471-17-7); the specific parameters of the electrodialysis are as follows: voltage 15V, current 2A, flow rate 100L/h.
The product was subjected to routine testing: the yield of PPS was 99.5%, the purity was 99.6%, Na, Fe, Al, Zn ions were <2ppm, and pyridine residue was <100 ppm.
FIG. 1 is an infrared spectrum of the above PPS; the absorption peak of ring deformation vibration in the pyridine molecular plane is 1580cm-1And 1572cm-1(ii) a The absorption peak of CH deformation vibration on the pyridine molecular skeleton is 1482cm-1And 1439cm-1(ii) a 1190cm as main characteristic peak of sulfonic acid group-1、1068cm-1、620cm-1、530cm-1。
FIG. 2 is an HPLC (high performance liquid chromatography) of the above PPS, and it can be seen that the purity of PPS in the present invention is up to 99.6% based on the dried product.
Example two
According to the parts by weight:
1. dissolving 80 parts of 3-hydroxypropanesulfonic acid sodium salt in 300 parts of water, and adding 0.08 part of aluminum trichloride and 0.08 part of zinc chloride to obtain a material 1;
2. preparing 80 parts of pyridine as a material 2;
3. conveying the material 1 and the material 2 to a micro-channel reactor, and reacting at 85 ℃ and 5Mpa for 1 h; after the reaction is finished, removing metal ions from the solution (reaction solution) obtained by the microchannel reactor through an electrodialysis technology to obtain a pyridinium propanesulfonate solution; the specific parameters of the electrodialysis are as follows: voltage 15V, current 2A, flow rate 110L/h.
The product was subjected to routine testing: the PPS purity is 99.5%, Na, Fe, Al and Zn ions are less than 2ppm, and pyridine residue is less than 100 ppm.
EXAMPLE III
According to the parts by weight:
1. dissolving 100 parts of 3-hydroxypropane sodium sulfonate in 600 parts of water, and adding 0.1 part of aluminum trichloride and 0.1 part of zinc chloride to obtain a material 1;
2. preparing 100 parts of pyridine as a material 2;
3. conveying the material 1 and the material 2 to a micro-channel reactor, and reacting at 80 ℃ and 5Mpa for 1 h; after the reaction is finished, removing metal ions from the solution (reaction solution) obtained by the microchannel reactor through an electrodialysis technology to obtain a pyridinium propanesulfonate solution; the specific parameters of the electrodialysis are as follows: voltage 15V, current 2A, flow rate 100L/h. The product was subjected to routine testing: the PPS purity is 98.3%.
Example four
According to the parts by weight:
1. dissolving 100 parts of sodium 3-hydroxypropanesulfonate in 300 parts of water, and adding 0.2 part of magnesium chloride to obtain a material 1;
2. preparing 100 parts of pyridine as a material 2;
3. conveying the material 1 and the material 2 to a micro-channel reactor, and reacting at 80 ℃ and 5Mpa for 1 h; after the reaction is finished, removing metal ions from the solution (reaction solution) obtained by the microchannel reactor through an electrodialysis technology to obtain a pyridinium propanesulfonate solution; the specific parameters of the electrodialysis are as follows: voltage 15V, current 2A, flow rate 100L/h. The product was subjected to routine testing: the PPS purity was 93.1%.
EXAMPLE five
According to the parts by weight:
1. dissolving 100 parts of 3-hydroxypropanesulfonic acid sodium salt in 300 parts of water, and adding 0.2 part of aluminum trichloride to obtain a material 1;
2. preparing 100 parts of pyridine as a material 2;
3. conveying the material 1 and the material 2 to a micro-channel reactor, and reacting at 80 ℃ and 5Mpa for 1 h; after the reaction is finished, removing metal ions from the solution (reaction solution) obtained by the microchannel reactor through an electrodialysis technology to obtain a pyridinium propanesulfonate solution; the specific parameters of the electrodialysis are as follows: voltage 15V, current 2A, flow rate 100L/h. The product was subjected to routine testing: the purity of PPS was 96.5%.
EXAMPLE six
According to the parts by weight:
1. dissolving 100 parts of 3-hydroxypropane sodium sulfonate in 300 parts of water, and adding 0.2 part of zinc chloride to obtain a material 1;
2. preparing 100 parts of pyridine as a material 2;
3. conveying the material 1 and the material 2 to a micro-channel reactor, and reacting at 80 ℃ and 5Mpa for 1 h; after the reaction is finished, removing metal ions from the solution (reaction solution) obtained by the microchannel reactor through an electrodialysis technology to obtain a pyridinium propanesulfonate solution; the specific parameters of the electrodialysis are as follows: voltage 15V, current 2A, flow rate 100L/h. The product was subjected to routine testing: the purity of PPS was 95.6%.
Comparative example 1
According to the parts by weight:
1. dissolving 100 parts of 3-hydroxypropanesulfonic acid sodium salt in 300 parts of water to obtain a material 1;
2. preparing 100 parts of pyridine as a material 2;
3. conveying the material 1 and the material 2 to a micro-channel reactor, and reacting at 80 ℃ and 5Mpa for 1 h; after the reaction is finished, the solution (reaction solution) obtained by the microchannel reactor is subjected to an electrodialysis technology, and a product cannot be obtained; the specific parameters of the electrodialysis are as follows: voltage 15V, current 2A, flow rate 100L/h.
Comparative example No. two
According to the parts by weight:
1. dissolving 100 parts of propanesulfonic acid in 300 parts of water, and adding 0.1 part of aluminum trichloride and 0.1 part of zinc chloride to obtain a material 1;
2. preparing 100 parts of pyridine as a material 2;
3. conveying the material 1 and the material 2 to a micro-channel reactor, and reacting at 80 ℃ and 5Mpa for 1 h; after the reaction is finished, the solution (reaction solution) obtained by the microchannel reactor is subjected to an electrodialysis technology, and a product cannot be obtained; the specific parameters of the electrodialysis are as follows: voltage 15V, current 2A, flow rate 100L/h.
Claims (10)
1. A preparation method of a high-purity pyridinium propanesulfonate solution is characterized in that 3-hydroxypropanesulfonic acid sodium salt and pyridine are used as raw materials and react in water under the catalysis of metal salt; and after the reaction is finished, carrying out electrodialysis treatment on the reaction solution to obtain a high-purity pyridinium propanesulfonate solution.
2. The method for preparing a high-purity pyridinium propanesulfonate solution as defined in claim 1, wherein the metal salt is aluminum trichloride or zinc chloride.
3. The method for preparing a high-purity pyridinium propanesulfonate solution according to claim 2, wherein the mass ratio of 3-hydroxypropanesulfonic acid sodium salt to pyridine to aluminum trichloride to zinc chloride is (80-100) to (0.01-2).
4. The method for preparing a high-purity pyridinium propanesulfonate solution according to claim 2, wherein the mass amounts of 3-hydroxypropanesulfonic acid sodium salt and pyridine are the same, and the mass amounts of aluminum trichloride and zinc chloride are the same.
5. The method for preparing a high-purity pyridinium propanesulfonate solution according to claim 4, characterized in that the reaction is carried out in a microchannel reactor, the reaction temperature is 60-100 ℃, the reaction time is 0.2-2 h, and the reaction pressure is 2-7 MPa.
6. The method for preparing a high-purity pyridinium propanesulfonate solution according to claim 1, wherein the parameters of the electrodialysis are voltage of 10-20V, current of 0.5-4A, and flow rate of 50-200L/h.
7. The method for producing a high-purity pyridinium propane sulfonate solution according to claim 1, wherein the purity of the high-purity pyridinium propane sulfonate is greater than 99%.
8. The application of aluminum trichloride and zinc chloride in preparing high-purity pyridinium propanesulfonate salt solution.
9. The application of claim 8, wherein the high-purity pyridinium propanesulfonate solution is prepared by aqueous phase catalytic reaction of 3-hydroxypropanesulfonic acid sodium salt and pyridine as raw materials.
10. Use of the high purity pyridinium propanesulfonate solution of claim 1 in the preparation of an electroplating solution.
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| DD276787A3 (en) * | 1984-06-13 | 1990-03-14 | Wolfen Filmfab Veb | METHOD FOR PRODUCING N-SULFO-ALKYL SUBSTITUTED CYCLAMMONIUM SALT BINS |
| CN1256267A (en) * | 1998-11-09 | 2000-06-14 | 河北省望都县冀都精细化工有限公司 | Preparation of pyridine propane sultones |
| CN102633771A (en) * | 2012-04-13 | 2012-08-15 | 保定满城金隆皂素有限公司 | Method for preparing 1,3-propane sultone |
| CN109265392A (en) * | 2018-10-19 | 2019-01-25 | 湖北吉和昌化工科技有限公司 | A kind of method of continuous synthesis of hydroxy propane sulfonic acid pyridinium salt |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| DD276787A3 (en) * | 1984-06-13 | 1990-03-14 | Wolfen Filmfab Veb | METHOD FOR PRODUCING N-SULFO-ALKYL SUBSTITUTED CYCLAMMONIUM SALT BINS |
| SU1456415A1 (en) * | 1986-12-03 | 1989-02-07 | Львовский политехнический институт им.Ленинского комсомола | Method of producing 1,3-propanosulfon |
| CN1256267A (en) * | 1998-11-09 | 2000-06-14 | 河北省望都县冀都精细化工有限公司 | Preparation of pyridine propane sultones |
| CN102633771A (en) * | 2012-04-13 | 2012-08-15 | 保定满城金隆皂素有限公司 | Method for preparing 1,3-propane sultone |
| CN109265392A (en) * | 2018-10-19 | 2019-01-25 | 湖北吉和昌化工科技有限公司 | A kind of method of continuous synthesis of hydroxy propane sulfonic acid pyridinium salt |
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