CN106946753A - The synthesis technique of sodium polydithio-dipropyl sulfonate - Google Patents
The synthesis technique of sodium polydithio-dipropyl sulfonate Download PDFInfo
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- CN106946753A CN106946753A CN201710092055.3A CN201710092055A CN106946753A CN 106946753 A CN106946753 A CN 106946753A CN 201710092055 A CN201710092055 A CN 201710092055A CN 106946753 A CN106946753 A CN 106946753A
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- Prior art keywords
- sodium
- dipropyl sulfonate
- sodium polydithio
- synthesis technique
- peng
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Links
- 239000011734 sodium Substances 0.000 title claims abstract description 63
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title claims abstract description 61
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 61
- -1 polydithio-dipropyl Polymers 0.000 title claims abstract description 60
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 title claims abstract description 56
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 52
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 38
- 150000003839 salts Chemical class 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 239000012046 mixed solvent Substances 0.000 claims abstract description 8
- 150000001298 alcohols Chemical class 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 5
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N dimethylmethane Natural products CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000001294 propane Substances 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 34
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 22
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 12
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 12
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 239000007800 oxidant agent Substances 0.000 claims description 5
- 230000001590 oxidative effect Effects 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 claims description 3
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 2
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 2
- 239000003570 air Substances 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 2
- 238000006116 polymerization reaction Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 5
- IHMZYLTUWRQEPK-UHFFFAOYSA-N S(O)(O)(=S)=O.[Na].[S] Chemical compound S(O)(O)(=S)=O.[Na].[S] IHMZYLTUWRQEPK-UHFFFAOYSA-N 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 22
- 239000007787 solid Substances 0.000 description 17
- 229910052938 sodium sulfate Inorganic materials 0.000 description 15
- 235000011152 sodium sulphate Nutrition 0.000 description 15
- 239000000706 filtrate Substances 0.000 description 8
- 238000001914 filtration Methods 0.000 description 8
- 238000001556 precipitation Methods 0.000 description 8
- 238000010792 warming Methods 0.000 description 8
- 239000005864 Sulphur Substances 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- VDQVEACBQKUUSU-UHFFFAOYSA-M disodium;sulfanide Chemical compound [Na+].[Na+].[SH-] VDQVEACBQKUUSU-UHFFFAOYSA-M 0.000 description 3
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 3
- HYHCSLBZRBJJCH-UHFFFAOYSA-M sodium hydrosulfide Chemical compound [Na+].[SH-] HYHCSLBZRBJJCH-UHFFFAOYSA-M 0.000 description 3
- 229910052979 sodium sulfide Inorganic materials 0.000 description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 2
- IOJUPLGTWVMSFF-UHFFFAOYSA-N benzothiazole Chemical compound C1=CC=C2SC=NC2=C1 IOJUPLGTWVMSFF-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- MQVMJSWYKLYFIG-UHFFFAOYSA-N propane-1-sulfonic acid;sodium Chemical compound [Na].CCCS(O)(=O)=O MQVMJSWYKLYFIG-UHFFFAOYSA-N 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- SRRKNRDXURUMPP-UHFFFAOYSA-N sodium disulfide Chemical compound [Na+].[Na+].[S-][S-] SRRKNRDXURUMPP-UHFFFAOYSA-N 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- LMPMFQXUJXPWSL-UHFFFAOYSA-N 3-(3-sulfopropyldisulfanyl)propane-1-sulfonic acid Chemical compound OS(=O)(=O)CCCSSCCCS(O)(=O)=O LMPMFQXUJXPWSL-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- ZLCCLBKPLLUIJC-UHFFFAOYSA-L disodium tetrasulfane-1,4-diide Chemical compound [Na+].[Na+].[S-]SS[S-] ZLCCLBKPLLUIJC-UHFFFAOYSA-L 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- PXQLVRUNWNTZOS-UHFFFAOYSA-N sulfanyl Chemical class [SH] PXQLVRUNWNTZOS-UHFFFAOYSA-N 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/22—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of hydropolysulfides or polysulfides
- C07C319/24—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of hydropolysulfides or polysulfides by reactions involving the formation of sulfur-to-sulfur bonds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C381/00—Compounds containing carbon and sulfur and having functional groups not covered by groups C07C301/00 - C07C337/00
- C07C381/02—Thiosulfates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention discloses a kind of synthesis technique of sodium polydithio-dipropyl sulfonate, belong to the synthesis technical field of sodium polydithio-dipropyl sulfonate.The present invention is with 1,3 propane sultones are raw material, preparation Peng Te salt is reacted in the mixed solvent of alcohols material and water with sulphur sodium thiosulfuric acid, then obtained Peng Te salt is alkalized and aoxidized again, sodium polydithio-dipropyl sulfonate is made in finally purification concentration, made sodium polydithio-dipropyl sulfonate has higher yield and purity, its yield is up to 98.1%, and purity is up to 99.5%, and synthesis technique raw material of the present invention is easy to get, synthesis step is few, suitable industrialized production.
Description
Technical field
The present invention relates to the synthesis technical field of sodium polydithio-dipropyl sulfonate, more particularly to a kind of polydithio-dipropyl
The synthesis technique of sodium sulfonate.
Background technology
Sodium polydithio-dipropyl sulfonate (bis- (3-sulfopropyl) disulfide, hereinafter referred to as SPS), molecular formula：
C6H12Na2O6S4, molecular weight：354.4, No. CAS：27206-35-5, is white to faint yellow solid powder, is mainly used in acidity
Copper brightener, is essential additive in copper facing, uses it for copper facing and can obtain ornamental and functional coating.SPS
It can also be used in combination with such as nonionic surfactant, polyamine and other hydrogen sulphur compounds in typical copper facing formula, can also
Used with dyestuff, if in conjunction with using N, N- dimethyl-dithio carbonyl propane sulfonic acid sodium (DPS), thiocarbamide propyl group sulfate
(UPS) or 3- (benzothiazole -2- sulfydryls)-propane sulfonic acid sodium (ZPS) etc., it will obtain more preferably effect.
Synthesis SPS method mainly has following two at present：
Method 1：Sodium disulfide is generated with vulcanized sodium and sulphur powder reaction, then life is reacted with PS (1,3-PS)
Into SPS.
Reaction equation is as follows：
Na2S+S→Na2S2
Side reaction：
Na2S+2S→Na2S3
Na2S+3S→Na2S4
This route is domestic production SPS main route, but this route is substantial amounts of more because first step side reaction is easily produced
Oxidation of sulfur compound impurities, cause production SPS it is of poor quality, its effective content is unable to reach more than 90%.
Method 2：With NaHS and 1,3- propane sultones (1,3-PS) reaction generation 3- sulphur (mercapto) base propane sulfonic acid sodium
(MPS) SPS, then by 3- mercapto propyl-sulfonates (MPS) oxidation reaction is generated, wherein NaHS is by hydrogen sulfide and NaOH
Reaction generation.
Reaction equation is as follows：
H2S+NaOH→NaHS+H2O
Hydrogen sulfide belongs to hypertoxic gas in the route, there is very big potential safety hazard, and secondly the process throughput time is long, step
Rapid many, high energy consumption, production cost is high, and is difficult to obtain high purity product.
The content of the invention
It is an object of the invention to overcome above-mentioned prior art to exist problem is easy to get there is provided a kind of raw material, synthesis step is few,
Yield and product purity is high, suitable industrialized production sodium polydithio-dipropyl sulfonate synthesis technique.
To achieve the above object, the present invention is adopted the following technical scheme that：
The synthesis technique of sodium polydithio-dipropyl sulfonate, the synthesis technique comprises the following steps：
1) synthesis of Peng Te salt：1,3- propane sultones and sodium thiosulfate dissolve reaction generation Peng Te salt in a solvent；
2) preparation of sodium polydithio-dipropyl sulfonate：By step 1) made from Peng Te salt and 30% sodium hydrate aqueous solution and
Oxidant is mixed, and Peng Te salt is oxidized polymerization, and sodium polydithio-dipropyl sulfonate is made.
Further, the step 1) in Peng Te salt synthesis condition be 20~30 DEG C of reaction temperature, the reaction time 1.5~
2.5h。
Further, the step 1) in solvent be methanol, ethanol, isopropanol in one or more of any alcohols things
The mixed solvent that matter is constituted with water.
Further, the step 1) in solvent constitute mixed solvent for isopropanol and water.
Further, in the mixed solvent alcohols material and water volume ratio 1: 1~3.
Further, the step 1) in PS and sodium thiosulfate mol ratio be 1: 1.05~1.1.
Further, the step 2) in sodium polydithio-dipropyl sulfonate preparation condition be 50~60 DEG C of reaction temperature,
4~6h of reaction time.
Further, the step 2) in oxidant be air, oxygen, hydrogen peroxide, persulfate, benzoyl peroxide first
One or two kinds of and two or more mixtures in acyl, TBHP.
Further, the step 2) in oxidant be hydrogen peroxide.
Further, the mol ratio of the hydrogen peroxide and sodium thiosulfate is 1: 0.5~0.6.
The present invention reaction equation be：
The invention has the advantages that：
1st, the present invention is using PS as raw material, with sulphur sodium thiosulfuric acid in the mixed solvent of alcohols material and water
Reaction prepares Peng Te salt, and then obtained Peng Te salt is alkalized and aoxidized again, and poly- two sulphur dipropyl is made in finally purification concentration
Alkyl sulfonic acid sodium, made sodium polydithio-dipropyl sulfonate has higher yield and purity, and its yield is up to 98.1%, and purity is reachable
99.5%.
2nd, synthesis technique raw material of the present invention is easy to get, and synthesis step is few, suitable industrialized production.
Embodiment
In order to be better understood from the present invention, the present invention is further described below by embodiment, embodiment is only used
In explaining the present invention, any limit is not constituted to the present invention.
Embodiment 1
The synthesis technique of sodium polydithio-dipropyl sulfonate, the synthesis technique comprises the following steps：
1) synthesis of Peng Te salt：79g (0.5mol) sodium thiosulfate is added in 500mL four-hole bottles and 300mL methanol is stirred
Mix uniform, be cooled to 20 DEG C, 61g (0.5mol) PS is slowly added dropwise, control dropping temperature is at 20~30 DEG C, drop
After adding, continue to react 2 hours at a temperature of 20 DEG C, Peng Te salt is made；
2) preparation of the propane sulfonic acid sodium of two sulphur two：In step 1) made from 30% NaOH regulation pH is added in Peng Te salt
It is worth to after 10, adds 22.5g (0.25mol) TBHP, is warming up to 55 DEG C and reacts 4 hours, be then cooled to 5 DEG C,
Solid sodium sulfate is separated by filtration, meanwhile, solid precipitation is concentrated the filtrate to, filters and is dried at a temperature of 70~80 DEG C, you can
Obtain sodium polydithio-dipropyl sulfonate.
The sodium polydithio-dipropyl sulfonate yield as made from above-mentioned steps is 77%, and purity is 75.3%, wherein containing sulphur
Sour sodium 24.5%, moisture 0.2%.
Embodiment 2
The synthesis technique of sodium polydithio-dipropyl sulfonate, the synthesis technique comprises the following steps：
1) synthesis of Peng Te salt：In 500mL four-hole bottles add 79g (0.5mol) sodium thiosulfate, 200mL isopropanols and
100mL water stirs, and is cooled to 20 DEG C, 61g (0.5mol) PS is slowly added dropwise, control dropping temperature is 20
~30 DEG C, after dripping, continue to react 2 hours at a temperature of 20 DEG C, Peng Te salt is made；
2) preparation of sodium polydithio-dipropyl sulfonate：In step 1) made from the regulation of 30% NaOH is added in Peng Te salt
PH value is warming up to 50 DEG C and reacts 4 hours, then to the hydrogen peroxide that 30g (0.25mol) mass fraction is 28% after 10, is added
5 DEG C are cooled to, solid sodium sulfate is separated by filtration, meanwhile, solid precipitation is concentrated the filtrate to, is filtered and at a temperature of 70~80 DEG C
Dry, you can obtain sodium polydithio-dipropyl sulfonate.
The sodium polydithio-dipropyl sulfonate yield as made from above-mentioned steps is 94.3%, and purity is 98.1%, wherein containing
Sodium sulphate 1.8%, moisture 0.1%.
Embodiment 3
The synthesis technique of sodium polydithio-dipropyl sulfonate, the synthesis technique comprises the following steps：
1) synthesis of Peng Te salt：In 500mL four-hole bottles add 79g (0.5mol) sodium thiosulfate, 250mL isopropanols and
50mL water stirs, and is cooled to 20 DEG C, 61g (0.5mol) PS is slowly added dropwise, control dropping temperature is 20
~30 DEG C, after dripping, continue to react 2 hours at a temperature of 20 DEG C, Peng Te salt is made；
2) preparation of sodium polydithio-dipropyl sulfonate：In step 1) made from the regulation of 30% NaOH is added in Peng Te salt
PH value is continually fed into oxygen to after 10, is warming up to 60 DEG C and reacts 4 hours, is then cooled to 5 DEG C, is separated by filtration solid sodium sulfate,
Meanwhile, solid precipitation is concentrated the filtrate to, filters and is dried at a temperature of 70~80 DEG C, you can obtain polydithio-dipropyl sulfonic acid
Sodium.
The sodium polydithio-dipropyl sulfonate yield as made from above-mentioned steps is 85.7%, and purity is 89.5%, wherein containing
Sodium sulphate 10.4%, moisture 0.1%.
Embodiment 4
The synthesis technique of sodium polydithio-dipropyl sulfonate, the synthesis technique comprises the following steps：
1) synthesis of Peng Te salt：87g (0.55mol) sodium thiosulfate, 150mL isopropanols are added in 500mL four-hole bottles
Stirred with 150mL water, be cooled to 20 DEG C, 61g (0.5mol) PS is slowly added dropwise, control dropping temperature exists
20~30 DEG C, after dripping, continue to react 2 hours at a temperature of 20 DEG C, Peng Te salt is made；
2) preparation of sodium polydithio-dipropyl sulfonate：In step 1) made from the regulation of 30% NaOH is added in Peng Te salt
PH value is warming up to 55 DEG C and reacts 4 hours, then to the hydrogen peroxide that 32g (0.26mol) mass fraction is 28% after 10, is added
5 DEG C are cooled to, solid sodium sulfate is separated by filtration, meanwhile, solid precipitation is concentrated the filtrate to, is filtered and at a temperature of 70~80 DEG C
Dry, you can obtain sodium polydithio-dipropyl sulfonate.
The sodium polydithio-dipropyl sulfonate yield as made from above-mentioned steps is 96.1%, and purity is 98.9%, wherein containing
Sodium sulphate 0.9%, moisture 0.2%.
Embodiment 5
The synthesis technique of sodium polydithio-dipropyl sulfonate, the synthesis technique comprises the following steps：
1) synthesis of Peng Te salt：87g (0.55mol) sodium thiosulfate, 150mL isopropanols are added in 500mL four-hole bottles
Stirred with 150mL water, be cooled to 20 DEG C, 61g (0.5mol) PS is slowly added dropwise, control dropping temperature exists
20~30 DEG C, after dripping, continue to react 1.5 hours at a temperature of 25 DEG C, Peng Te salt is made；
2) preparation of sodium polydithio-dipropyl sulfonate：In step 1) made from the regulation of 30% NaOH is added in Peng Te salt
PH value is warming up to 55 DEG C and reacts 5 hours, then to the hydrogen peroxide that 32g (0.26mol) mass fraction is 28% after 10, is added
5 DEG C are cooled to, solid sodium sulfate is separated by filtration, meanwhile, solid precipitation is concentrated the filtrate to, is filtered and at a temperature of 70~80 DEG C
Dry, you can obtain sodium polydithio-dipropyl sulfonate.
The sodium polydithio-dipropyl sulfonate yield as made from above-mentioned steps is 95.2%, and purity is 97.5%, wherein containing
Sodium sulphate 2.4%, moisture 0.1%.
Embodiment 6
The synthesis technique of sodium polydithio-dipropyl sulfonate, the synthesis technique comprises the following steps：
1) synthesis of Peng Te salt：87g (0.55mol) sodium thiosulfate, 150mL isopropanols are added in 500mL four-hole bottles
Stirred with 150mL water, be cooled to 20 DEG C, 61g (0.5mol) PS is slowly added dropwise, control dropping temperature exists
20~30 DEG C, after dripping, continue to react 2.5 hours at a temperature of 25 DEG C, Peng Te salt is made；
2) preparation of sodium polydithio-dipropyl sulfonate：In step 1) made from the regulation of 30% NaOH is added in Peng Te salt
PH value is warming up to 55 DEG C and reacts 6 hours, then to the hydrogen peroxide that 32g (0.26mol) mass fraction is 28% after 10, is added
5 DEG C are cooled to, solid sodium sulfate is separated by filtration, meanwhile, solid precipitation is concentrated the filtrate to, is filtered and at a temperature of 70~80 DEG C
Dry, you can obtain sodium polydithio-dipropyl sulfonate.
The sodium polydithio-dipropyl sulfonate yield as made from above-mentioned steps is 97.8%, and purity is 99.4%, wherein containing
Sodium sulphate 0.4%, moisture 0.2%.
Embodiment 7
The synthesis technique of sodium polydithio-dipropyl sulfonate, the synthesis technique comprises the following steps：
1) synthesis of Peng Te salt：87g (0.55mol) sodium thiosulfate, 150mL isopropanols are added in 500mL four-hole bottles
Stirred with 150mL water, be cooled to 20 DEG C, 61g (0.5mol) PS is slowly added dropwise, control dropping temperature exists
20~30 DEG C, after dripping, continue to react 2 hours at a temperature of 30 DEG C, Peng Te salt is made；
2) preparation of sodium polydithio-dipropyl sulfonate：In step 1) made from the regulation of 30% NaOH is added in Peng Te salt
PH value is warming up to 60 DEG C and reacts 4 hours, then to the hydrogen peroxide that 32g (0.26mol) mass fraction is 28% after 10, is added
5 DEG C are cooled to, solid sodium sulfate is separated by filtration, meanwhile, solid precipitation is concentrated the filtrate to, is filtered and at a temperature of 70~80 DEG C
Dry, you can obtain sodium polydithio-dipropyl sulfonate.
The sodium polydithio-dipropyl sulfonate yield as made from above-mentioned steps is 98.1%, and purity is 99.5%, wherein containing
Sodium sulphate 0.3%, moisture 0.2%.
Embodiment 8
The synthesis technique of sodium polydithio-dipropyl sulfonate, the synthesis technique comprises the following steps：
1) synthesis of Peng Te salt：87g (0.55mol) sodium thiosulfate, 150mL isopropanols are added in 500mL four-hole bottles
Stirred with 150mL water, be cooled to 20 DEG C, 61g (0.5mol) PS is slowly added dropwise, control dropping temperature exists
20~30 DEG C, after dripping, continue to react 2.5 hours at a temperature of 30 DEG C, Peng Te salt is made；
2) preparation of sodium polydithio-dipropyl sulfonate：In step 1) made from the regulation of 30% NaOH is added in Peng Te salt
PH value is warming up to 50 DEG C and reacts 6 hours, then to the hydrogen peroxide that 32g (0.26mol) mass fraction is 28% after 10, is added
5 DEG C are cooled to, solid sodium sulfate is separated by filtration, meanwhile, solid precipitation is concentrated the filtrate to, is filtered and at a temperature of 70~80 DEG C
Dry, you can obtain sodium polydithio-dipropyl sulfonate.
The sodium polydithio-dipropyl sulfonate yield as made from above-mentioned steps is 95.3%, and purity is 97.2%, wherein containing
Sodium sulphate 2.6%, moisture 0.2%.
Claims (8)
1. the synthesis technique of sodium polydithio-dipropyl sulfonate, it is characterised in that：The synthesis technique comprises the following steps：
1) synthesis of Peng Te salt：1,3- propane sultones and sodium thiosulfate dissolve reaction generation Peng Te salt in a solvent；
2) preparation of sodium polydithio-dipropyl sulfonate：By step 1) made from Peng Te salt and 30% sodium hydrate aqueous solution and oxidation
Agent is mixed, and Peng Te salt is oxidized polymerization, and sodium polydithio-dipropyl sulfonate is made.
2. the synthesis technique of sodium polydithio-dipropyl sulfonate according to claim 1, it is characterised in that：The step 1) in
The synthesis condition of Peng Te salt is 20~30 DEG C of reaction temperature, 1.5~2.5h of reaction time.
3. the synthesis technique of sodium polydithio-dipropyl sulfonate according to claim 1, it is characterised in that：The step 1) in
Solvent be mixed solvent that one or more of any alcohols materials and water in methanol, ethanol, isopropanol are constituted.
4. the synthesis technique for the sodium polydithio-dipropyl sulfonate stated according to claim 3, it is characterised in that：The step 1) in
Solvent is that isopropanol constitutes mixed solvent with water.
5. according to the synthesis technique of the sodium polydithio-dipropyl sulfonate described in claim 3, it is characterised in that：In the mixed solvent
Alcohols material and water volume ratio 1: 1~3.
6. the synthesis technique of sodium polydithio-dipropyl sulfonate according to claim 1, it is characterised in that：The step 2) in
The preparation condition of sodium polydithio-dipropyl sulfonate is 50~60 DEG C of reaction temperature, 4~6h of reaction time.
7. the synthesis technique of sodium polydithio-dipropyl sulfonate according to claim 1, it is characterised in that：The step 2) in
Oxidant be air, oxygen, hydrogen peroxide, persulfate, benzoyl peroxide, TBHP in one kind or two
Plant and two or more mixtures.
8. the synthesis technique of sodium polydithio-dipropyl sulfonate according to claim 7, it is characterised in that：The step 2) in
Oxidant be hydrogen peroxide.
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| CN112142631A (en) * | 2020-09-30 | 2020-12-29 | 江苏梦得新材料科技有限公司 | Synthesis process of high-purity sodium polydithio-dipropyl sulfonate |
| CN115611791A (en) * | 2022-11-03 | 2023-01-17 | 湖北吉和昌化工科技有限公司 | Preparation method of sodium polydithio-dipropyl sulfonate |
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| CN101519369B (en) * | 2009-04-03 | 2012-12-26 | 武汉中德远东精细化工有限公司 | Synthetic method of sodium polydithio-dipropyl sulfonate |
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| CN108912022A (en) * | 2018-07-26 | 2018-11-30 | 湖北吉和昌化工科技有限公司 | A kind of method of purification of sodium polydithio-dipropyl sulfonate |
| CN112142631A (en) * | 2020-09-30 | 2020-12-29 | 江苏梦得新材料科技有限公司 | Synthesis process of high-purity sodium polydithio-dipropyl sulfonate |
| CN115611791A (en) * | 2022-11-03 | 2023-01-17 | 湖北吉和昌化工科技有限公司 | Preparation method of sodium polydithio-dipropyl sulfonate |
| CN115611791B (en) * | 2022-11-03 | 2023-12-26 | 湖北吉和昌化工科技有限公司 | Preparation method of sodium polydithio-dipropyl sulfonate |
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