CN117263837A - Preparation method of potassium thioacetate - Google Patents
Preparation method of potassium thioacetate Download PDFInfo
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- CN117263837A CN117263837A CN202311086523.8A CN202311086523A CN117263837A CN 117263837 A CN117263837 A CN 117263837A CN 202311086523 A CN202311086523 A CN 202311086523A CN 117263837 A CN117263837 A CN 117263837A
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- CN
- China
- Prior art keywords
- potassium thioacetate
- stirring
- mixture
- antioxidant
- thioacetic acid
- 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.)
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- JYWKEVKEKOTYEX-UHFFFAOYSA-N 2,6-dibromo-4-chloroiminocyclohexa-2,5-dien-1-one Chemical compound ClN=C1C=C(Br)C(=O)C(Br)=C1 JYWKEVKEKOTYEX-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 47
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims abstract description 44
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 22
- 229910000027 potassium carbonate Inorganic materials 0.000 claims abstract description 22
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 20
- KOUKXHPPRFNWPP-UHFFFAOYSA-N pyrazine-2,5-dicarboxylic acid;hydrate Chemical compound O.OC(=O)C1=CN=C(C(O)=O)C=N1 KOUKXHPPRFNWPP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002904 solvent Substances 0.000 claims abstract description 20
- 239000002270 dispersing agent Substances 0.000 claims abstract description 19
- 239000004094 surface-active agent Substances 0.000 claims abstract description 19
- 239000003463 adsorbent Substances 0.000 claims abstract description 18
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 18
- 239000012153 distilled water Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000002425 crystallisation Methods 0.000 claims abstract description 7
- 230000008025 crystallization Effects 0.000 claims abstract description 7
- 239000013078 crystal Substances 0.000 claims description 16
- 239000000706 filtrate Substances 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- 239000004927 clay Substances 0.000 claims description 6
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 claims description 6
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- LDVVTQMJQSCDMK-UHFFFAOYSA-N 1,3-dihydroxypropan-2-yl formate Chemical compound OCC(CO)OC=O LDVVTQMJQSCDMK-UHFFFAOYSA-N 0.000 claims description 3
- SPSPIUSUWPLVKD-UHFFFAOYSA-N 2,3-dibutyl-6-methylphenol Chemical compound CCCCC1=CC=C(C)C(O)=C1CCCC SPSPIUSUWPLVKD-UHFFFAOYSA-N 0.000 claims description 3
- BGNXCDMCOKJUMV-UHFFFAOYSA-N Tert-Butylhydroquinone Chemical compound CC(C)(C)C1=CC(O)=CC=C1O BGNXCDMCOKJUMV-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 239000005456 alcohol based solvent Substances 0.000 claims description 3
- 238000004061 bleaching Methods 0.000 claims description 3
- CZBZUDVBLSSABA-UHFFFAOYSA-N butylated hydroxyanisole Chemical compound COC1=CC=C(O)C(C(C)(C)C)=C1.COC1=CC=C(O)C=C1C(C)(C)C CZBZUDVBLSSABA-UHFFFAOYSA-N 0.000 claims description 3
- 235000010354 butylated hydroxytoluene Nutrition 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 3
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 3
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 3
- 229940048086 sodium pyrophosphate Drugs 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
- 239000004250 tert-Butylhydroquinone Substances 0.000 claims description 3
- 235000019281 tert-butylhydroquinone Nutrition 0.000 claims description 3
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 description 10
- 238000000034 method Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C327/00—Thiocarboxylic acids
- C07C327/02—Monothiocarboxylic acids
- C07C327/04—Monothiocarboxylic acids having carbon atoms of thiocarboxyl groups bound to hydrogen atoms or to acyclic carbon atoms
- C07C327/06—Monothiocarboxylic acids having carbon atoms of thiocarboxyl groups bound to hydrogen atoms or to acyclic carbon atoms to hydrogen atoms or to carbon atoms of an acyclic saturated carbon skeleton
Abstract
The invention provides a preparation method of potassium thioacetate, which relates to the technical field of potassium thioacetate and comprises the following steps: s1: proper amounts of potassium carbonate, thioacetic acid, an absolute alcohol solvent, an antioxidant, an adsorbent, a surfactant, a dispersant and distilled water are prepared. According to the invention, potassium carbonate, thioacetic acid, an antioxidant, a surfactant and distilled water are poured into a vacuum reaction tank together for vacuumizing and heating reaction, then the reacted mixture is dried, the anhydrous alcohol solvent, the mixture and a dispersing agent are poured into the reaction tank together for stirring and filtering, then an adsorbent is added for adsorption and filtering, then cooling and crystallization are carried out, and the crystallization is detected, so that the finished product potassium thioacetate can be obtained.
Description
Technical Field
The invention relates to the technical field of potassium thioacetate, in particular to a preparation method of potassium thioacetate.
Background
While potassium thioacetate is an important thioagent in the organic chemical combination reaction, most of the existing preparation methods of potassium thioacetate need hydrogen sulfide gas for preparing thioacetic acid, and meanwhile, in the process of the preparation methods, hydrogen sulfide is more fully reacted, the utilization rate is lower, the cost is higher, the subsequent waste gas yield needs to be treated additionally, and the better preparation and use effects are difficult to achieve, so that improvement is needed.
Disclosure of Invention
The present invention is directed to solving the technical problems set forth in the background art.
The invention adopts the following technical scheme: a method for preparing potassium thioacetate, comprising the following steps:
s1: preparing proper amounts of potassium carbonate, thioacetic acid, absolute alcohol solvents, antioxidants, adsorbents, surfactants, dispersants and distilled water;
s2: pouring potassium carbonate, thioacetic acid, an antioxidant, a surfactant and distilled water into a vacuum reaction tank together, carrying out vacuumizing, heating and heat preservation reaction, wherein the vacuum degree is between-0.04 MPa and-0.08 MPa, the heating temperature is between 60 and 75 ℃, the reaction time is between 2 and 3 hours, stirring is carried out in the reaction process, and the stirring rotating speed is between 60 and 90 revolutions per minute, so as to obtain a mixture for standby;
s3: drying the mixture for 2-3 hours at 90-100 ℃, and taking out the mixture for standby;
s4: pouring the anhydrous alcohol solvent and the dispersing agent into a reaction tank together, adding the mixture, stirring for 30-40 minutes at a stirring speed of 30-60 revolutions per minute, filtering after stirring to obtain filtrate, adding the adsorbent into the filtrate, stirring again for 15-20 minutes at a stirring speed unchanged, and filtering again;
s5: pouring the filtrate obtained by filtration into a crystallization furnace, cooling and crystallizing at the cooling temperature of-5-0 ℃, and then filtering to obtain crystals;
s6: and drying the crystals, detecting the purity of the crystals, and after the crystals are detected to be qualified, placing the crystals into a sealed container for storage to obtain the finished product potassium thioacetate.
Preferably, the mass ratio of the thioacetic acid to the potassium carbonate in the S1 is 1:1-1.5, and the mass ratio of the potassium carbonate, the distilled water and the absolute alcohol solvent is 1:0.5-0.8: 6-10. The amount of the main materials is moderate, so that a good preparation effect can be achieved later.
Preferably, the amount of the antioxidant, the surfactant and the dispersant in the S1 is 0.3-1.2% by weight of the thioacetic acid, and the total amount is not more than 3% by weight of the thioacetic acid, and the amount of the adsorbent in the S1 is 6-10% by weight of the potassium carbonate. The dosage of each auxiliary additive is moderate, and meanwhile, a better preparation effect can be achieved.
Preferably, the antioxidant in S1 is one of butyl hydroxy anisole, dibutyl hydroxy toluene or tert-butyl hydroquinone. Here, the antioxidant can play an antioxidant role, preventing a small amount of air in the vacuum tank from affecting the reaction effect.
Preferably, the anhydrous alcohol solvent in S1 is one of ethanol, isopropanol, isobutanol, n-butanol and isoamyl alcohol. Here, potassium thioacetate is allowed to dissolve smoothly in an absolute alcohol solvent for the subsequent extraction to proceed.
Preferably, the adsorbent in S1 is one or more of acid activated clay, bleaching clay and activated carbon in any proportion. The adsorbent can adsorb impurities in the filtrate, so that the finished product potassium thioacetate can have higher purity.
Preferably, the surfactant in S1 is one of monoglyceride and diglyceride. Here, the surfactant can promote the progress of the reaction so as to achieve a faster potassium thioacetate production effect.
Preferably, the dispersant in the step S1 is one of sodium hexametaphosphate and sodium pyrophosphate. Here, the dispersant can promote the dispersion of the mixture in the absolute alcohol solvent so that the potassium thioacetate can be sufficiently dissolved in the absolute alcohol solvent.
Compared with the prior art, the invention has the advantages and positive effects that:
according to the invention, potassium carbonate, thioacetic acid, an antioxidant, a surfactant and distilled water are poured into a vacuum reaction tank together for vacuumizing and heating reaction, then the reacted mixture is dried, the anhydrous alcohol solvent, the mixture and a dispersing agent are poured into the reaction tank together for stirring and filtering, the potassium carbonate is removed, an adsorbent is added for adsorption and filtering, most of impurities are removed, then cooling crystallization is carried out, and the crystallization is detected, so that the finished product potassium thioacetate can be obtained, hydrogen sulfide gas is not used in the whole process, harmful gas is not generated, and the potassium carbonate and the anhydrous alcohol solvent can be recycled, so that the preparation cost is lower, and a better preparation effect can be achieved.
Drawings
Fig. 1 is a flow chart showing a method for preparing potassium thioacetate according to the present invention.
Detailed Description
In order that the above objects, features and advantages of the invention will be more clearly understood, a further description of the invention will be rendered by reference to the appended drawings and examples. It should be noted that, in the case of no conflict, the embodiments of the present application and the features in the embodiments may be combined with each other.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced otherwise than as described herein, and therefore the present invention is not limited to the specific embodiments of the disclosure that follow.
Examples
Referring to fig. 1, the present invention provides a technical solution: a method for preparing potassium thioacetate, comprising the following steps:
s1: preparing proper amounts of potassium carbonate, thioacetic acid, absolute alcohol solvents, antioxidants, adsorbents, surfactants, dispersants and distilled water;
s2: pouring potassium carbonate, thioacetic acid, an antioxidant, a surfactant and distilled water into a vacuum reaction tank together, carrying out vacuumizing, heating and heat preservation reaction, wherein the vacuum degree is between-0.04 MPa and-0.08 MPa, the heating temperature is between 60 and 75 ℃, the reaction time is between 2 and 3 hours, stirring is carried out in the reaction process, and the stirring rotating speed is between 60 and 90 revolutions per minute, so as to obtain a mixture for standby;
s3: drying the mixture for 2-3 hours at 90-100 ℃, and taking out the mixture for standby;
s4: pouring the anhydrous alcohol solvent and the dispersing agent into a reaction tank together, adding the mixture, stirring for 30-40 minutes at a stirring speed of 30-60 revolutions per minute, filtering after stirring to obtain filtrate, adding the adsorbent into the filtrate, stirring again for 15-20 minutes at a stirring speed unchanged, and filtering again;
s5: pouring the filtrate obtained by filtration into a crystallization furnace, cooling and crystallizing at the cooling temperature of-5-0 ℃, and then filtering to obtain crystals;
s6: and drying the crystals, detecting the purity of the crystals, and after the crystals are detected to be qualified, placing the crystals into a sealed container for storage to obtain the finished product potassium thioacetate.
Referring to FIG. 1, the mass ratio of thioacetic acid to potassium carbonate in S1 is 1:1-1.5, and the mass ratio of potassium carbonate, distilled water and absolute alcohol solvent is 1:0.5-0.8: 6-10, the dosage of main materials is moderate so as to achieve better preparation effect later, the dosage of the antioxidant, the surfactant and the dispersant in S1 is 0.3-1.2 percent of the weight of the thioacetic acid, and the total dosage is not more than 3 percent of the weight of the thioacetic acid, the dosage of the adsorbent in S1 is 6-10 percent of the weight of the potassium carbonate, the dosage of each auxiliary additive is moderate, simultaneously, better preparation effect can be achieved, the antioxidant in S1 is one of butyl hydroxy anisole, dibutyl hydroxy toluene or tertiary butyl hydroquinone, the antioxidant can play an antioxidant effect, the reaction effect is prevented from being influenced by a small amount of air in a vacuum tank, the absolute alcohol solvent in S1 is one of ethanol, isopropanol, isobutanol, n-butanol and isoamyl alcohol, the potassium thioacetate can be smoothly dissolved into an absolute alcohol solvent for subsequent extraction, the adsorbent in S1 is one or a mixture of more of acid activated clay, bleaching clay and active carbon in any proportion, the adsorbent can adsorb impurities in filtrate so as to achieve higher purity of finished potassium thioacetate, the surfactant in S1 is one of monoglyceride and diglyceride, the surfactant can promote reaction so as to achieve a faster preparation effect of potassium thioacetate, the dispersing agent in S1 is one of sodium hexametaphosphate and sodium pyrophosphate, and the dispersing agent can promote the mixture to be dispersed in the absolute alcohol solvent so that the potassium thioacetate can be fully dissolved into the absolute alcohol solvent.
Working principle: the potassium thioacetate finished product is obtained by pouring potassium carbonate, thioacetic acid, an antioxidant, a surfactant and distilled water into a vacuum reaction tank together, carrying out vacuumizing heating reaction, then drying the reacted mixture, pouring an anhydrous alcohol solvent, the mixture and a dispersing agent into the reaction tank together, stirring and filtering, removing potassium carbonate, adding an adsorbent for adsorption filtration, removing most of impurities, cooling and crystallizing, and detecting the crystals.
The present invention is not limited to the above embodiments, and any equivalent embodiments which can be changed or modified by the technical disclosure described above can be applied to other fields, but any simple modification, equivalent changes and modification to the above embodiments according to the technical matter of the present invention will still fall within the protection scope of the technical disclosure.
Claims (8)
1. The preparation method of the potassium thioacetate is characterized by comprising the following steps:
s1: preparing proper amounts of potassium carbonate, thioacetic acid, absolute alcohol solvents, antioxidants, adsorbents, surfactants, dispersants and distilled water;
s2: pouring potassium carbonate, thioacetic acid, an antioxidant, a surfactant and distilled water into a vacuum reaction tank together, carrying out vacuumizing, heating and heat preservation reaction, wherein the vacuum degree is between-0.04 MPa and-0.08 MPa, the heating temperature is between 60 and 75 ℃, the reaction time is between 2 and 3 hours, stirring is carried out in the reaction process, and the stirring rotating speed is between 60 and 90 revolutions per minute, so as to obtain a mixture for standby;
s3: drying the mixture for 2-3 hours at 90-100 ℃, and taking out the mixture for standby;
s4: pouring the anhydrous alcohol solvent and the dispersing agent into a reaction tank together, adding the mixture, stirring for 30-40 minutes at a stirring speed of 30-60 revolutions per minute, filtering after stirring to obtain filtrate, adding the adsorbent into the filtrate, stirring again for 15-20 minutes at a stirring speed unchanged, and filtering again;
s5: pouring the filtrate obtained by filtration into a crystallization furnace, cooling and crystallizing at the cooling temperature of-5-0 ℃, and then filtering to obtain crystals;
s6: and drying the crystals, detecting the purity of the crystals, and after the crystals are detected to be qualified, placing the crystals into a sealed container for storage to obtain the finished product potassium thioacetate.
2. The method for producing potassium thioacetate of claim 1 wherein: the mass ratio of the thioacetic acid to the potassium carbonate in the S1 is 1:1-1.5, and the mass ratio of the potassium carbonate, the distilled water and the absolute alcohol solvent is 1:0.8-1: 6-10.
3. The method for producing potassium thioacetate of claim 1 wherein: the amount of the antioxidant, the surfactant and the dispersing agent in the S1 is 0.3-1.2% of the weight of the thioacetic acid, and the total amount of the antioxidant, the surfactant and the dispersing agent is not more than 3% of the weight of the thioacetic acid, and the amount of the adsorbent in the S1 is 6-10% of the weight of the potassium carbonate.
4. The method for producing potassium thioacetate of claim 1 wherein: the antioxidant in the S1 is one of butyl hydroxy anisole, dibutyl hydroxy toluene or tertiary butyl hydroquinone.
5. The method for producing potassium thioacetate of claim 1 wherein: the absolute alcohol solvent in the S1 is one of ethanol, isopropanol, isobutanol, n-butanol and isoamyl alcohol.
6. The method for producing potassium thioacetate of claim 1 wherein: the adsorbent in the S1 is one or a mixture of more of acid activated clay, bleaching clay and activated carbon in any proportion.
7. The method for producing potassium thioacetate of claim 1 wherein: the surfactant in the S1 is one of monoglyceride and diglyceride.
8. The method for producing potassium thioacetate of claim 1 wherein: the dispersing agent in the S1 is one of sodium hexametaphosphate and sodium pyrophosphate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311086523.8A CN117263837A (en) | 2023-08-28 | 2023-08-28 | Preparation method of potassium thioacetate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311086523.8A CN117263837A (en) | 2023-08-28 | 2023-08-28 | Preparation method of potassium thioacetate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117263837A true CN117263837A (en) | 2023-12-22 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311086523.8A Pending CN117263837A (en) | 2023-08-28 | 2023-08-28 | Preparation method of potassium thioacetate |
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| Country | Link |
|---|---|
| CN (1) | CN117263837A (en) |
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2023
- 2023-08-28 CN CN202311086523.8A patent/CN117263837A/en active Pending
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