CN111302994A - Novel preparation method of potassium thioacetate - Google Patents
Novel preparation method of potassium thioacetate Download PDFInfo
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- CN111302994A CN111302994A CN202010292302.6A CN202010292302A CN111302994A CN 111302994 A CN111302994 A CN 111302994A CN 202010292302 A CN202010292302 A CN 202010292302A CN 111302994 A CN111302994 A CN 111302994A
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- potassium thioacetate
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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 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 65
- 238000006243 chemical reaction Methods 0.000 claims abstract description 48
- 238000000034 method Methods 0.000 claims abstract description 31
- 239000000047 product Substances 0.000 claims abstract description 31
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims abstract description 30
- 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
- 229910000027 potassium carbonate Inorganic materials 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 239000012452 mother liquor Substances 0.000 claims abstract description 12
- 238000001291 vacuum drying Methods 0.000 claims abstract description 10
- 238000005119 centrifugation Methods 0.000 claims abstract description 7
- 238000009461 vacuum packaging Methods 0.000 claims abstract description 7
- 238000002386 leaching Methods 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 9
- 239000002920 hazardous waste Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000004744 fabric Substances 0.000 claims description 5
- 238000000703 high-speed centrifugation Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 238000004806 packaging method and process Methods 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 239000006227 byproduct Substances 0.000 claims description 4
- 239000011888 foil Substances 0.000 claims description 4
- 238000012856 packing Methods 0.000 claims description 4
- 239000011541 reaction mixture Substances 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 230000003068 static effect Effects 0.000 claims description 4
- 239000004033 plastic Substances 0.000 claims description 3
- 239000002826 coolant Substances 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims description 2
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 230000009102 absorption Effects 0.000 abstract description 6
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000003860 storage Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 230000007062 hydrolysis Effects 0.000 abstract description 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract description 2
- 239000007795 chemical reaction product Substances 0.000 abstract 1
- 235000019441 ethanol Nutrition 0.000 description 15
- 235000011181 potassium carbonates Nutrition 0.000 description 11
- 239000012267 brine Substances 0.000 description 6
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 6
- 239000011521 glass Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000011736 potassium bicarbonate Substances 0.000 description 3
- 235000015497 potassium bicarbonate Nutrition 0.000 description 3
- 229910000028 potassium bicarbonate Inorganic materials 0.000 description 3
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 3
- 239000003507 refrigerant Substances 0.000 description 3
- 238000003892 spreading Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 231100000572 poisoning Toxicity 0.000 description 2
- 230000000607 poisoning effect Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- WARIWGPBHKPYON-UHFFFAOYSA-N Ethiolate Chemical compound CCSC(=O)N(CC)CC WARIWGPBHKPYON-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000002259 anti human immunodeficiency virus agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- DUYAAUVXQSMXQP-UHFFFAOYSA-N ethanethioic S-acid Chemical compound CC(S)=O DUYAAUVXQSMXQP-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 235000015320 potassium carbonate Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000005406 washing Methods 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 discloses a novel preparation method of potassium thioacetate, and belongs to the technical field of synthesis and purification. The method comprises the following steps: the method is characterized in that high-concentration ethanol is used as a solvent, the thioacetic acid and potassium carbonate react and crystallize synchronously in the same reaction kettle in a lower-temperature environment, and the reaction product is subjected to centrifugation, leaching, vacuum drying, vacuum packaging and other operations to obtain high-quality potassium thioacetate. The preparation method has the advantages of simple operation process, high product yield, good quality and convenient storage, the treatment method of the mother liquor after centrifugation is more environment-friendly, the product can effectively prevent moisture absorption, hydrolysis, oxidation, color change and the like by utilizing vacuum drying and vacuum packaging, the product quality is ensured, the purity of the potassium thioacetate prepared by the method can reach more than 99.0 percent, and the potassium thioacetate is convenient to feed in a pharmaceutical process using the potassium thioacetate as a raw material, long in quality guarantee period and good in using effect of customers.
Description
Technical Field
The invention relates to a novel preparation method of potassium thioacetate, belonging to the technical field of organic synthesis and purification.
Background
Potassium thioacetate (CAS number: 10387-40-3), also called potassium ethiolate, potassium thioacetate and the like, is white crystalline powder with a melting point of 173-176 ℃, and is mainly used for introducing sulfur atoms in a molecular structure and synthesizing anti-AIDS drugs and the like.
The traditional process for preparing the potassium thioacetate comprises the following steps:
1. dissolving 100kg of potassium carbonate in 200kg of water, and dropwise adding 100kg of thioacetic acid at the temperature of 80 ℃;
2. adding 5kg of active carbon into the synthetic solution, and performing reflux decoloring;
3. cooling the decolorized solution, separating out and filtering unreacted excessive potassium carbonate, potassium bicarbonate and activated carbon to obtain clear liquid;
4. concentrating the clear liquid, evaporating part of water, cooling, crystallizing, washing the centrifugal solid with water, concentrating the mother liquid and the eluting water, crystallizing again, and repeating the steps.
The reaction equation is:
2CH3COSH+K2CO3→2CH3COSK+CO2↑+H2O
the above process has the following defects:
1. the prepared potassium thioacetate has low purity and contains more potassium carbonate and potassium bicarbonate.
2. High energy consumption and low yield.
3. The CH3COSK is strong in water absorption, is easy to oxidize in air, and can react with water for a long time at high temperature.
The Chinese patent CN201710009412.5 discloses a preparation method of potassium thioacetate, which comprises the following steps: adding 190-240 kg of potassium carbonate or potassium bicarbonate into a 500L conical spiral belt vacuum dryer, starting a spiral belt to stir, adding 200kg of thioacetic acid, uniformly stirring, adding 10-20 kg of water in a spraying mode, starting vacuum, keeping the vacuum degree of-0.01 MPa to-0.09 MPa, heating to 40-80 ℃, heating for 20-30 minutes, keeping the temperature to 40-80 ℃, reacting for 2-5 hours, dissolving, separating, decoloring and crystallizing to obtain the potassium thioacetate. But the purity of the prepared potassium thioacetate is not high, so that the pharmaceutical process using the potassium thioacetate as a raw material is influenced, and the potassium thioacetate with low purity is easy to poison a catalyst. And the preparation method and process disclosed by the invention are complicated.
Therefore, the method for preparing the potassium thioacetate with high purity by simple and convenient operation is of great significance.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a novel preparation method of potassium thioacetate, which has the advantages of simple operation process, high product yield and good quality and is beneficial to storage.
The synthesis reaction formula related to the invention is shown as follows:
in order to achieve the technical purpose, the technical scheme of the invention is as follows:
a novel preparation method of potassium thioacetate comprises the following steps:
(1) adding high-concentration ethanol into a reaction kettle, starting stirring, adding potassium carbonate, and controlling the temperature in the reaction kettle at-15-40 ℃ for later use;
(2) slowly dropwise adding thioacetic acid into the reaction kettle, reacting to obtain potassium thioacetate, and crystallizing and separating out the generated potassium thioacetate from the solvent in the form of crystals; after the dropwise addition of the thioacetic acid is finished, controlling the temperature in the reaction kettle to be-15-40 ℃, and reacting for 3-20 hours; after the reaction is finished, controlling the temperature in the reaction kettle to be-15-40 ℃, and preparing for centrifugation;
(3) starting a centrifugal machine to slowly run, slowly putting the reaction mixture obtained in the step (2) into the centrifugal machine to uniformly distribute the potassium thioacetate solid in the centrifugal machine, and firstly centrifuging at a low speed and then centrifuging at a high speed;
(4) after high-speed centrifugation is finished, leaching with high-concentration ethanol at the temperature of-15-40 ℃, and spin-drying the solvent to obtain a white centrifugal solid;
(5) and drying the centrifugal solid in a vacuum environment, drying at 50-130 ℃, and vacuum packaging the dried solid by using a packaging bag to obtain the target product potassium thioacetate.
(6) And (3) treating the centrifugal mother liquor as hazardous waste, or simply distilling the mother liquor, recycling hydrous ethanol as a byproduct for sale, and treating the salt with the recycled solvent as solid hazardous waste.
Preferably, the mass ratio of the thioacetic acid to the potassium carbonate is 1 (0.75-1).
Preferably, the mass ratio of the thioacetic acid to the high-concentration ethanol in the step (1) is 1 (0.8-3).
Preferably, in the step (2), after the reaction is finished, the temperature in the reaction kettle is controlled to be-10-30 ℃.
Preferably, the reaction kettle is a jacketed glass lining reaction kettle.
Further preferably, the temperature in the reaction kettle is controlled by introducing a cooling medium into a jacket to reduce the temperature.
More preferably, the volume of the jacketed glass lining reaction kettle is 100L-5000L.
Preferably, the rotating speed of the stirring is 50-110 r/min.
Preferably, the high-concentration ethanol is ethanol with the content of more than 90%.
Preferably, the dropping speed of the thioacetic acid is controlled to be 5-150 kg/hour.
Preferably, after the centrifuge is started in the step (3), nitrogen can be filled into the centrifuge so as to improve the safety factor and reduce the contact between the product and the air.
Preferably, the vacuum environment in the step (5) is a vacuum environment of-0.099 to-0.07 MPa.
Preferably, in the step (5), the drying method is to dry the packaged materials by cloth bags in a way of being spread flatly in a way of being divided into 5-15 kg/bag.
Preferably, the drying manner in the step (5) is static vacuum drying or rotary vacuum drying.
Preferably, the heat source for drying in step (5) is a steam heat source or a hot water heat source.
Preferably, in step (5), the packaging bag is an aluminum foil bag or an air-tight and light-tight plastic bag.
Preferably, the weight of the vacuum-packed product in the step (5) is 2-25 Kg/bag.
As can be seen from the above description, the present invention has the following advantageous effects:
1. according to the invention, high-concentration ethanol is used as a solvent, potassium thioacetate generated by the reaction of potassium carbonate and thioacetic acid is crystallized and separated out under a low-temperature environment by utilizing the low solubility property of potassium thioacetate in the high-concentration ethanol, the synthesis and crystallization are synchronously carried out in the same reaction kettle, and the use efficiency of equipment is improved.
2. According to the invention, high-concentration ethanol is used as a solvent, the solubility of potassium carbonate in the solvent is low, and the synthesized potassium thioacetate does not have the problem of coating, so that the purity of the potassium thioacetate product is high and can reach more than 99.0%.
3. The invention adopts the centrifugal operation and utilizes the new high-concentration ethanol to leach the mother liquor mixed in the solid in the centrifugal process, thereby reducing the residue of the mother liquor, improving the product quality and obtaining the colorless white crystalline solid.
4. The centrifugal mother liquor can be used for hazardous waste disposal, such as being sent to a qualified incineration unit for incineration and carrying out pollution-free treatment; or simply distilling the mother liquor to recover about 80% ethanol, wherein the recovered ethanol can be sold as a byproduct or used for other industrial purposes; the recycled ethanol can not be used as the solvent of the invention, namely, the recycled ethanol can not be recycled, and the problems of low product yield, yellow product color, easy poisoning of catalyst used by customers, low customer yield, poor effect and the like can be caused by the recycling. And recycling the salt of the solvent as solid hazardous waste for disposal.
5. According to the invention, the target product of potassium thioacetate is obtained by vacuum drying, and after drying, the product is packaged by vacuum, so that moisture absorption, hydrolysis, oxidation, color change and the like of the product can be prevented, the product quality is effectively ensured, the storage of the potassium thioacetate is facilitated, and the quality guarantee period of the product is prolonged; during vacuum packaging, the weight of the product can be 2-25 Kg/bag, preferably 5-10 Kg/bag, because the vacuum-packaged product is easy to agglomerate, and the excessive packaging weight brings inconvenience to the feeding and use of the subsequent production (if the product is not easy to easily crumble, the product needs external force, and the use is very troublesome); if the weight of the package is too small, the packaging cost is increased and the subsequent production and feeding are complicated.
6. The potassium thioacetate prepared by the method avoids catalyst poisoning, improves the yield and has good use effect for customers in a pharmaceutical process taking the potassium thioacetate as a raw material.
Detailed Description
The features of the invention will be further elucidated by the following examples, without limiting the claims of the invention in any way.
Example 1:
(1) starting a tail gas absorption system, adding 550kg of absolute ethyl alcohol into a 1500L glass lining reaction kettle with a jacket, introducing a refrigerant brine ice into the jacket, starting stirring, controlling the rotation speed at 50-90 r/min, adding 360kg of potassium carbonate, and controlling the temperature in the reaction kettle at-15-20 ℃;
(2) slowly dripping 400Kg of thioacetic acid into the reaction kettle at a dripping speed of 80 Kg/h; the reaction releases heat, the temperature of the kettle is controlled to be-15-20 ℃ by using jacket brine ice, the thioacetic acid is dripped, and the constant temperature reaction is controlled to be-15-20 ℃ for 10 hours; after the constant-temperature reaction is finished, controlling the temperature in the reaction kettle to be-10 ℃ and preparing for centrifugation;
(3) starting the centrifugal machine to slowly operate, filling nitrogen into the centrifugal machine to improve the safety coefficient and reduce the contact of the product and air, slowly putting the reactant obtained in the step (2) into the centrifugal machine to uniformly distribute the potassium thioacetate solid in the centrifugal machine, centrifuging at a low speed for 10 minutes, and centrifuging at a high speed for 10 minutes;
(4) after the high-speed centrifugation is finished, leaching with absolute ethyl alcohol at the temperature of-10 ℃ for 1-3 minutes, and then centrifuging at high speed for 10 minutes to obtain a white centrifugal solid;
(5) packing the centrifugal solid into 10-15 kg/bag by cloth bags under the vacuum condition of-0.09 to-0.08 MPa, flatly spreading, drying by a static vacuum drying device under the heating of a hot water heat source at 90-100 ℃ for 8 hours to obtain white crystalline solid; then, 5-10 Kg/bag of aluminum foil bags are used for vacuum packaging to obtain 480Kg of target product potassium thioacetate, and the purity of the product is determined to be 99.4% by an iodometry method;
(6) and (4) hazardous waste disposal of the centrifuged mother liquor.
Example 2:
(1) starting a tail gas absorption system, adding 500kg of absolute ethyl alcohol into a 1500L glass lining reaction kettle with a jacket, introducing a refrigerant brine ice into the jacket, starting stirring, controlling the rotation speed at 50-90 r/min, adding 355kg of potassium carbonate, and controlling the temperature in the reaction kettle to be-10-30 ℃;
(2) slowly dripping 400Kg of thioacetic acid into the reaction kettle at a dripping speed of 80 Kg/h; the reaction releases heat, the temperature of the kettle is controlled to be-10-30 ℃ by using jacket brine ice, the thioacetic acid is dripped, and the constant temperature reaction is controlled to be-10-30 ℃ for 10 hours; after the constant-temperature reaction is finished, controlling the temperature in the reaction kettle to be-10-20 ℃ and preparing for centrifugation;
(3) starting the centrifugal machine to slowly operate, filling nitrogen into the centrifugal machine to improve the safety coefficient and reduce the contact of the product and air, slowly putting the reaction mixture obtained in the step (2) into the centrifugal machine to uniformly distribute the potassium thioacetate solid in the centrifugal machine, centrifuging at a low speed for 10 minutes, and then centrifuging at a high speed for 10 minutes;
(4) after the high-speed centrifugation is finished, leaching the mixture for 1 to 3 minutes by adopting absolute ethyl alcohol at the temperature of minus 10 to 20 ℃, and then centrifuging the mixture for 10 minutes at a high speed to obtain a white centrifugal solid;
(5) packing the centrifugal solid into 10-15 kg/bag by cloth bags under the vacuum condition of-0.09 to-0.08 MPa, flatly spreading, drying by adopting rotary vacuum drying equipment under the heating of a hot water heat source at 90-100 ℃ for 8 hours to obtain white crystalline solid; then, 5-10 Kg of aluminum foil bags are packed in vacuum, 481Kg of target product potassium thioacetate is obtained, and the purity of the product is 99.3% by an iodometry method;
(6) and (3) simply distilling the centrifuged mother liquor, recycling 80-90% ethanol as a byproduct for sale, and treating the salt with the recycled solvent as solid hazardous waste.
Example 3:
(1) starting a tail gas absorption system, adding 550kg of absolute ethyl alcohol into a 1500L glass lining reaction kettle with a jacket, introducing a refrigerant brine ice into the jacket, starting stirring, adding 360kg of potassium carbonate at the rotating speed of 50-90 rpm, and controlling the temperature in the reaction kettle to be 0-40 ℃;
(2) slowly dripping 400Kg of thioacetic acid into the reaction kettle at a dripping speed of 80 Kg/h; performing reaction heat release, controlling the temperature of the kettle to be 0-40 ℃ by using jacket brine ice, controlling the temperature to be 0-40 ℃ to perform constant temperature reaction for 10 hours after the thioacetic acid is dripped; after the constant-temperature reaction is finished, controlling the temperature in the reaction kettle to be-5-30 ℃ and preparing for centrifugation;
(3) starting the centrifugal machine to slowly operate, filling nitrogen into the centrifugal machine to improve the safety coefficient and reduce the contact of the product and air, slowly putting the reaction mixture obtained in the step (2) into the centrifugal machine to uniformly distribute the potassium thioacetate solid in the centrifugal machine, centrifuging at a low speed for 10 minutes, and then centrifuging at a high speed for 10 minutes;
(4) after the high-speed centrifugation is finished, leaching with absolute ethyl alcohol at the temperature of-5-30 ℃ for 1-3 minutes, and then centrifuging at high speed for 10 minutes to obtain a white centrifugal solid;
(5) packing the centrifugal solid into 10-15 kg/bag by cloth bags under the vacuum condition of-0.09 to-0.08 MPa, flatly spreading, drying for 8 hours by adopting static vacuum drying equipment at the temperature of 110 ℃ under a steam heat source to obtain white crystalline solid; then, 5-10 Kg/bag of airtight and light-tight plastic bags are used for vacuum packaging to obtain 470Kg of target product potassium thioacetate, and the purity of the product is 99.15% by an iodometry method;
(6) and (4) hazardous waste disposal of the centrifuged mother liquor.
It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (17)
1. A novel preparation method of potassium thioacetate is characterized by comprising the following steps:
(1) adding high-concentration ethanol into a reaction kettle, starting stirring, adding potassium carbonate, and controlling the temperature in the reaction kettle at-15-40 ℃ for later use;
(2) slowly dropwise adding thioacetic acid into the reaction kettle, reacting to obtain potassium thioacetate, and crystallizing and separating out the generated potassium thioacetate from the solvent in the form of crystals; after the dropwise addition of the thioacetic acid is finished, controlling the temperature in the reaction kettle to be-15-40 ℃, reacting for 3-20 hours, and after the reaction is finished, controlling the temperature in the reaction kettle to be-15-40 ℃, and preparing for centrifugation;
(3) starting a centrifugal machine to slowly run, slowly putting the reaction mixture obtained in the step (2) into the centrifugal machine to uniformly distribute the potassium thioacetate solid in the centrifugal machine, and firstly centrifuging at a low speed and then centrifuging at a high speed;
(4) after high-speed centrifugation is finished, leaching with high-concentration ethanol at the temperature of-15-40 ℃, spin-drying the solvent, and centrifuging to obtain a white solid;
(5) and drying the centrifugal solid in a vacuum environment, drying at 50-130 ℃, and vacuum packaging the dried solid by using a packaging bag to obtain the target product potassium thioacetate.
(6) And (3) treating the centrifugal mother liquor as hazardous waste, or simply distilling the mother liquor, recycling hydrous ethanol as a byproduct for sale, and treating the salt with the recycled solvent as solid hazardous waste.
2. The novel method for preparing potassium thioacetate according to claim 1, wherein the mass ratio of the thioacetic acid to the potassium carbonate is 1 (0.75-1).
3. The novel method for preparing potassium thioacetate according to claim 1, wherein the mass ratio of the thioacetic acid to the high concentration ethanol in the step (1) is 1 (0.8-3).
4. The novel method for preparing potassium thioacetate according to claim 1, wherein in the step (2), after the reaction is completed, the temperature in the reaction vessel is controlled to be-10 to 30 ℃.
5. The novel process for preparing potassium thioacetate according to claim 1, wherein the reaction kettle is a jacketed glass-lined reaction kettle.
6. The method for preparing potassium thioacetate according to claim 5, wherein the temperature in the reaction vessel is controlled by introducing a cooling medium into a jacket to reduce the temperature.
7. The novel process for preparing potassium thioacetate according to claim 5, wherein the jacketed glass-lined reactor has a volume of 100L to 5000L.
8. The method of claim 1, wherein the high concentration ethanol is ethanol with a content of more than 90%.
9. The novel method for preparing potassium thioacetate according to claim 1, wherein the rotation speed of the stirring is 50-110 rpm.
10. The novel method for preparing potassium thioacetate according to claim 1, wherein the dropping rate of the thioacetic acid is controlled to be 5 to 150 kg/hour.
11. The novel process for producing potassium thioacetate of claim 1, wherein after the centrifuge is turned on in the step (3), nitrogen gas is introduced into the centrifuge.
12. The novel method for preparing potassium thioacetate according to claim 1, wherein the vacuum environment in the step (5) is a vacuum environment of-0.099 to-0.07 MPa.
13. The novel method for preparing potassium thioacetate according to claim 1, wherein the drying method in the step (5) is to dry the potassium thioacetate in a way that the potassium thioacetate is packaged into 5-15 kg/bag by cloth bags and laid flat.
14. The method for preparing potassium thioacetate according to claim 1, wherein the drying manner in the step (5) is static vacuum drying or rotary vacuum drying.
15. The novel process for the preparation of potassium thioacetate according to claim 1, wherein the heat source for drying in the step (5) is a steam heat source or a hot water heat source.
16. The method for preparing potassium thioacetate according to claim 1, wherein the packing bag in the step (5) is an aluminum foil bag or an air-tight and light-tight plastic bag.
17. The novel method for preparing potassium thioacetate of claim 1, wherein the weight of the vacuum-packed product in the step (5) is 2 to 25 Kg/bag.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112521307A (en) * | 2020-12-17 | 2021-03-19 | 宁夏启元药业有限公司 | Separation method of tetracycline hydrochloride |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1756739A (en) * | 2003-03-03 | 2006-04-05 | 隆萨股份公司 | Method for the production of a thioacetic acid and salts thereof |
| CN101045701A (en) * | 2006-03-27 | 2007-10-03 | 浙江医药股份有限公司新昌制药厂 | Preparation method of thioacetic acid potassium |
| CN106831513A (en) * | 2017-01-06 | 2017-06-13 | 绍兴市上虞区耕创化工技术服务部 | The preparation method of thioacetic acid potassium |
-
2020
- 2020-04-14 CN CN202010292302.6A patent/CN111302994A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1756739A (en) * | 2003-03-03 | 2006-04-05 | 隆萨股份公司 | Method for the production of a thioacetic acid and salts thereof |
| CN101045701A (en) * | 2006-03-27 | 2007-10-03 | 浙江医药股份有限公司新昌制药厂 | Preparation method of thioacetic acid potassium |
| CN106831513A (en) * | 2017-01-06 | 2017-06-13 | 绍兴市上虞区耕创化工技术服务部 | The preparation method of thioacetic acid potassium |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112521307A (en) * | 2020-12-17 | 2021-03-19 | 宁夏启元药业有限公司 | Separation method of tetracycline hydrochloride |
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