CN113788854A - Preparation method of isooctyl thioglycolate trimethyl tin - Google Patents
Preparation method of isooctyl thioglycolate trimethyl tin Download PDFInfo
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- CN113788854A CN113788854A CN202111124013.6A CN202111124013A CN113788854A CN 113788854 A CN113788854 A CN 113788854A CN 202111124013 A CN202111124013 A CN 202111124013A CN 113788854 A CN113788854 A CN 113788854A
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- isooctyl thioglycolate
- trimethyl tin
- trimethyl
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- -1 isooctyl thioglycolate trimethyl tin Chemical compound 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- KWTSZCJMWHGPOS-UHFFFAOYSA-M chloro(trimethyl)stannane Chemical compound C[Sn](C)(C)Cl KWTSZCJMWHGPOS-UHFFFAOYSA-M 0.000 claims abstract description 45
- 238000006243 chemical reaction Methods 0.000 claims abstract description 38
- IUNVCWLKOOCPIT-UHFFFAOYSA-N 6-methylheptylsulfanyl 2-hydroxyacetate Chemical compound CC(C)CCCCCSOC(=O)CO IUNVCWLKOOCPIT-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000007864 aqueous solution Substances 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 9
- 239000003960 organic solvent Substances 0.000 claims abstract description 8
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 57
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 11
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 9
- 239000003054 catalyst Substances 0.000 claims description 9
- 239000012267 brine Substances 0.000 claims description 7
- 230000018044 dehydration Effects 0.000 claims description 7
- 238000006297 dehydration reaction Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- DMEGYFMYUHOHGS-UHFFFAOYSA-N cycloheptane Chemical compound C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 claims description 6
- RGSFGYAAUTVSQA-UHFFFAOYSA-N Cyclopentane Chemical compound C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 claims description 4
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 239000001632 sodium acetate Substances 0.000 claims description 4
- 235000017281 sodium acetate Nutrition 0.000 claims description 4
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- YAHBZWSDRFSFOO-UHFFFAOYSA-L dimethyltin(2+);2-(2-ethylhexoxy)-2-oxoethanethiolate Chemical compound CCCCC(CC)COC(=O)CS[Sn](C)(C)SCC(=O)OCC(CC)CCCC YAHBZWSDRFSFOO-UHFFFAOYSA-L 0.000 abstract description 12
- 239000003381 stabilizer Substances 0.000 abstract description 9
- LYRCQNDYYRPFMF-UHFFFAOYSA-N trimethyltin Chemical compound C[Sn](C)C LYRCQNDYYRPFMF-UHFFFAOYSA-N 0.000 abstract description 7
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 4
- 239000000047 product Substances 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 6
- 238000004811 liquid chromatography Methods 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 230000002572 peristaltic effect Effects 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 3
- 231100000331 toxic Toxicity 0.000 description 3
- 230000002588 toxic effect Effects 0.000 description 3
- 206010000117 Abnormal behaviour Diseases 0.000 description 1
- 206010010071 Coma Diseases 0.000 description 1
- 208000004547 Hallucinations Diseases 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- 206010026749 Mania Diseases 0.000 description 1
- 208000009205 Tinnitus Diseases 0.000 description 1
- 206010003549 asthenia Diseases 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000000071 blow moulding Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000003490 calendering Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 231100000566 intoxication Toxicity 0.000 description 1
- 230000035987 intoxication Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 230000001314 paroxysmal effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000886 tinnitus Toxicity 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- YFRLQYJXUZRYDN-UHFFFAOYSA-K trichloro(methyl)stannane Chemical compound C[Sn](Cl)(Cl)Cl YFRLQYJXUZRYDN-UHFFFAOYSA-K 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/22—Tin compounds
- C07F7/226—Compounds with one or more Sn-S linkages
Abstract
The invention belongs to the technical field of preparation of stabilizer methyl tin mercaptide reagent, and particularly relates to a preparation method of isooctyl thioglycolate trimethyl tin, which comprises the following steps: (1) mixing isooctyl thioglycolate and an organic solvent uniformly, and injecting the mixture into a first channel of a microchannel reactor; (2) injecting a trimethyl tin chloride aqueous solution into a second channel of the microchannel reactor, and controlling the reaction temperature of the system to be 25-40 ℃; (3) injecting an alkaline substance into a third channel of the microchannel reactor, and continuously keeping the reaction temperature of 25-40 ℃ for 0.5-1 h; (4) and further carrying out post-treatment on the obtained reaction liquid to obtain isooctyl thioglycolate trimethyl tin. The preparation method has high reaction yield, and the obtained isooctyl thioglycolate has high content of the main component of trimethyl tin.
Description
Technical Field
The invention belongs to the technical field of preparation of a stabilizer methyl tin mercaptide reagent, and particularly relates to a preparation method of isooctyl thioglycolate trimethyl tin.
Background
The methyl tin mercaptide is used as a plastic stabilizer with excellent performance and is widely applied to PVC calendering, blow molding, extrusion molding and injection molding processing. Isooctyl thioglycolate trimethyl tin [ (CH)3)3SnSCH2COOCH(C2H5)C4H9]Is one kind of methyl tin mercaptide, widely exists in methyl tin mercaptide stabilizer, is an important byproduct of the toxicity generated by methyl tin mercaptide, and the decomposed product trimethyl tin chloride is extremely toxic and has high toxicity to human bodyThe symptoms in the stage are asthenia, accompanying paroxysmal headache, tinnitus and dysmnesia. The severe intoxication may cause hallucinations, mania and abnormal behavior, even coma and death. In the preparation method in the prior art, raw materials of isooctyl thioglycolate, methyl tin chloride, alkaline substances and a solvent are added into a reactor for one-step reaction, the trimethyl tin mercaptide in the methyl tin mercaptide produced by the preparation method has unstable data, most of the trimethyl tin chloride enters water and cannot completely generate the trimethyl tin mercaptide, so that the prepared methyl tin mercaptide stabilizer contains a certain amount of trimethyl tin mercaptide, but the trimethyl tin mercaptide cannot be detected in the methyl tin mercaptide stabilizer by conventional means.
At present, no standard substance is used as a reference for detection in the determination of isooctyl thioglycolate trimethyl tin in a methyl tin mercaptide stabilizer, trimethyl tin chloride is very soluble in water, isooctyl thioglycolate in an aqueous solution is difficult to completely react with trimethyl tin chloride, trimethyl tin mercaptide prepared by the conventional process for producing the methyl tin mercaptide stabilizer is not enough to be used as a chemical reagent for identification and analysis because the content of main components is insufficient, and the prepared isooctyl thioglycolate trimethyl tin can be used as a standard chemical reagent for detecting the content of isooctyl thioglycolate trimethyl tin in the methyl tin mercaptide stabilizer.
Disclosure of Invention
In order to overcome the defects of complex reaction process, low reaction yield, low content of main components and more highly toxic trimethyl tin chloride in aqueous solution in the prior art, the invention provides a preparation method of isooctyl thioglycolate trimethyl tin.
The invention is realized by the following technical scheme:
the invention aims to provide a preparation method of isooctyl thioglycolate trimethyl tin, which specifically comprises the following steps:
(1) mixing isooctyl thioglycolate and an organic solvent uniformly, and injecting the mixture into a first channel of a microchannel reactor;
(2) injecting a trimethyl tin chloride aqueous solution into a second channel of the microchannel reactor, and controlling the reaction temperature of the system to be 25-40 ℃;
(3) injecting an alkaline substance into a third channel of the microchannel reactor, and continuously keeping the reaction temperature of 25-40 ℃ for 0.5-1 h;
(4) and further carrying out post-treatment on the obtained reaction liquid to obtain isooctyl thioglycolate trimethyl tin.
Preferably, the mass ratio of the isooctyl thioglycolate to the organic solvent in the step (1) is (50-100): 100.
Preferably, the organic solvent is one or more of n-hexane, cyclohexane, n-heptane, cycloheptane, n-pentane, cyclopentane, benzene and toluene. Is beneficial to extracting the trimethyl tin chloride in the trimethyl tin chloride aqueous solution and is convenient to fully react with the isooctyl thioglycolate.
Preferably, the mass fraction of the trimethyltin chloride aqueous solution in the step (2) is 20 wt% to 50 wt%.
Preferably, the trimethyl tin chloride aqueous solution contains the catalyst, and the addition amount of the catalyst is 1 (0.5-1.5) of the molar ratio of trimethyl tin chloride to the catalyst based on the molar weight of trimethyl tin chloride.
Preferably, the catalyst is sodium carboxylate or/and sodium acetate.
In order to make the reaction between isooctyl thioglycolate and trimethyltin chloride more complete, the invention preferably adds sodium carboxylate or/and sodium acetate as catalyst into the trimethyltin chloride aqueous solution, aiming at improving the main component content of the target product isooctyl thioglycolate trimethyltin.
Preferably, the alkaline substance in the step (3) is NaOH aqueous solution with the mass fraction of 15-25 wt%.
Preferably, the molar ratio of the isooctyl thioglycolate to the trimethyl tin chloride to the NaOH is (1-1.1):1 (0.98-1.02).
Further, the post-treatment of the step (4) is specifically as follows: and standing the reaction solution after the reaction is finished for 1h, separating liquid and removing a water phase, distilling an oil phase under reduced pressure, cooling by using chilled brine at the temperature of 20 ℃ below zero to recover n-hexane, and filtering a product after dehydration and desolventization to obtain the isooctyl thioglycolate trimethyl tin.
Wherein the conditions of the reduced pressure distillation of the oil phase are as follows: distilling under the pressure of-0.1 MPa and the temperature of 60-120 ℃ (the highest temperature is less than or equal to 135 ℃).
Compared with the prior art, the invention has the beneficial effects that:
1) the invention adopts the microchannel reactor to carry out the synthesis process, has mild reaction conditions and more sufficient reaction, ensures that the prepared product has high purity and good yield (up to 100 percent) and is suitable for being used as a standard chemical substance of chemical purity or superior grade purity;
2) the organic solvent adopted by the invention is beneficial to extracting the trimethyl tin chloride in the trimethyl tin chloride aqueous solution, is convenient to fully react with the isooctyl thioglycolate, obtains the isooctyl thioglycolate trimethyl tin product with high yield, does not contain the highly toxic trimethyl tin chloride in the wastewater generated by the reaction, and is safe and environment-friendly.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first" and "second" are used to define the solutions obtained in the different steps, and are only used for the convenience of distinguishing the solutions generated in the respective reaction steps, and unless otherwise stated, the terms do not have any special meaning, and therefore, the scope of the present invention is not to be construed as being limited.
Example 1
A preparation method of isooctyl thioglycolate trimethyl tin comprises the following steps:
(1) adding 84 g of isooctyl thioglycolate and 100 g of n-hexane into a 500 ml conical flask, uniformly mixing, and then injecting the mixed solution into a first channel of a microchannel reactor through a peristaltic pump;
(2) adding 45 g of trimethyl tin chloride and 100 g of water into a 250 ml conical flask, uniformly mixing to obtain a trimethyl tin chloride aqueous solution, then injecting the trimethyl tin chloride aqueous solution into a second channel of the microchannel reactor, and controlling the reaction temperature of a constant temperature system to be 35 ℃;
(3) slowly injecting NaOH solution with the mass fraction of 25 wt% into a third channel of the microchannel reactor, wherein the addition amount of the NaOH solution ensures that the ratio of the molar weight of the NaOH to the molar weight of the trimethyl tin chloride is 1:1, and continuously keeping the reaction temperature of 35 ℃ for 0.5 h;
(4) after the heat preservation reaction is finished, injecting the reaction solution into a standing kettle, standing for 1 hour, separating liquid and removing a water phase, and distilling an oil phase under reduced pressure of-0.1 MPa for 60-120 ℃ (the highest temperature is less than or equal to 135 ℃); the n-hexane is cooled and recycled by frozen brine at the temperature of 20 ℃ below zero, a product after dehydration and desolventization is filtered to obtain the isooctyl thioglycolate trimethyl tin, the yield is 100 percent, the content of a main component is 99 percent by liquid chromatography analysis, the content of the isooctyl thioglycolate is 0.4 percent, and the water content is 0.6 percent.
Example 2
A preparation method of isooctyl thioglycolate trimethyl tin comprises the following steps:
(1) adding 80 g of isooctyl thioglycolate and 100 g of n-hexane into a 500 ml conical flask, uniformly mixing, and then injecting the mixed solution into a first channel of a microchannel reactor through a peristaltic pump;
(2) adding 30 g of trimethyl tin chloride and 100 g of water into a 250 ml conical flask, uniformly mixing to obtain a trimethyl tin chloride aqueous solution, then injecting the trimethyl tin chloride aqueous solution into a second channel of the microchannel reactor, and controlling the reaction temperature of a constant temperature system to be 40 ℃;
(3) slowly injecting NaOH solution with the mass fraction of 20 wt% into a third channel of the microchannel reactor, wherein the addition amount of the NaOH solution ensures that the ratio of the molar weight of the NaOH to the molar weight of the trimethyl tin chloride is 1.01:1, and continuously maintaining the reaction temperature of 40 ℃ for 0.7 h;
(4) after the heat preservation reaction is finished, injecting the reaction solution into a standing kettle, standing for 1 hour, separating liquid and removing a water phase, and distilling an oil phase under reduced pressure of-0.1 MPa for 60-120 ℃ (the highest temperature is less than or equal to 135 ℃); the n-hexane is cooled and recycled by frozen brine at the temperature of 20 ℃ below zero, and a product after dehydration and desolventization is filtered to obtain isooctyl thioglycolate trimethyl tin, wherein the yield is 99.9 percent, the content of a main component is 98.8 percent, the content of isooctyl thioglycolate is 0.6 percent, and the content of water is 0.6 percent by liquid chromatography analysis.
Example 3
A preparation method of isooctyl thioglycolate trimethyl tin comprises the following steps:
(1) adding 94 g of isooctyl thioglycolate and 100 g of n-heptane into a 500 ml conical flask, uniformly mixing, and then injecting the mixed solution into a first channel of a microchannel reactor through a peristaltic pump;
(2) adding 50 g of trimethyl tin chloride and 100 g of water into a 250 ml conical flask, uniformly mixing to obtain a trimethyl tin chloride aqueous solution, then injecting the trimethyl tin chloride aqueous solution into a second channel of the microchannel reactor, and controlling the reaction temperature of a constant temperature system to be 25 ℃;
(3) slowly injecting NaOH solution with the mass fraction of 15 wt% into a third channel of the microchannel reactor, wherein the addition amount of the NaOH solution ensures that the ratio of the molar weight of the NaOH to the molar weight of the trimethyl tin chloride is 0.98:1, and continuously maintaining the reaction temperature of 40 ℃ for 1 h;
(4) after the heat preservation reaction is finished, injecting the reaction solution into a standing kettle, standing for 1 hour, separating liquid and removing a water phase, and distilling an oil phase under reduced pressure of-0.1 MPa for 60-120 ℃ (the highest temperature is less than or equal to 135 ℃); the n-hexane is cooled and recycled by frozen brine at the temperature of 20 ℃ below zero, and a product after dehydration and desolventization is filtered to obtain isooctyl thioglycolate trimethyl tin, wherein the yield is 99.95 percent, the content of a main component is 98.7 percent, the content of isooctyl thioglycolate is 0.7 percent, and the water content is 0.6 percent by liquid chromatography analysis.
Example 4
A preparation method of isooctyl thioglycolate trimethyl tin comprises the following steps:
(1) adding 50 g of isooctyl thioglycolate and 100 g of n-hexane into a 500 ml conical flask, uniformly mixing, and then injecting the mixed solution into a first channel of a microchannel reactor through a peristaltic pump;
(2) adding 45 g of trimethyltin chloride and 100 g of water into a 250 ml conical flask, uniformly mixing to obtain a trimethyltin chloride aqueous solution, adding 25 g of sodium carboxylate into the trimethyltin chloride aqueous solution, mixing for 30min at normal temperature, injecting into a second channel of a microchannel reactor, and controlling the reaction temperature of a constant temperature system to be 25 ℃;
(3) slowly injecting NaOH solution with the mass fraction of 15 wt% into a third channel of the microchannel reactor, wherein the addition amount of the NaOH solution ensures that the molar weight of NaOH is equal to that of trimethyl tin chloride, and continuously keeping the reaction temperature of 40 ℃ for 1 h;
(4) after the heat preservation reaction is finished, injecting the reaction solution into a standing kettle, standing for 1 hour, separating liquid and removing a water phase, and distilling an oil phase under reduced pressure of-0.1 MPa for 60-120 ℃ (the highest temperature is less than or equal to 135 ℃); the n-hexane is cooled and recycled by frozen brine at the temperature of 20 ℃ below zero, and a product after dehydration and desolventization is filtered to obtain the isooctyl thioglycolate trimethyl tin, wherein the yield is 99.99 percent, the content of the main component is 99.1 percent, the content of the isooctyl thioglycolate is 0.5 percent, and the water content is 0.4 percent by liquid chromatography analysis.
Example 5
A preparation method of isooctyl thioglycolate trimethyl tin comprises the following steps:
(1) adding 85 g of isooctyl thioglycolate and 100 g of n-pentane into a 500 ml conical flask, uniformly mixing, and then injecting the mixed solution into a first channel of a microchannel reactor through a peristaltic pump;
(2) adding 20 g of trimethyltin chloride and 100 g of water into a 250 ml conical flask, uniformly mixing to obtain a trimethyltin chloride aqueous solution, adding 40 g of sodium acetate into the trimethyltin chloride aqueous solution, mixing for 20min at normal temperature, injecting into a second channel of a microchannel reactor, and controlling the reaction temperature of a constant temperature system to be 25 ℃;
(3) slowly injecting NaOH solution with the mass fraction of 15 wt% into a third channel of the microchannel reactor, wherein the addition amount of the NaOH solution ensures that the ratio of the molar weight of the NaOH to the molar weight of the trimethyl tin chloride is 1.02:1, and continuously maintaining the reaction temperature of 40 ℃ for 1 h;
(4) after the heat preservation reaction is finished, injecting the reaction solution into a standing kettle, standing for 1 hour, separating liquid and removing a water phase, and distilling an oil phase under reduced pressure of-0.1 MPa for 60-120 ℃ (the highest temperature is less than or equal to 135 ℃); the n-hexane is cooled and recycled by frozen brine at the temperature of 20 ℃ below zero, and a product after dehydration and desolventization is filtered to obtain the isooctyl thioglycolate trimethyl tin, wherein the yield is 99.96 percent, the content of a main component is 99 percent, the content of the isooctyl thioglycolate is 0.6 percent, and the water content is 0.4 percent through liquid chromatography analysis.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of isooctyl thioglycolate trimethyl tin is characterized by comprising the following steps:
(1) mixing isooctyl thioglycolate and an organic solvent uniformly, and injecting the mixture into a first channel of a microchannel reactor;
(2) injecting a trimethyl tin chloride aqueous solution into a second channel of the microchannel reactor, and controlling the reaction temperature of the system to be 25-40 ℃;
(3) injecting an alkaline substance into a third channel of the microchannel reactor, and continuously keeping the reaction temperature of 25-40 ℃ for 0.5-1 h;
(4) and further carrying out post-treatment on the obtained reaction liquid to obtain isooctyl thioglycolate trimethyl tin.
2. The method for preparing isooctyl thioglycolate trimethyl tin according to claim 1, wherein the mass ratio of isooctyl thioglycolate to organic solvent in step (1) is (50-100): 100.
3. The method for preparing isooctyl thioglycolate trimethyltin according to claim 1 or 2, wherein the organic solvent is one or more of n-hexane, cyclohexane, n-heptane, cycloheptane, n-pentane, cyclopentane, benzene and toluene.
4. The method for preparing isooctyl thioglycolate trimethyl tin, according to claim 1, wherein the mass fraction of the trimethyl tin chloride aqueous solution in the step (2) is 20 wt% to 50 wt%.
5. The method for preparing isooctyl thioglycolate trimethyl tin, according to claim 1, wherein the aqueous solution of trimethyl tin chloride contains a catalyst, and the catalyst is added in a molar ratio of trimethyl tin chloride to catalyst of 1 (0.5-1.5) based on the molar amount of trimethyl tin chloride.
6. The method for preparing isooctyl thioglycolate trimethyltin according to claim 5, wherein said catalyst is sodium carboxylate or/and sodium acetate.
7. The method for preparing isooctyl thioglycolate trimethyl tin according to claim 1, wherein said basic substance in step (3) is NaOH aqueous solution with mass fraction of 15-25 wt%.
8. The method for preparing isooctyl thioglycolate trimethyltin according to claim 1, wherein the molar ratio of isooctyl thioglycolate, trimethyltin chloride and NaOH is (1-1.1):1 (0.98-1.02).
9. The method for preparing isooctyl thioglycolate trimethyl tin according to claim 1, wherein the post-treatment of the step (4) is specifically: and standing the reaction solution after the reaction is finished for 1h, separating liquid and removing a water phase, distilling an oil phase under reduced pressure, cooling by using chilled brine at the temperature of 20 ℃ below zero to recover n-hexane, and filtering a product after dehydration and desolventization to obtain the isooctyl thioglycolate trimethyl tin.
10. The method for preparing isooctyl thioglycolate trimethyl tin according to claim 9, wherein the reduced pressure distillation conditions of the oil phase are as follows: distilling under the pressure of-0.1 MPa and the temperature of 60-120 ℃.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4062881A (en) * | 1974-07-26 | 1977-12-13 | Cincinnati Milacron Chemicals, Inc. | Sulfide containing tin stabilizers |
| US20090023940A1 (en) * | 2007-07-20 | 2009-01-22 | Francis Joseph Lipiecki | Method of preparing organometallic compounds |
-
2021
- 2021-09-24 CN CN202111124013.6A patent/CN113788854A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4062881A (en) * | 1974-07-26 | 1977-12-13 | Cincinnati Milacron Chemicals, Inc. | Sulfide containing tin stabilizers |
| US4062881B1 (en) * | 1974-07-26 | 1989-12-26 | ||
| US20090023940A1 (en) * | 2007-07-20 | 2009-01-22 | Francis Joseph Lipiecki | Method of preparing organometallic compounds |
Non-Patent Citations (1)
| Title |
|---|
| C.A.M.AFONSO: "《绿色分离过程—基础与应用》", 31 May 2008, 华东理工大学出版社, pages: 29 - 32 * |
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