CN113816988A - Synthetic method of triphenyl tin acetate - Google Patents
Synthetic method of triphenyl tin acetate Download PDFInfo
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- CN113816988A CN113816988A CN202111251775.2A CN202111251775A CN113816988A CN 113816988 A CN113816988 A CN 113816988A CN 202111251775 A CN202111251775 A CN 202111251775A CN 113816988 A CN113816988 A CN 113816988A
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- acetate
- triphenyl tin
- water
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- triphenyltin
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- 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
- C07F7/2224—Compounds having one or more tin-oxygen linkages
Abstract
The invention discloses a synthesis method of triphenyl tin acetate, which takes sodium acetate and triphenyl tin chloride as raw materials and water as a solvent, and finally directly generates triphenyl tin acetate after reaction and centrifugation and drying. The invention overcomes the use of a mixed solvent of toluene and methanol in the prior art, is safe and environment-friendly, protects the environment and saves the cost. In the process, the circulating pump is added in the reaction kettle, so that the materials are more uniformly mixed, the reaction speed is accelerated, the reaction time is shortened, the energy consumption is reduced, and the method has the advantages of high yield, good product quality, less three wastes and the like.
Description
Technical Field
The invention relates to the technical field of organic synthesis, in particular to a synthesis method of triphenyl tin acetate.
Background
Triphenyltin acetate, also known as distemper tin, has a molecular formula of C20H18O2Sn is a protective bactericide without systemic action and is mainly applied to preventing and treating beet brown spot and potato lateEpidemic disease, soybean anthracnose, black spot, brown spot, and purpura. It also has good control effect on rice blast, false smut and streak disease. Has good control effect on onion black spot, celery leaf blight, bean anthracnose and coffee green tail spore disease. It has special control effect on ampullaria gigas, algae and water snail. In addition, it also has effects of increasing sugar and increasing yield.
The existing synthesis method of the triphenyl tin acetate is disclosed in documents WebERS, Becker E.I, J.org.chem,1661, vol.27 and p.1258-1260, and the triphenyl tin chloride and the triphenyl tin acetate are used as raw materials to synthesize the triphenyl tin acetate; triphenyltin acetate and 1-ethoxy-1-hexene are produced from acetic acid and (Z) -1-ethoxy-2-triphenylstannylhex-1-ene as described in Lebl, Holecek, Dymak, Steinborn, et al, J.org.chem,2001, vol.625,1 p.86-64; if the triphenyl tin acetate synthesized by the two-step method is firstly adopted, triphenyl tin chloride reacts with sodium hydroxide, the intermediate triphenyl tin hydroxide is firstly synthesized, and then reacts with acetic acid to obtain the triphenyl tin acetate; chinese patent CN1181385A also discloses a new method for synthesizing triphenyl tin acetate, which takes toluene and isopropanol as solvent, triphenyl tin chloride and anhydrous sodium acetate as raw materials, and synthesizes triphenyl tin acetate by a one-step method.
The above prior art solutions have the following drawbacks: the synthetic method of the triphenyltin acetate has a complex reaction route and a long total synthetic process flow, particularly adopts mixed solvents such as toluene, methanol, hexane, isopropanol and the like, has high solvent consumption and higher requirements on equipment and processes, and diphenyl tin dichloride serving as a byproduct in the synthetic process is difficult to convert into a target product of the triphenyltin acetate, so that loss of raw materials or intermediates inevitably exists in each step of the process flow, thereby causing the low yield of the triphenyltin acetate.
Disclosure of Invention
In view of this, the present invention provides a method for synthesizing triphenyl tin acetate, so as to solve the above technical problems.
The invention provides the following technical scheme:
the invention adopts sodium acetate and triphenyl tin chloride as raw materials, water as solvent, and triphenyl tin acetate is finally and directly generated under the action of a circulating pump. The reaction formula is as follows:
the synthesis method of the triphenyl tin acetate comprises the following steps:
s1: adding 1500 kg-2000 kg of water and 140 kg-180 kg of sodium acetate into a reaction kettle in sequence, starting stirring, heating to 30-50 ℃, and stirring for 1-3 hours;
s2: adding 360 kg-420 kg of triphenyltin chloride, heating to 60-80 ℃, starting a circulating pump, preserving heat for 1-3 hours, cooling to 5-10 ℃ after heat preservation, discharging, centrifuging, and performing filter pressing to obtain a filter cake;
s3: and washing the filter cake with water, and drying under reduced pressure to obtain the triphenyl tin acetate.
Preferably, in step S1, the stirring speed is 1000r/min to 5000 r/min.
Preferably, in step S3, the temperature of the reduced pressure drying is 60 to 60 ℃.
Preferably, the synthesis method of the triphenyl tin acetate comprises the following steps:
s1: adding 1500 kg-1800 kg of water and 140 kg-160 kg of sodium acetate into a reaction kettle in sequence, starting stirring, heating to 30-45 ℃, and stirring for 1-2 hours;
s2: adding 360 kg-400 kg of triphenyltin chloride, heating to 60-70 ℃, starting a circulating pump, preserving heat for 1-2 hours, cooling to 5-10 ℃ after heat preservation, discharging, centrifuging, and performing filter pressing to obtain a filter cake;
s3: and washing the filter cake with water, and drying under reduced pressure to obtain the triphenyl tin acetate.
Preferably, the synthesis method of the triphenyl tin acetate comprises the following steps:
s1: adding 1500kg of water and 140kg of sodium acetate into a reaction kettle in sequence, starting stirring, heating to 30 ℃, and stirring for 1 hour;
s2: adding 360kg of triphenyl tin chloride, heating to 60 ℃, starting a circulating pump, preserving heat for 1 hour, cooling to 5-10 ℃ after heat preservation is finished, discharging, centrifuging, and performing filter pressing to obtain a filter cake;
s3: and washing the filter cake with water, and drying under reduced pressure to obtain the triphenyl tin acetate.
Preferably, in step S3, the content of triphenyl tin acetate is greater than or equal to 66%.
According to the technical scheme, the invention has the beneficial effects that:
(1) the synthesis method of the triphenyl tin acetate adopted by the invention adopts fewer process flows, only adopts water as a reaction solvent, overcomes the defect of using a toluene and methanol mixed solvent in the old process, is safe and environment-friendly, protects the environment and saves the cost.
(2) The invention adds the circulating pump in the reaction kettle in the process, not only the materials are more uniformly mixed, but also the reaction speed is accelerated, the reaction time is shortened, the energy consumption is reduced, and the invention has the advantages of high yield, good product quality, less three wastes and the like.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention.
FIG. 1 is a process flow diagram of the synthesis method of triphenyltin acetate.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the following embodiments and accompanying drawings. The exemplary embodiments and descriptions of the present invention are provided to explain the present invention, but not to limit the present invention.
Example 1
Synthetic method of triphenyl tin acetate
The synthesis method of the triphenyl tin acetate comprises the following steps:
s1: adding 1500kg of water and 140kg of sodium acetate into a reaction kettle in sequence, starting stirring, heating to 30 ℃, and stirring for 1 hour;
s2: adding 360kg of triphenyl tin chloride, heating to 60 ℃, starting a circulating pump, preserving heat for 1 hour, cooling to 5 ℃ after heat preservation is finished, discharging, centrifuging, and performing filter pressing to obtain a filter cake;
s3: and washing the filter cake with water, and drying under reduced pressure to obtain the triphenyl tin acetate.
In step S1, the stirring speed was 1000 r/min.
In step S3, the temperature of the reduced pressure drying was 70 ℃.
By the above synthesis method, 365kg of triphenyl tin acetate is prepared in this example, and the content of the prepared triphenyl tin acetate stannate is 66.2%.
Example 2
Synthetic method of triphenyl tin acetate
The synthesis method of the triphenyl tin acetate comprises the following steps:
s1: 1600kg of water and 145kg of sodium acetate are sequentially added into a reaction kettle, stirring is started, the temperature is raised to 40 ℃, and stirring is carried out for 2 hours;
s2: adding 380kg of triphenyl tin chloride, heating to 70 ℃, starting a circulating pump, preserving heat for 2 hours, cooling to 10 ℃ after heat preservation is finished, discharging, centrifuging, and performing filter pressing to obtain a filter cake;
s3: washing the filter cake with water, and drying at 70 ℃ under reduced pressure to obtain the triphenyl tin acetate.
In step S1, the stirring speed was 2000 r/min.
Through the synthesis method, 381kg of triphenyl tin acetate is prepared in the embodiment, and the content of the prepared triphenyl tin acetate stannate is 66.7%.
Example 3
Synthetic method of triphenyl tin acetate
The synthesis method of the triphenyl tin acetate comprises the following steps:
s1: adding 1500kg of water and 140kg of sodium acetate into a reaction kettle in sequence, starting stirring, heating to 30 ℃, and stirring for 1 hour;
s2: adding 360kg of triphenyl tin chloride, heating to 60 ℃, starting a circulating pump, preserving heat for 1 hour, cooling to 10 ℃ after heat preservation is finished, discharging, centrifuging, and performing filter pressing to obtain a filter cake;
s3: washing the filter cake with water, and drying at 60 ℃ under reduced pressure to obtain the triphenyl tin acetate.
In step S1, the stirring speed was 3000 r/min.
Through the above synthesis method, in this example, 377kg of triphenyltin acetate was prepared, and the content of the prepared triphenyltin acetate stannate was 66%.
Example 4
Synthetic method of triphenyl tin acetate
The synthesis method of the triphenyl tin acetate comprises the following steps:
s1: adding 1800kg of water and 160kg of sodium acetate into a reaction kettle in sequence, starting stirring, heating to 45 ℃, and stirring for 2 hours;
s2: adding 400kg of triphenyl tin chloride, heating to 70 ℃, starting a circulating pump, preserving heat for 2 hours, cooling to 10 ℃ after heat preservation is finished, discharging, centrifuging, and performing filter pressing to obtain a filter cake;
s3: and washing the filter cake with water, and drying under reduced pressure to obtain the triphenyl tin acetate.
In step S1, the stirring speed was 4000 r/min.
In step S3, the temperature of the reduced pressure drying was 80 ℃.
Through the above synthesis method, in this example, 376kg of triphenyltin acetate was obtained, and the content of the obtained triphenyltin acetate stannate was 66.3%.
Example 5
Synthetic method of triphenyl tin acetate
The synthesis method of the triphenyl tin acetate comprises the following steps:
s1: adding 2000kg of water and 180kg of sodium acetate into a reaction kettle in sequence, starting stirring, heating to 50 ℃, and stirring for 3 hours;
s2: adding 420kg of triphenyl tin chloride, heating to 80 ℃, starting a circulating pump, preserving heat for 3 hours, cooling to 10 ℃ after heat preservation is finished, discharging, centrifuging, and performing filter pressing to obtain a filter cake;
s3: and washing the filter cake with water, and drying under reduced pressure to obtain the triphenyl tin acetate.
In step S1, the stirring speed was 5000 r/min.
In step S3, the temperature of the reduced pressure drying is 60 ℃.
By the above synthesis method, in this example, 368kg of triphenyl tin acetate is prepared, and the content of the prepared triphenyl tin acetate stannate is 67.1%.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes may be made to the embodiment of the present invention by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A synthetic method of triphenyl tin acetate is characterized by comprising the following steps:
s1: adding 1500 kg-2000 kg of water and 140 kg-180 kg of sodium acetate into a reaction kettle in sequence, starting stirring, heating to 30-50 ℃, and stirring for 1-3 hours;
s2: adding 360 kg-420 kg of triphenyltin chloride, heating to 60-80 ℃, starting a circulating pump, preserving heat for 1-3 hours, cooling to 5-10 ℃ after heat preservation, discharging, centrifuging, and performing filter pressing to obtain a filter cake;
s3: and washing the filter cake with water, and drying under reduced pressure to obtain the triphenyl tin acetate.
2. The method for synthesizing triphenyltin acetate according to claim 1, wherein in step S1, the stirring speed is 1000 to 5000 r/min.
3. The method for synthesizing triphenyltin acetate according to claim 1, wherein in step S3, the temperature of the reduced pressure drying is 60 ℃ to 60 ℃.
4. The method for synthesizing the triphenyltin acetate according to claim 1, wherein the method for synthesizing the triphenyltin acetate comprises the following steps:
s1: adding 1500 kg-1800 kg of water and 140 kg-160 kg of sodium acetate into a reaction kettle in sequence, starting stirring, heating to 30-45 ℃, and stirring for 1-2 hours;
s2: adding 360 kg-400 kg of triphenyltin chloride, heating to 60-70 ℃, starting a circulating pump, preserving heat for 1-2 hours, cooling to 5-10 ℃ after heat preservation, discharging, centrifuging, and performing filter pressing to obtain a filter cake;
s3: and washing the filter cake with water, and drying under reduced pressure to obtain the triphenyl tin acetate.
5. The method for synthesizing the triphenyltin acetate according to claim 1, wherein the method for synthesizing the triphenyltin acetate comprises the following steps:
s1: adding 1500kg of water and 140kg of sodium acetate into a reaction kettle in sequence, starting stirring, heating to 30 ℃, and stirring for 1 hour;
s2: adding 360kg of triphenyl tin chloride, heating to 60 ℃, starting a circulating pump, preserving heat for 1 hour, cooling to 5-10 ℃ after heat preservation is finished, discharging, centrifuging, and performing filter pressing to obtain a filter cake;
s3: and washing the filter cake with water, and drying under reduced pressure to obtain the triphenyl tin acetate.
6. The method for synthesizing triphenyltin acetate according to claim 1, wherein in step S3, the content of triphenyltin acetate is not less than 66%.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS50123046A (en) * | 1974-03-15 | 1975-09-27 | ||
| JPS5116646A (en) * | 1974-07-29 | 1976-02-10 | Sankyo Organic Chemicals Co | SUISANKATORIFUENIRUSUZUKARYUNO SEIZOHO |
| JPS52113950A (en) * | 1976-03-23 | 1977-09-24 | Hokko Chem Ind Co Ltd | Synthesis of high-purity triphenyltin oxide crystals |
| JPS54157549A (en) * | 1978-05-31 | 1979-12-12 | Tokyo Fuainkemikaru Kk | Manufacture of triphenyltin compound |
| CN1181385A (en) * | 1996-11-01 | 1998-05-13 | 双鸭山市光明精细化工厂 | Method for synthetizing triphenyl tin acetate |
| CN102516317A (en) * | 2011-11-08 | 2012-06-27 | 聊城大学 | Phenanthroline sodium formate triphenyltin chloride compound, preparation method and application thereof |
| CN104804034A (en) * | 2015-02-01 | 2015-07-29 | 云南锡业锡化学品有限公司 | Preparation method of butyltin tris(2-ethylhexanoate) catalyst |
| CN106749389A (en) * | 2015-11-22 | 2017-05-31 | 宁夏际华环境安全科技有限公司 | A kind of dibutyl tin dilaurate production technology |
-
2021
- 2021-10-25 CN CN202111251775.2A patent/CN113816988A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS50123046A (en) * | 1974-03-15 | 1975-09-27 | ||
| JPS5116646A (en) * | 1974-07-29 | 1976-02-10 | Sankyo Organic Chemicals Co | SUISANKATORIFUENIRUSUZUKARYUNO SEIZOHO |
| JPS52113950A (en) * | 1976-03-23 | 1977-09-24 | Hokko Chem Ind Co Ltd | Synthesis of high-purity triphenyltin oxide crystals |
| JPS54157549A (en) * | 1978-05-31 | 1979-12-12 | Tokyo Fuainkemikaru Kk | Manufacture of triphenyltin compound |
| CN1181385A (en) * | 1996-11-01 | 1998-05-13 | 双鸭山市光明精细化工厂 | Method for synthetizing triphenyl tin acetate |
| CN102516317A (en) * | 2011-11-08 | 2012-06-27 | 聊城大学 | Phenanthroline sodium formate triphenyltin chloride compound, preparation method and application thereof |
| CN104804034A (en) * | 2015-02-01 | 2015-07-29 | 云南锡业锡化学品有限公司 | Preparation method of butyltin tris(2-ethylhexanoate) catalyst |
| CN106749389A (en) * | 2015-11-22 | 2017-05-31 | 宁夏际华环境安全科技有限公司 | A kind of dibutyl tin dilaurate production technology |
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