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Tetrabutyl tin preparation method

A technology of tetrabutyltin and anhydrous tin tetrachloride, applied in chemical instruments and methods, tin organic compounds, compounds of elements of Group 4/14 of the periodic table, etc., can solve problems such as spraying fire and eliminating safety hazards

Inactive Publication Date: 2018-05-29
SHANGHAI NO 4 REAGENT & H V CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method has some effects, it cannot fundamentally eliminate potential safety hazards. When the reaction starts, there will still be a period of time when the material is sprayed. If the cooling is not good, a fire accident will still occur when the material is sprayed.

Method used

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  • Tetrabutyl tin preparation method

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Experimental program
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Effect test

Embodiment 1

[0014] Drop into 12.2 grams of magnesium powder (0.50mol) and 150 grams of 2-methyltetrahydrofuran in the flask of 500 milliliters, open and stir and be heated to reflux, add 7.5 grams of n-chlorobutane (0.08mol) and 0.5 grams of YF-017 catalyst The mixture, and then a mixture of 38.8 g of n-chlorobutane (0.42 mol) and 34.2 g of anhydrous tin tetrachloride (0.13 mol) was slowly added dropwise, and refluxed for 5 hours after the dropwise addition was completed. After cooling, 100 g of 10% hydrochloric acid was added, and the layers were allowed to stand. Emit the lower floor water phase, carry out atmospheric distillation to the organic phase, change the reduced pressure distillation after all solvents are evaporated, collect 148~150 ℃ of cuts (vacuum tightness is-650Pa), obtain 33.8 grams of products, tetrabutyltin content 96.5% ( GC), the yield was 77.87% (calculated as n-chlorobutane).

Embodiment 2

[0016] Drop into 12.2 gram magnesium powders (0.50mol) and 100 gram isopropyl ethers in the flask of 500 milliliters, open and stir and be heated to reflux, add the mixture of 7.5 gram n-chlorobutanes (0.08mol) and 0.5 gram YF-017 catalysts, Then, a mixed solution of 38.8 grams of n-chlorobutane (0.42 mol) and 34.2 grams of anhydrous tin tetrachloride (0.13 mol) was slowly added dropwise, and refluxed for 5 hours after the dropwise addition was completed. After cooling, 100 g of 10% hydrochloric acid was added, and the layers were allowed to stand. Emit the lower floor water phase, carry out atmospheric distillation to the organic phase, change the reduced pressure distillation after all solvents are steamed, collect 148~150 ℃ of cuts (vacuum tightness is-650Pa), obtain 32.5 grams of products, tetrabutyltin content 96.8% ( GC), the yield was 74.49% (calculated as n-butane chloride).

Embodiment 3

[0018] Drop into 12.2 gram of magnesium powders (0.53mol) and 150 gram of isopropyl ethers in the flask of 500 milliliters, open stirring and be heated to reflux, add the mixture of 7.5 gram of chlorobutane (0.08mol) and 1 gram of YF-017 catalyst, Then, a mixed solution of 38.8 grams of n-chlorobutane (0.42 mol) and 34.2 grams of anhydrous tin tetrachloride (0.13 mol) was slowly added dropwise, and refluxed for 5 hours after the dropwise addition was completed. After cooling, 100 g of 10% hydrochloric acid was added, and the layers were allowed to stand. Release the lower floor water phase, carry out normal pressure distillation to the organic phase, change the reduced pressure distillation after all solvents are evaporated, collect 148~150 ℃ of cuts (vacuum degree is-650Pa), obtain 33.1 grams of products, tetrabutyltin content 97.1% ( GC), the yield was 76.28% (calculated as n-chlorobutane).

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Abstract

The invention discloses a tetrabutyl tin preparation method. The preparation method comprises the following steps: adding magnesium powder and an ether solvent into a reactor with a stirring and refluxing device, starting to stir and heat till refluxing; then adding a small quantity of chlorobutane and a YF-017 catalyst, slowly adding a mixed solution of chlorobutane and anhydrous tin tetrachloride dropwise, conducting a refluxing reaction to the end after finishing adding; cooling to the normal temperature, adding hydrochloric acid while stirring, then allowing standing still for layering; releasing an aqueous phase on the lower layer, distilling an organic phase at the normal pressure, changing to perform reduced pressure distillation after the solvent is completely distilled, and collecting a fraction of 148-150 DEG C under the condition of the vacuum degree of minus 650 Pa, to obtain tetrabutyl tin. A small quantity of catalyst is added into a one-step reaction device, the Grignardreaction is started immediately, the heat produced in the Grignard reaction in the first step is rapidly absorbed by the alkylation reaction in the second step. Therefore, the phenomenon of materialspraying of the reaction is avoided, and safety in the industrial production is guaranteed.

Description

technical field [0001] The invention relates to a synthesis method of chemical products, in particular to a preparation method of tetrabutyltin. Background technique [0002] Tetrabutyltin is an important organic chemical intermediate, an important intermediate for the manufacture of organotin heat stabilizers and organotin catalysts (such as dibutyltin oxide, dibutyltin dilaurate, etc.), and can also be used as gasoline Anti-knock agent. [0003] The synthesis methods of tetrabutyltin generally include Grignard reagent method, alkylaluminum method, Wu's method and direct method. Because Grignard method has the advantages of convenient raw material storage and wide sources, industrial production is mainly based on Grignard reagent method technology. . [0004] The materials related to the Grignard synthesis method are: (1) French chemist Victor Greenia discovered in the laboratory that metal magnesium reacted with ether solutions of many halogenated hydrocarbons to form a ...

Claims

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Application Information

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IPC IPC(8): C07F7/22
CPCC07F7/2296
Inventor 杜骏廖本仁
Owner SHANGHAI NO 4 REAGENT & H V CHEM
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