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Process for production of dialkyltin dialkoxides

A manufacturing method and technology of dialkyl tin, applied in chemical instruments and methods, tin organic compounds, compounds of elements of Group 4/14 of the periodic table, etc. Carbonate cost and unresolved waste issues

Active Publication Date: 2009-09-02
ASAHI KASEI KK
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, a method for producing a dialkyltin alkoxide compound by the neutralization reaction of a trialkylacetoxytin and an alkylacetoxytin oxide compound has not been known so far
[0028] As mentioned above, there is still a problem in the development of technology to regenerate a modified product of a dialkyltin alkoxide compound into a dialkyltin alkoxide compound as an active body. Therefore, the current situation is cost and waste in the production process of carbonate The matter remains unresolved

Method used

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  • Process for production of dialkyltin dialkoxides
  • Process for production of dialkyltin dialkoxides
  • Process for production of dialkyltin dialkoxides

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0314] Step (1-1): Production of dialkyltin catalyst

[0315] Add 627g (2.7mol) of dibutyltin oxide (manufactured by Sankyo Organic Synthesis Co., Ltd.) and 2000g (22.7mol) of 3-methyl-1-butanol (manufactured by Kuraray Corporation) into an eggplant-shaped flask with a capacity of 5000mL . The flask was installed in an oil bath with a temperature regulator (manufactured by Masuda Physical and Chemical Industry Co., Ltd., Japan, OBH-24), a vacuum pump (manufactured by Japan ULVAC Co., Ltd., G-50A) and a vacuum controller (manufactured by Okano Seisakusho, Japan). , VC-10S) evaporator (manufactured by Japan Shibata Corporation, R-144). The outlet of the purge valve of the evaporator is connected with the pipeline flowing nitrogen at normal pressure. Close the vent valve of the evaporator to depressurize the system, then slowly open the vent valve, flow nitrogen into the system, and return to normal pressure. The temperature of the oil bath was set to about 145°C, the flask wa...

Embodiment 2

[0331] Step (2-1): Substituent exchange reaction of deactivated form of dialkyltin catalyst

[0332] Under a nitrogen atmosphere, 125 g of the inactivated body composition obtained in the same manner as in the procedure (1-2) of Example 1 was added to a 500 mL eggplant-shaped flask, and then 145.0 g of acetic anhydride was added, and stirred at 25° C. for 1 Hour. A fractionating head with a reflux cooler connected to the distillate receiver and a thermometer were installed on the flask, and after vacuum-nitrogen exchange was performed in the flask, the flask was immersed in an oil bath heated to 50°C. The pressure in the container was gradually reduced, and the remaining acetic anhydride and the like were distilled off to obtain 125.9 g of a residue in the flask. carry out on the residue 1 H and 119 Sn-NMR measurement, the residue is tri-n-butylacetoxytin and di-n-butyldiacetoxytin and has 119 In Sn-NMR, a mixture of organotin compounds with tin atoms showing two or more c...

Embodiment 3

[0338] Step (3-1): Substituent exchange reaction of deactivated form of dialkyltin catalyst

[0339] 130 g of the inactivated body composition obtained by the same method as in the step (1-2) of Example 1 and 100 g of toluene (manufactured by Wako Pure Chemical Industries, Ltd., special grade) were put into a 500 mL eggplant-shaped flask. A Dean Stark tube, a Dimroth cooler and a three-way stopcock were installed on the eggplant flask. Connect the three-way cock to a line flowing with nitrogen at normal pressure.

[0340] This flask was immersed in an oil bath previously heated to 140° C., toluene was refluxed, and hydrogen chloride gas was flowed into this flask at a flow rate of about 150 mL / min. While the toluene was refluxing, water was recovered into the Dean Stark tube, and the reaction was terminated after 16 hours of reaction. After cooling the flask to around room temperature, nitrogen gas was released into the flask for 3 hours. Toluene was distilled off from the ...

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Abstract

The object of the present invention is to provide a process for producing a dialkyl tin compound from a composition of deactivated forms of a dialkyl tin catalyst, and to provide a process for producing the dialkyl tin catalyst from the dialkyl tin compound and using the dialkyl tin catalyst to produce a carbonic acid ester. According to the present invention, a process for producing a dialkyl tincompound is provided that subjects a composition of the deactivated forms of the dialkyl tin catalyst, formed when producing an ester compound, to an alkyl group redistribution reaction and / or dealkylation reaction.

Description

technical field [0001] The present invention relates to the manufacture of dialkyltin alkoxide compounds and the manufacture of esters and carbonates using the dialkyltin alkoxide compounds which are used in the manufacture of esters and carbonates catalyst. Background technique [0002] Dialkyltin dialkoxides are extremely useful as catalysts such as ester synthesis catalysts, carbonate synthesis catalysts, transesterification reaction catalysts, silicone polymers, or urethane curing catalysts. Among them, in addition to being used as gasoline additives to increase the octane number and diesel additives to reduce particulates in exhaust gas, carbonates are also used to synthesize organic compounds such as polycarbonate or carbamate, pharmaceuticals / pesticides, etc. useful compounds such as alkylating agents, carbonylating agents, and solvents; or useful compounds used as electrolytes for lithium batteries, raw materials for lubricating oil, and raw materials for deoxidizer...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/22
CPCC07F7/2244C07F7/2232C07F7/2256C07F7/2224C07F7/22
Inventor 篠畑雅亮三宅信寿
Owner ASAHI KASEI KK
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