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Coordination methyl tin mercaptide compound, preparation method and application thereof

A technology of methyl tin thiol and compound, applied in the direction of tin organic compounds and the like, can solve the problems of easy precipitation and strong odor of mercaptan, and achieve the effects of non-volatile precipitation, low odor and strong practicability

Active Publication Date: 2010-07-07
湖北犇星新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, most of the domestic manufacturers have improved their production technology, such as Chinese patent CN1117495A, CN1597764A, CN1137048A, CN1737003A, usually adopt the raw material isooctyl thioglycolate, water, sodium bicarbonate, solvent to join in the reactor, drop formazan The aqueous solution of tin chloride is reacted, and the product is a mixture of isooctyl monomethyltin trimercaptoacetate and isooctyl dimethyltin dimercaptoacetate. Among them, the ratio of A and D is from 1:9 to 4:6. For example, the commercial brands are SS-218, YT-181, ZT-181, etc. This type of stabilizer is widely used in PVC processing, but It has a strong smell of mercaptan and is easy to precipitate during processing, which has a certain impact on PVC processing

Method used

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  • Coordination methyl tin mercaptide compound, preparation method and application thereof
  • Coordination methyl tin mercaptide compound, preparation method and application thereof
  • Coordination methyl tin mercaptide compound, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] In a stainless steel high-pressure reaction kettle equipped with a stirrer, thermometer, pressure gauge and pipeline, at a temperature of 200°C, add 175Kg of metal tin powder, 10Kg of ethers, 130Kg of tin tetrachloride, and slowly feed 150Kg Chloromethane and heated up to 220-230°C, keep the pressure at 1.0-2.0 MPa, react for 7 hours, distill and absorb with pure water to obtain 1448Kg of methyl tin chloride aqueous solution (containing 448Kg of methyl tin chloride).

[0037] In an enamel reaction kettle equipped with a stirrer, thermometer, and pH meter, add 10Kg of catalyst BX-2S, and add 1448Kg of methyl tin chloride aqueous solution (including 448Kg of methyl tin chloride) to 510Kg at a speed of 6L / min In isooctyl mercaptoacetate, add and stir at a temperature of 0°C to 20°C, react for 0.5 hours, then slowly add 10% to 20% lye by mass fraction, continue to stir and react, and keep the temperature at 0°C to 40°C, Until the pH value of the reaction system reached 7.5,...

Embodiment 2

[0039] In a stainless steel high-pressure reaction kettle equipped with a stirrer, thermometer, pressure gauge and pipeline, at a temperature of 200°C, add 175Kg of metal tin powder, 15Kg of ethers, 135Kg of tin tetrachloride, and slowly feed 150Kg Chloromethane and heated up to 220-230°C, keep the pressure at 1.0-2.0MPa, react for 7 hours, distill and absorb with pure water to obtain 1450Kg of methyl tin chloride aqueous solution (containing 450Kg of methyl tin chloride).

[0040] In an enamel reaction kettle equipped with a stirrer, thermometer, and pH meter, add 15Kg of catalyst BX-2S, add 1450Kg of methyl tin chloride aqueous solution (containing 450Kg of methyl tin chloride) to 515Kg at a speed of 6L / min In isooctyl mercaptoacetate, add and stir at a temperature of 0°C to 20°C, react for 0.5 hours, then slowly add 10% to 20% lye by mass fraction, continue to stir and react, and keep the temperature at 0°C to 40°C, Until the pH value of the reaction system reached 7.0, the...

Embodiment 3

[0042]In a stainless steel high-pressure reaction kettle equipped with a stirrer, thermometer, pressure gauge and pipeline, at a temperature of 200°C, add 175Kg metal tin powder, 15Kg ethers, 130Kg tin tetrachloride, and slowly feed 155Kg Chloromethane and heated up to 220-230°C, keep the pressure at 1.0-2.0 MPa, react for 7 hours, distill and absorb with pure water to obtain 1445Kg of methyl tin chloride aqueous solution (containing 445Kg of methyl tin chloride).

[0043] In the enamel reaction kettle equipped with stirrer, thermometer and pH meter, add 15Kg of catalyst BX-2S, and add 1445Kg of methyl tin chloride aqueous solution (containing 450Kg of methyl tin chloride) to 520Kg at a speed of 6L / min In isooctyl mercaptoacetate, add and stir at a temperature of 0°C to 20°C, react for 0.5 hours, then slowly add 10% to 20% lye by mass fraction, continue to stir and react, and keep the temperature at 0°C to 40°C, Until the pH value of the reaction system reached 8.0, then the t...

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Abstract

The invention provides a coordination methyl tin mercaptide compound, a preparation method and application thereof. The coordination methyl tin mercaptide compound is prepared by adopting one-step process catalysis to synthesize an intermediate and condensation reacting with isooctyl thioglycolate, and the intermediate is an aqueous solution of the methyl tin chloride and has a molar ratio of 1:5 with the isooctyl thioglycolate. The preparation method of the coordination methyl tin mercaptide compound comprises steps of preparing the methyl tin chloride and preparing the methyl tin mercaptide. The product provided in the invention is used as a heat stabilizer in the PVC processing and has the advantages of high molecular weight, difficult volatilization and precipitation in the processing and excellent heat stability compared with the traditional methyl tin mercaptide mixture.

Description

technical field [0001] The invention relates to the field of fine chemical production, in particular to a coordination type mercaptan methyl tin compound and its preparation method and application. Background technique [0002] There are many patents on the use of organotin compounds in PVC resin as stabilizers, such as US patents 3222317, 3396185, etc., mainly butyltin and octyltin, because propyltin has an odor, and ethyltin is poisonous and replaced. [0003] In the 1970s, American Morton Chemical Company developed dimethyl tin bis(isooctyl thioglycolate), namely TM-181FS, which is a high-efficiency stabilizer for the preparation of PVC and PVC copolymers. [0004] There are many preparation methods for TM-181FS, and the synthesis of the methyl tin chloride intermediate of TM-181FS is the most critical step, which directly affects the quality of TM-181FS. Such as U.S. Patent No. 3810868, 3887519, 351966 and 4129584 etc., what they synthesized adopted is Grignard reagent ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/22C08L27/06C08K5/58
Inventor 戴百雄宫庭吴勇徐善武刘勇王少培温至鹏张建广蒋俊
Owner 湖北犇星新材料股份有限公司
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