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The preparation method of methyl tin maleate

A technology of methyl tin acid and maleic acid, which is applied in the field of preparation of methyl tin maleate, can solve the problems of poor compatibility between maleic anhydride and solvents, difficulty in judging the end point of the reaction, long reaction cycle, etc. The effect of shortening, avoiding wall-adhering paste, and short reaction cycle

Active Publication Date: 2018-06-05
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

Using maleic anhydride as a raw material, reacting at 40-130°C, due to the poor compatibility between maleic anhydride and solvents, the phenomenon of sticking paste is prone to occur; The acid value of the system is used to judge the end point of the reaction), the reaction cycle is long, etc.

Method used

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  • The preparation method of methyl tin maleate
  • The preparation method of methyl tin maleate
  • The preparation method of methyl tin maleate

Examples

Experimental program
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Effect test

Embodiment 1

[0034] The preparation method of embodiment 1 methyl tin maleate

[0035] Add 0.250L of an aqueous solution of monomethyl tin trichloride compound with a chloride ion concentration of 5.60mol / L to a 500ml three-necked flask, stir, heat to 50°C, start the dropwise addition of liquid caustic soda reaction, control the dripping speed of liquid caustic soda to 5ml / min, control The reaction temperature is 55-75°C, and the pH value of the reaction system is adjusted to 7.5 as the end point of the reaction. Insulate and react for 30 minutes, cool, and the product is filtered through a plate and frame filter press, washed with water, and squeezed (pressing pressure reaches more than 10 MPa) to obtain a wet product methyl tin oxide (tin content is about 40%-50%).

[0036] After the above-mentioned methyl tin oxide was simply crushed, it was fed into a stirred 1000ml three-necked flask filled with 600ml of n-hexane, and 0.707mol of maleic acid was added. Set up a water separator on the...

Embodiment 2

[0038] The preparation method of embodiment 2 methyl tin maleate

[0039] Add 0.250L of an aqueous solution of monomethyl tin trichloride compound with a chloride ion concentration of 6.00mol / L to a 500ml three-necked flask, stir, heat to 55°C, start dropwise addition of liquid caustic soda reaction, control the liquid caustic soda dropping rate to 9ml / min, and control The reaction temperature is 60-80°C, and the pH value of the reaction system is adjusted to 8.0 as the end point of the reaction. Insulate and react for 50 minutes, cool, and the product is filtered through a plate and frame filter press, washed with water, and squeezed (pressing pressure reaches above 10MPa) to obtain a wet product methyl tin oxide (tin content is about 40%-50%).

[0040] After the above-mentioned methyl tin oxide was simply crushed, it was fed into a stirred 1000ml three-neck flask filled with -650ml of n-hexane, and 0.78mol of maleic acid was added. Set up a water separator on the reactor, c...

Embodiment 3

[0042] The preparation method of embodiment 3 methyl tin maleate

[0043] Add 0.200L of an aqueous solution of dimethyl tin dichloride compound with a chloride ion concentration of 6.50mol / L to a 500ml three-necked flask, stir, heat to 68°C, start dropwise addition of liquid caustic soda reaction, control the dripping speed of liquid caustic soda to 7ml / min, and control The reaction temperature is 60-85°C, and the pH value of the reaction system is adjusted to 8.2 as the end point of the reaction. Heat preservation reaction for 45 minutes, cool, and the product is filtered through a plate and frame filter press, washed with water, and squeezed (pressing pressure reaches above 10MPa) to obtain the wet product methyl tin oxide (tin content is about 40%-50%).

[0044] After the above-mentioned methyl tin oxide was simply crushed, it was fed into a stirring 1000ml three-necked flask containing 650ml of n-hexane, and 0.66mol of maleic acid was added. Set up a water separator on th...

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Abstract

The invention provides a method for preparing methyltin maleate. The method includes the steps that methyl tin chloride and maleic acid serve as raw materials for preparing the methyltin maleate; a water-discarding solvent is added into wet-product methyl tin chloride and maleic acid in reacting, the mixture is subjected to a reflux reaction for discarding water at the temperature of 60 DEG C to 130 DEG C, the reaction is finished when no water is separated from an oil-water separator, and after aqueous phases are separated, a solid-phase product and a liquid-phase solvent are subjected to filter pressing and separated, the solid-phase product is washed and subjected to drying under reduced pressure through a fluidized-bed drier to obtain the finished methyl tin maleate powder, and the liquid-phase solvent can be recycled. The methyltin maleate prepared with the method can be used as a CPVC heat stabilizer; the raw materials are selected from industrial products, the reaction condition is mild and easy to control, the terminal point is easy to judge, the conversion rate is high, and the method has good industrial prospects.

Description

technical field [0001] The invention belongs to the field of chemical industry, in particular to a preparation method of methyl tin maleate. Background technique [0002] CPVC is the product of continuous chlorination of polyvinyl chloride resin, with a chlorine content of 61-68%. Physical properties, especially weather resistance, heat distortion temperature, solubility, flame retardancy, etc., are greatly improved compared with PVC. It is widely used in insulating and flame retardant materials, coatings and adhesives, foaming materials, artificial fibers, etc. However, the high chlorine content of CPVC leads to poor processing performance of the resin and a narrow processing temperature range (180-190°C). Therefore, excellent heat stabilizers are particularly important in CPVC processing. [0003] In the traditional CPVC stabilizer industry, the use of lead salt stabilizers is being gradually restricted due to the environmental protection of lead. Calcium-zinc heat stabi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/22
Inventor 戴百雄宫庭刘闯张建广张硕罗斌刘勇
Owner 湖北犇星新材料股份有限公司
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