Preparation process of thermal stabilizer of tin methyl thio hydroacetate tin isooctoate for PVC

A technology of isooctyl tin methyl thioglycolate and isooctyl thioglycolate is applied in the field of preparation of isooctyl tin methyl thioglycolate as heat stabilizer for PVC, and can solve the problem of high process equipment conditions and energy consumption, Can not really improve product quality, loss of raw material isooctyl thioglycolate, etc., to achieve the effect of reducing energy consumption, low production equipment requirements, and shortening reaction time

Inactive Publication Date: 2009-06-24
江从宇
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process and conditions of this method are more complicated, and a large amount of solvent must be added. To recover the solvent, it is necessary to invest in a solvent recovery device, which increases the production cost of the product.
At present, the latest domestic report such as Chinese patent CN1439670A adopts the direct reaction method. Although the method overcomes the above-mentioned disadvantages, the required process equipment conditions and energy consumption are relatively high. Under the true penetration and temperature conditions of the method, raw materials There will also be a certain degree of loss of isooctyl thioglycolate
If the original baking intermediate methyl tin chloride used in it is not purified by a certain method, the resulting product will have a certain color and smell, and the purpose of improving product quality cannot really be achieved.

Method used

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  • Preparation process of thermal stabilizer of tin methyl thio hydroacetate tin isooctoate for PVC

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Transfer the mixture of 250 grams of methyl tin chloride (dimethyl tin dichloride: monomethyl tin trichloride = 80: 20) into a 500 ml distillation flask, and use an air duct to connect with a 2000 ml reaction flask equipped with electromagnetic stirring Connect, add 450 grams of isooctyl thioglycolate and 0.2 gram of triethylamine in the reaction bottle, the reaction bottle is connected with the vacuum pump, turn on the vacuum pump and electromagnetic stirring and heat the distillation bottle to start the purification and absorption of the intermediate, and use a water bath to keep the temperature of the absorption solution at Between 35°C and 40°C, when the weight of the reaction bottle increases to 220g-223g, stop the distillation and purification, remove the distillation device, change the magnetic stirring to strong stirring, and add to the reaction bottle several times within 1 hour 120 grams of powdery sodium carbonate, the reaction temperature of adding alkali is ...

Embodiment 2

[0016] In a 2000ml reaction flask equipped with strong stirring, add 450 grams of isooctyl thioglycolate and 0.2 grams of triethylamine, start stirring and keep the temperature between 35 ° C and 40 ° C, add 223 grams of purified methyl tin chloride Compound mixture (dimethyl tin dichloride: monomethyl tin trichloride = 80: 20), after the added intermediate is completely dissolved, add 120 grams of powder in the reaction bottle several times within 1 hour Sodium carbonate, the reaction temperature of adding alkali is 40°C-45°C, after adding alkali, continue to stir for 0.5 hours, filter to obtain 668.0 g of colorless transparent oily liquid product, the yield is 99.2%.

[0017] The response is as follows:

[0018] (CH 3 ) 2 SnCl 2 +2HSCH 2 COOC 8 h 17 →(CH 3 ) 2 Sn(SCH 2 COOC 8 h 17 ) 2 +2HCl

[0019] CH 3 SnCl 3 +3HSCH 2 COOC 8 h 17 →CH 3 Sn(SCH 2 COOC 8 h 17 ) 3 +3HCl

[0020] Product Analysis Results:

[0021] Tin content: 19.45%, sulfur content: 11...

Embodiment 3

[0022] Embodiment 3: thermal stabilizer performance comparison test

[0023] Recipe: polyhydroethylene 100 parts

[0024] 2 parts isooctyl phthalate

[0025] Anti-buffer improver 5 parts

[0026] Organotin added as required

[0027] Operation: Set the roller temperature of the double-roll plastic refining machine to 165°C. After the temperature rises stably, add the primary mixed material to the upper part of the roll gap for plastic refining. Observe that the color of the material is uniform, there is no hair grain on the cross-section, the surface is smooth and has certain When the strength is reached, the rolling process is over, quickly take a one-inch square sample blank, heat the upper and lower templates of the flat filling machine press to 180°C, set the appropriate pressure, place the cut sample between the stainless steel templates, put At the center of the press workbench, start the press, close the mold and pressurize after the mold preheats th...

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Abstract

The invention discloses a preparation method of a heat stabilizer for PVC, isooctyltin methyl thioglycolate, which comprises adding methyl tin chloride to an equimolar amount of isooctyl thioglycolate, and the temperature is 0°C. React at -50°C for 1-6 hours, then under stirring conditions, the stirring speed is 60-300 rpm, add 0.02%-0.1% of organic base and 10%-30% of inorganic base, at a temperature of 0°C React at -50°C for 0.5-1 hour, and filter to obtain the product. The method has simple technological process, low requirements on production equipment and technological conditions, less energy consumption, no solvent and post-treatment, and excellent processing performance and product performance of the final product.

Description

technical field [0001] The invention relates to a preparation method of a heat stabilizer for PVC, isooctyltin methyl thioglycolate. Background technique [0002] Isooctyltin methyl thioglycolate (a mixture of isooctyltin monomethyltrithioglycolate and isooctyltin dimethyl dimercaptoacetate) is a PVC plastic heat stabilizer that is widely used and has excellent performance. agent, the synthetic method provided by the prior art, such as Chinese patent CN1117495A, CN1137048A, usually adopts raw material isooctyl thioglycolate, water, sodium bicarbonate, solvent to be added in the reactor, in the dripping of methyl tin chloride The reaction is carried out in an aqueous solution, and the reactant undergoes strict post-treatment to obtain the product after removing low boilers. Using this method, the process and conditions are more complicated, and a large amount of solvent must be added. To recover the solvent, it is necessary to invest in a solvent recovery device, which incre...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L27/06C08K5/57
Inventor 江从宇
Owner 江从宇
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