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Preparation method of organotin PVC stabilizer
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A stabilizer and organotin technology, which is applied in the field of preparation of organotin PVC stabilizers, can solve the problems of inconvenient transportation and storage, and achieve the effect of low cost and simple synthesis method
Inactive Publication Date: 2017-09-22
毛龙飞
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Problems solved by technology
Organotin heat stabilizers have the advantages of good thermal stability, compatibility and transparency, but these heat stabilizers are all liquid, which is not very convenient in transportation and storage
Method used
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Embodiment 1
[0028] In the reaction flask, add 17g of 3,4-dichlorobenzaldehyde into 200mL of acetone, then add 5g of solid acidic catalyst HZSM-5, and under the protection of nitrogen, heat to reflux for a period of time. to room temperature, filter the reaction solution with suction, evaporate unreacted acetone under vacuum to obtain 15 g of the product 3-butene-(3,4-dichlorophenyl)-2-one, and the solid acidic catalyst HZSM-5 can be recovered Apply; 1 H NMR (400MHz, CDCl 3 )δ: 7.93(d, J=12.0Hz, 1H), 7.66(d, J=8.0Hz, 1H), 7.34(s, 1H), 7.29(s, 1H), 6.68(s, 1H), 2.86( s, 3H).
Embodiment 2
[0030] Add 20 g of 3-butene-(3,4-dichlorophenyl)-2-one into the autoclave, then add 300 mL of cyclohexane and 4 g of silver iodide addition positioning catalyst, and feed liquid ammonia into the autoclave. Make the pressure in the reaction kettle reach 0.2MPa, raise the temperature to 50°C and react for a period of time, monitor the complete reaction of the raw materials by TLC, slowly discharge the unreacted ammonia gas, evaporate the solvent in vacuum, add a certain amount of pure water, and extract the reaction solution with chloroform Multiple times, after merging the organic phases, chloroform was distilled off to obtain 17 g of 3-aminobutane-(3,4-dichlorophenyl)-2-one;1 H NMR (400MHz, DMSO-d 6 )δ: 7.71(d, J=4.0Hz, 1H), 7.42(d, J=4.0Hz, 1H), 7.11(s, 1H), 5.18(s, 2H), 3.89(s, 1H), 3.21- 3.17(m,2H),2.23(s,3H).
Embodiment 3
[0032] In the reaction flask, add 23g of 3-aminobutane-(3,4-dichlorophenyl)-2-one into 300mL of water, then add 10g of NaOH, react at room temperature for a period of time, then dropwise add tert Aminobutyl alcohol 10mL, add (Boc) after the dropwise addition 2 O 20 g, stirred overnight at room temperature. After the reaction, the reaction solution was extracted three times with 100 mL of dichloromethane, and then the organic phases were combined and concentrated to obtain 21 g of 3-Boc-aminobutane-(3,4-dichlorophenyl)-2-one; 1 H NMR (400MHz, DMSO-d 6 )δ: 7.71(d, J=4.0Hz, 1H), 7.42(d, J=4.0Hz, 1H), 7.11(s, 1H), 5.18(s, 2H), 3.89(s, 1H), 3.21- 3.17(m,2H),2.23(s,3H).
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Abstract
The invention discloses a preparation method of an organotin PVC stabilizer, and belongs to the technical field of synthesis of PVC stabilizers. According to the technical scheme, the preparation method of the organotin PVC stabilizer is technically characterized in that according to the preparation method, a specific synthetic route of the organotin PVC stabilizer is shown in the description. The preparation method of the organotin PVC stabilizer is simple, the cost is relatively low, and the effects of the prepared organotin PVC stabilizer surpass those of traditional lead-composite stabilizers, calcium-zinc composite stabilizers and organotin stabilizers.
Description
technical field [0001] The invention belongs to the technical field of synthesis of PVC stabilizers, and in particular relates to a preparation method of an organotin PVC stabilizer. Background technique [0002] Polyvinyl chloride (PVC for short) is one of the five general-purpose plastics. It is an ideal material for its low price and outstanding balance performance. It is also an ancient and active variety in the history of plastic applications. Its global output is second only to polyvinyl chloride Vinyl comes in second. my country is one of the largest producers of PVC resin. The domestic PVC industry has made great progress after more than 50 years of development. At present, there are more than 100 PVC production enterprises in China, and the production capacity ranks first among domestic synthetic resins. [0003] Generally, when PVC is heated to above 130°C, it begins to release HCl. This is because in the process of manufacturing PVC, due to auto-oxidation reactio...
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