Preparation method for cold-resistant plasticizer dioctyl sebacate

A technology of dioctyl sebacate and cold-resistant plasticizer, which is applied in the field of preparation of PVC additives, can solve the problems of low product yield and purity, long esterification reaction time, and incomplete catalytic reaction, etc. The effect of esterification reaction time, reduction of water consumption and sewage discharge, and quality assurance

Inactive Publication Date: 2016-03-16
ANHUI XIANGFENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Dioctyl sebacate is a cold-resistant plasticizer that has been industrialized for many years. In the prior art, acid is still used as a catalyst, and the production process of first neutralizing, washing with water, and dealcoholization is adopted; the shortcomings of its existence are: corrosion to equipment High resistance, incomplete catalytic reaction, long esterification reaction time and incomplete neutralization, prone to emulsification, high energy consumption, low product yield and purity

Method used

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  • Preparation method for cold-resistant plasticizer dioctyl sebacate

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Experimental program
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specific Embodiment 1

[0028] A kind of preparation method of cold-resistant plasticizer dioctyl sebacate described in the present embodiment, comprises the following steps:

[0029] Step 1, esterification reaction process

[0030] Add 2940 kilograms of 2-ethylhexanol and 1200 kilograms of sebacic acid into 6m by mass ratio 2.45:1.0 3 In the esterification reaction kettle, the temperature was raised to 150°C while stirring, 5.0 kg of tetraisopropyl titanate was added, and the temperature was raised to 215°C. After 3.5 hours of reaction, samples were taken, and the acid value of the reaction product was measured to be 0.185 mgKOH / g .

[0031] Step 2, dealcoholization process

[0032] After the esterification reaction is complete, dealcoholize under normal pressure for 1 hour at 190°C to remove 1200 kg of excess alcohol, and then dealcoholize in vacuum for 30 minutes at a vacuum degree of -0.085 to -0.075MPa to remove excess alcohol and 162 kg of partial esters, the acid value of the detected produ...

specific Embodiment 2

[0041] A kind of preparation method of cold-resistant plasticizer dioctyl sebacate described in the present embodiment, comprises the following steps:

[0042] Step 1, esterification reaction process

[0043] According to the ratio of mass ratio 2.5:1.0, put 2800 kg of 2-ethylhexanol and 1120 kg of sebacic acid into 6m 3 In the esterification reaction kettle, the temperature was raised to 160°C while stirring, 4.8 kg of butyl phthalate was added, and the temperature was raised to 220°C to carry out the esterification reaction; after 3 hours, a sample was taken, and the acid value of the product was measured to be 0.178mgKOH / g .

[0044] Step 2, dealcoholization process

[0045] After the esterification reaction is completed, dealcoholize under normal pressure at 205°C for 1 hour to remove 1150 kg of excess alcohol, and then dealcoholize in vacuum for 40 minutes at a vacuum degree of -0.090 to -0.080 MPa to remove excess alcohol and 172 kg of partial esters; the acid value of ...

specific Embodiment 3

[0054] A kind of preparation method of cold-resistant plasticizer dioctyl sebacate described in the present embodiment, comprises the following steps:

[0055] Step 1, esterification reaction process

[0056] According to the mass ratio of 2.6:1.0, put 2990 kg of 2-ethylhexanol and 1150 kg of sebacic acid into the esterification reaction kettle, heat up to 155 °C while stirring, add 4.6 kg of tetramethyl titanate, and heat up After the esterification reaction was carried out at 225° C. for 4.0 hours, a sample was taken, and the acid value of the product was measured to be 0.186 mgKOH / .

[0057] Step 2, dealcoholization process

[0058] After the esterification reaction is completed, dealcoholize under normal pressure for 1 hour and 20 minutes at 200°C to remove 1,260 kg of excess alcohol, and then use vacuum dealcoholization for 40 minutes at a vacuum degree of -0.090 to -0.080 MPa to remove excess alcohol. 220 kg of alcohols and some esters; the acid value of the tested pro...

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Abstract

The invention relates to a preparation method for a cold-resistant plasticizer dioctyl sebacate, and belongs to the field of PVC auxiliary agents. The preparation method comprises the following steps: esterification, dealcoholysis, neutralization, distillation, adsorption and press filtration. The technical scheme employs 2-ethylhexanol and sebacic acid as raw materials and employs one or more titanates as a catalyst for esterificatoin, and then excessive 2-ethylhexanol is removed; then neutralization is performed, and a dioctyl sebacate crude product is prepared; and then the dioctyl sebacate crude product is subjected to reduced-pressure distillation, adsorption and press filtration, the high-quality high-yield high-purity cold-resistant plasticizer dioctyl sebacate product is prepared. The product quality reaches super grade standard.

Description

technical field [0001] The invention relates to a preparation method of a cold-resistant plasticizer dioctyl sebacate, and belongs to the technical field of preparation methods of PVC additives. Background technique [0002] Plasticizers are a class of "solvent-like" substances. Adding it to materials such as plastics, resins or elastomers can improve their processability, increase plasticity, flexibility, stretchability or expansion. Adding a plasticizer can reduce the melt viscosity, glass transition temperature and elastic modulus of the plastic without changing the basic chemical properties of the plasticized substance. [0003] A plasticizer with low viscosity and low viscosity coefficient can reduce the glass transition temperature of the polymer, making hard and rigid plastic soft and tough; plastic products used under low temperature conditions need to add plasticizers with cold resistance , and the cold resistance of the plasticizer is closely related to its struc...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C67/48C07C67/62C07C67/54C07C67/56C07C69/50
CPCC07C67/08C07C67/48C07C67/54C07C67/56C07C67/62C07C69/50
Inventor 潘学松
Owner ANHUI XIANGFENG NEW MATERIALS
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