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Preparation method of low-migration di (2-ethylhexyl) terephthalate plasticizer

A technology of di-terephthalic acid and terephthalic acid, which is applied in the field of preparation of low-migration terephthalate diester plasticizers, can solve the problem of affecting the appearance and feel of PVC products, increasing the complexity of the processing process, and increasing the manufacturing cost and other issues, to achieve the effect of good processability, simplified production process and good compatibility

Pending Publication Date: 2022-07-29
NANYA PLASTICS CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Bis(2-ethylhexyl) terephthalate (di-2-ethylhexyl terephthalate, DOTP) is a non-toxic and environmentally friendly non-phthalic plasticizer, which is often used in the molding and processing of polyvinyl chloride (PVC) resin. PVC is plasticized and easy to process; however, the compatibility between DOTP and PVC is poor, and it is easy to precipitate on the surface of PVC products (oil spit phenomenon), which affects the appearance and feel of PVC products
[0003] There is a solution in the prior art, which is to add additional components (such as citric acid ester) to the PVC material, and inhibit the migration of DOTP through the interaction between it and DOTP, thereby improving the oil spit phenomenon of PVC products ; However, additional ingredients will increase manufacturing costs
There is another solution in the prior art, which is to apply an acrylic coating on the surface of PVC products. Although the acrylic coating can reduce the migration of DOTP and also achieve the purpose of improving the oil spit phenomenon of PVC products, this method It will not only increase the manufacturing cost, but also increase the complexity of the processing process

Method used

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  • Preparation method of low-migration di (2-ethylhexyl) terephthalate plasticizer

Examples

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preparation example

[0039] The preparation method of low mobility terephthalate di(2-ethylhexyl) ester plasticizer of the present invention, comprises the following steps:

[0040] 1) Use terephthalic acid (PTA) or its derivative, 2-ethylhexanol (2-EH) and 911 alcohol mixture as raw materials, wherein the equivalent molar ratio of PTA, 2EH and 911 alcohol is 1:2.2 -3.8:0.029, based on the total weight of the reactants (PTA and 2-EH weight), take 23-35wt% of terephthalic acid or its derivatives, 65-77wt% of 2-EH alcohol and 0.0014wt% of 911 alcohol for addition;

[0041] 2) based on the total amount of di(2-ethylhexyl) terephthalate with low mobility, take 0.1-6wt% metal-containing catalyst or inorganic acid catalyst as an esterification catalyst to add;

[0042] 3) Under the reaction pressure of 5-1033 mbar and the reaction temperature of 200-250 ° C, preferably the reaction pressure of 15-950 mbar and the reaction temperature of 220-240 ° C, for step 1) terephthalic acid or its derivatives, 2 et...

Embodiment 1

[0067] According to the formula in Table 1, take 120 g of terephthalic acid (PTA), 310 g of 2EH alcohol, 0.168 g of 911 alcohol (diluted with 2-EH), and the amount of catalyst TIPT (tetraisopropyl titanate) added is 0.6 g, terephthalic acid, 2EH alcohol, 911 alcohol mixture and catalyst are simultaneously fed into a four-necked flask, the reaction temperature is 225 ° C under nitrogen, the reaction time is 6 hours, and the reaction pressure is 5-1033 mbar, which must be removed during the reaction process. When the water is reacted to an acid value of 1 mgKOH / g or less, neutralize it with an aqueous solution of an alkali metal oxyhydroxide until the acid value of the synthesis reaction mixture is less than 0.07 mgKOH / g, then perform distillation to reduce the alcohol content to 300 ppm or less, and then filter After purification, low-migration bis(2-ethylhexyl) terephthalate was obtained and used as a plasticizer.

[0068] The basic physical properties and processing propertie...

Embodiment 2

[0070] As in the preparation method of Example 1, according to the formula in Table 1, the 911 alcohol therein was changed to 2-PH (2-phenylphenol). Under the same process conditions, the esterified DOTP plasticizer was obtained.

[0071] The basic physical properties and processing properties of the prepared DOTP plasticizer ester compound, the test results are shown in Table 1, wherein, the hue: 12APHA, acid value: 0.06mgKOH / g, purity: 99.8%, migration rate: 3.01% (at 80PHR), Transparency: 89.5%, and plasticization coefficient: 1.05.

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Abstract

The invention discloses a preparation method of a low-migration di (2-ethylhexyl) terephthalate plasticizer, which comprises the following steps: when terephthalic acid and 2-ethylhexanol are subjected to esterification reaction, adding short carbon chain unit alcohol and long carbon chain unit alcohol to graft and modify the formed dioctyl terephthalate at the reaction temperature of 30-225 DEG C under the reaction pressure of 80-1033 mbar. The low-mobility di (2-ethylhexyl) terephthalate prepared by the preparation method disclosed by the invention can be used as an environment-friendly functional plasticizer, and has low mobility and good processability.

Description

technical field [0001] The present invention relates to a preparation method of di(2-ethylhexyl) terephthalate, in particular to a preparation method of di(2-ethylhexyl) terephthalate plasticizer with low mobility. The prepared low-migration di(2-ethylhexyl) terephthalate can be applied to polyvinyl chloride (PVC) products as a low-migration environment-friendly plasticizer. Background technique [0002] Plasticizers are widely used in the processing of plastics, rubber, etc. The purpose is to increase their plasticity and processability, so that the finished product has excellent softness, elasticity and toughness. It is one of the commonly used additives in the polymer industry. Di-2-ethylhexyl terephthalate (DOTP) is a non-toxic, environmentally friendly, non-phthalate plasticizer, commonly used in the molding of polyvinyl chloride (PVC) resins. PVC is plasticized and easy to process; however, the compatibility between DOTP and PVC is poor, and it is easy to precipitate ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C67/48C07C69/82C08K5/12C08L27/06
CPCC07C67/08C07C67/48C08K5/12C08L27/06C07C69/82C08K5/0016
Inventor 廖德超庄荣仁陈仲裕林训民
Owner NANYA PLASTICS CORP