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High-molecular-weight and multi-branched biomass plasticizer synthesized from citrate and soybean oil and preparation method thereof

A citric acid ester, large molecular weight technology, applied in the field of synthesis of biomass plasticizers, can solve the problems of complex synthesis process, unsuitable for daily life products, limited application range, etc., to achieve low mobility, volatility resistance to water/oil extraction , low volatility effect

Inactive Publication Date: 2017-05-31
CHANGZHOU UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Chinese patent application 201610204615 proposes to polymerize ricinoleic acid at high temperature to obtain a homopolymer with a molecular weight of 3000-5000, which is a plasticizer with good durability, but the synthesis process of the product is complicated, and the product color is brownish black. The scope is limited, not suitable for general life products

Method used

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  • High-molecular-weight and multi-branched biomass plasticizer synthesized from citrate and soybean oil and preparation method thereof
  • High-molecular-weight and multi-branched biomass plasticizer synthesized from citrate and soybean oil and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: in the reactor with mechanical stirring, add 300g soybean oil (contain 1.42mol unsaturated double bond about, iodine number 120gI 2 / 100g oil), 391g triethyl citrate, 20.7g boron trifluoride pyridine complex, that is: citric acid ester: unsaturated double bond=1.0 (molar ratio) in oily ester, catalyst consumption is the reaction mass weight 3%. Under the protection of nitrogen, the reaction was carried out at 140° C. for 6 hours to complete the etherification reaction. The etherification rate of the double bond (that is, the conversion rate of the etherification reaction) was 94.2%. The average molecular weight of the obtained product triethyl polycitrate soybean oil ether (referred to as TSE-1) was about 2075 g / mol. The tensile test results of the plasticized PVC test piece are listed in Table 1, and the migration performance measurement results in ethanol medium are listed in Table 2, and compared with traditional plasticizers diisooctyl phthalate (DOP...

Embodiment 2

[0025] Embodiment 2: in the reactor with mechanical stirring, add 300g soybean oil (contain 1.65mol unsaturated double bond about, iodine number 140gI 2 / 100g oil), 1047g trioctyl citrate, 13.5g methanesulfonic acid, namely: citric acid ester: unsaturated double bond=1.2 (molar ratio) in oily ester, catalyst consumption is 1% of reaction mass weight. Under the protection of nitrogen, the reaction at 120° C. was controlled for 4 hours to complete the etherification reaction. The etherification rate of the double bond was 93.8%. The average molecular weight of the obtained product trioctyl polycitrate soybean oil ether (referred to as TSE-2) is about 3500 g / mol. The tensile test results of the plasticized PVC test piece are listed in Table 1, and the migration performance measurement results in ethanol medium are listed in Table 2, and compared with traditional plasticizers diisooctyl phthalate (DOP), tributyl citrate The properties of ester (TBC) and epoxidized soybean oil (E...

Embodiment 3

[0026] Embodiment 3: in the reactor with mechanical stirring, add 300g soybean oil (contain 1.48mol unsaturated double bond about, iodine number 125gI 2 / 100g oil), 530g tributyl citrate, 2.5g vitriol oil, namely: citric acid ester: unsaturated double bond=1.0 (molar ratio) in oily ester, catalyst consumption is 0.3% of reaction mass weight. Under nitrogen protection, the etherification reaction was completed at 80° C. for 8 hours. The etherification rate of the double bond was 90.9%. The average molecular weight of the resulting product tributyl polycitrate soybean oil ether (referred to as TSE-3) is about 2500 g / mol. The tensile test results of the plasticized PVC test piece are listed in Table 1, and the migration performance measurement results in ethanol medium are listed in Table 2, and compared with traditional plasticizers diisooctyl phthalate (DOP), tributyl citrate The properties of ester (TBC) and epoxidized soybean oil (ESO) were compared.

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Abstract

The invention belongs to the field of a synthetic material plasticizer and provides a synthesis method of a biomass plasticizer. The synthesis method takes citrate and soybean oil as raw materials to synthesize a new high-molecular-weight and multi-branched biomass plasticizer through a catalytic etherification reaction and the average molecular weight is about 2075g / mol-3500g / mol. Compared with a traditional phthalate ester plasticizer, the substance has the characteristics of safety and no toxin, greenness and environment friendliness, low mobility, low volatility and water / oil extraction resistance, so that the plasticizing effect is durable and a PVC (Polyvinyl Chloride) product plasticized by a synthetic product has long-term durability.

Description

technical field [0001] The invention belongs to the field of plasticizers for synthetic materials, and relates to a method for synthesizing biomass plasticizers. Specifically, it involves a chemical reaction between citric acid ester and unsaturated double bond-containing oil ester to synthesize a macromolecular biomass plasticizer. [0002] technical background [0003] Phthalate plasticizers, because they contain aromatic rings, are not easy to biodegrade, and have the possibility of carcinogenicity, the European Union has issued a number of laws and directives to strictly limit the use of phthalate plasticizers in food In packaging, medical supplies, children's toys and other polyvinyl chloride (hereinafter referred to as PVC) products that are in close contact with the human body, it is imperative to develop and produce green plasticizers. [0004] Epoxidized soybean oil has been used as a non-toxic and environmentally friendly biomass plasticizer, widely used as a plast...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L27/06C08L91/00
CPCC08L27/06C08L91/00
Inventor 单玉华刘入强单炜韬王超封东廷毛翠霞
Owner CHANGZHOU UNIV