A kind of method for preparing pvc rare earth heat stabilizer by solid phase method

A technology of rare earth heat stabilizer and solid-phase method, which is applied in the preparation of carboxylic acid amide, chemical instruments and methods, and the preparation of organic compounds, etc., and can solve the problems of endangering the rapid development of PVC products and metal pollution of stabilizers.

Inactive Publication Date: 2020-01-21
SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND +1
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Problems solved by technology

[0019] At present, most of the PVC heat stabilizers are metal heat stabilizers, so these stabilizers all have the problem of metal pollution, which endangers the rapid development of PVC products. Therefore, developing new metal-free heat stabilizers to replace or partially replace metal stabilizers is currently the One of the research directions of heat stabilizers

Method used

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  • A kind of method for preparing pvc rare earth heat stabilizer by solid phase method
  • A kind of method for preparing pvc rare earth heat stabilizer by solid phase method
  • A kind of method for preparing pvc rare earth heat stabilizer by solid phase method

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Experimental program
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Effect test

Embodiment 1-16

[0046] 1) Synthesis of N-hexylmaleamic acid:

[0047] 1.1) Dissolve a certain amount of 0.1mol maleic anhydride in 10ml ethyl acetate to obtain solution A;

[0048] 1.2) Dissolve 0.1mol n-hexylamine in an appropriate amount of 10ml ethyl acetate to obtain solution B;

[0049] 1.3) Add solution B dropwise to solution A under constant stirring, heat, filter with suction after the reaction is completed, wash with ethyl acetate, and dry in vacuum to synthesize N-hexylmaleamic acid;

[0050] 2) Prepare N-hexylmaleamic acid lanthanum by solid-phase method, the specific method is: take 0.05mol N-hexylmaleamic acid and 0.016mol lanthanum hydroxide in a mortar, grind at 40°C for 10min , placed in a vacuum drying oven at a baking temperature of 90°C for 40 minutes, when the quality of the product no longer changes, take it out of the drying oven, wash the obtained product with absolute ethanol and distilled water 5 times, and dry it in a vacuum oven Obtain N-hexylmaleamido lanthanum c...

Embodiment 17

[0064] The invention adopts the Congo red method to test the static thermal stability of the complex to PVC. Mix the compound prepared in Example 7 with PVC, heat in an oil bath at 180°C under the condition of isolation from air, and record the time required for the Congo red test paper to turn blue. The effects of complexes on the stability of PVC with different contents in PVC were studied. The experimental formula is shown in Table 2.

[0065] The thermal stability experiment formula of table 2 complex

[0066] serial number Proportion PVC / (g) Complex / (g) 1 0％ 4.00 0.00 2 2％ 3.92 0.08 3 4％ 3.84 0.16 4 5％ 3.80 0.20 5 7％ 3.72 0.28 6 10％ 3.60 0.40 7 15％ 3.40 0.60

[0067] Through the experimental data, the above figure 1 . from figure 1 It can be seen from the figure that as the content of the complex increases, the stability of PVC is better. When the content of the complex reaches 10%, the thermal stab...

Embodiment 18

[0069] pass figure 2 It is the infrared spectrogram of N-hexylmaleamic acid and image 3 The N-hexyl maleamic acid lanthanum infrared spectrogram comparison and the infrared spectrum peak frequency and group comparison table obtained for embodiment 7 obtain the following conclusions, the carboxyl νOH of the ligand occurs at 3141cm -1 At , the characteristic absorption peak of νOH disappeared after the complex was formed, indicating that the hydrogen ion in the carboxyl group was replaced by lanthanum, and the carboxyl group participated in the reaction. Compared with the ligand, in the infrared spectrum of the complex, νC-N has a red shift of 29-35cm -1 , δN-H red shifted by 4-8cm -1 , the stretching vibration of C=O has little change and remains at 1631cm -1 nearby. This shows that the lanthanum ion forms a coordination bond with the lone pair of electrons of the nitrogen atom in the amide, which makes the original chemical bond length slightly elongated, and the bond fo...

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Abstract

The present invention relates to a method for preparing a novel environmentally friendly PVC rare earth heat stabilizer by a solid phase method, and the method comprises the following steps: 1) synthesizing N-hexylmaleamic acid; and 2) synthesizing a N-hexylmaleamic acid lanthanum complex, to be more specific, taking a certain amount of N-hexylmaleamic acid and a certain amount of lanthanum hydroxide to put in a mortar, grinding at 20-40 DEG C for 5-20min, placing in a vacuum drying oven for drying at 80-110 DEG C for 10-40min, when the quality of the product no longer changes, taking the product from the drying oven, washing the obtained product with anhydrous ethanol and distilled water for 3-5 times, drying in the vacuum drying oven to a constant weight to obtain the N-hexylmaleamic acid lanthanum complex. The novel environmentally friendly PVC rare earth heat stabilizer is prepared by the solid phase method, the PVC coloring property can be tested by combination of a heat aging box method with UV-visible spectrophotometry, and the thermal stability property is measured by a Congo red test paper method.

Description

technical field [0001] The invention belongs to the field of PVC heat stabilizers, and in particular relates to a preparation method of a PVC rare earth heat stabilizer. Background technique [0002] In 2010, the world's plastic output was as high as 300 million tons, and in 2011, China's primary plastic output was 47.98 million tons. Plastic products are closely related to people's lives because of their light weight, good comprehensive performance, and easy processing and molding, and are favored by people. However, the decomposition temperature and plasticizing temperature of plastic products are relatively close, resulting in poor thermal stability and processing performance, which limits the application range of plastic products. Adding additives can effectively improve the performance of plastic products, among which heat stabilizers can effectively improve the thermal stability of plastic and rubber products. According to the thermal decomposition mechanism of polyv...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/12C07C231/02C07C233/09C08K5/20C08L27/06
CPCC07C231/02C07C231/12C08K5/0091C08L2201/08C07C233/09C08L27/06
Inventor 康洁李侃社屈孟男曲建林白燕
Owner SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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