Preparation method of stearoylbenzoylmethane and application thereof to molding processing of thermoplastic resin
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A technology of stearoyl benzoyl methane and fatty acyl benzoyl methane is applied in the field of preparation of beta-diketones, can solve the problems of toxic crystallization solvent, many by-products, and high raw material cost, and achieves cost reduction and performance improvement Improved, efficient recycling
Active Publication Date: 2012-06-20
SHANDONG RUIFENG CHEM
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[0003] The preparation method of stearoylbenzoylmethane in the prior art has the problem that the cost of main raw materials is high, and also has a long condensation reac
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Embodiment 1
[0057] Prepare Stearoylbenzoylmethane according to the following steps
[0058] ①. Synthesis of methyl stearate
[0059] Put stearic acid and methanol into a three-necked flask according to the set formula, raise the temperature to 70°C, and after the stearic acid is completely melted, add concentrated sulfuric acid dropwise, and reflux for 2 to 3 hours.
[0060] a. Esterification process conditions
[0061] Stearic acid / methanol molar ratio 1:3~1:4
[0062] Esterification reaction temperature is 65~70°C
[0063] Reaction time hours 2~3
[0064] b.washing
[0065] Put the esterification solution from step a into a separatory funnel, wash with 200ml water 4-5 times until pH=7. Stand to separate the phases, the organic phase is crude methyl stearate, to be distilled;
[0066] c. Distillation
[0067] Put the crude methyl stearate from step b into a three-necked flask, raise the temperature to 100° C., and distill under reduced pressure to remove low-boiling fractions to obt...
Embodiment 2～ Embodiment 5
[0087] According to the method and step of Example 1, the stearoylbenzoylmethane product of the present invention is prepared according to the formula of Table 1
[0088] Table 1
[0089] Raw material and yield
Embodiment 6
[0091] Stearoylbenzoylmethane of the present invention is as follows according to the application formula of mass fraction agent in PVC resin molding process:
[0092]
[0093] Weigh 120g of the test materials mixed according to the above formula, and masticate them on a double-roll plasticizer with a roller distance of 1mm. Sampling at 90 seconds, 120 seconds, 240 seconds, 360 seconds, and 510 seconds for comparison is the dynamic thermal stabilization time. Record the color change time from light yellow, light red, red, deep red, brown black, black, and compare.
[0094] Test Results:
[0095] 90 seconds
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Abstract
The invention discloses a preparation method of stearoylbenzoylmethane and an application thereof to molding processing of thermoplastic resin, which belong to preparation of a compound which only contains a CO radical and is only connected with a carbon atom or a hydrogen atom, and particularly relate to preparation of beta-diketone. The stearoylbenzoylmethane is obtained by undergoing a condensation reaction on methyl stearate and acetophenone in an alkaline environment, wherein the methyl stearate is obtained by taking stearic acid and methanol as raw materials, taking sulfuric acid as a catalyst and undergoing an esterification reaction. The invention provides a preparation method of the stearoylbenzoylmethane, which has the advantages of low costs of major raw materials, short condensation reaction period, small quantity of byproducts, high yield of stearoylbenzoylmethane, complete recycling of a solvent, nontoxicity of a crystallization solvent and high crystal yield. The condensation yield is up to 88 percent, the solvent is completely recycled, the crystallization solvent is nontoxic and environmentally-friendly, the crystal yield is up to 95 percent, and the purity of a product, i.e., stearoylbenzoylmethane is up to 98 percent. The invention further provides a method for applying the stearoylbenzoylmethane to molding processing of thermoplastic resin.
Description
technical field [0001] The invention relates to a preparation method of stearoylbenzoylmethane and its application in thermoplastic resin molding processing. It belongs to the preparation of compounds containing CO groups and only connected to carbon or hydrogen atoms, especially the preparation of β-diketones. Background technique [0002] Stearoylbenzoylmethane is an important light and heat stabilizer for thermoplastics with β-diketone structure. It can be compounded with a variety of stabilizers, and through the synergistic effect between components, it can effectively improve the stability of polyvinyl chloride. The transparency and weather resistance of the product can avoid precipitation and "zinc burning" during processing. It can not only reduce the coloring of plastic products in the early stage, but also improve the thermal stability in the later stage. Stearoylbenzoylmethane products are non-toxic and tasteless, so they are widely used in food and pharmaceutica...
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