Preparation method of cyclic trimethylolpropane formaldehyde

A trimethylolpropane formal and cyclic technology, which is applied in the field of preparation of cyclic trimethylolpropane formal, can solve the problems of unsuitability for large-scale industrial production, cumbersome process, poor product quality, etc., and achieve reaction The effect of sufficient heat utilization, economical process and short reaction time

Inactive Publication Date: 2018-08-10
天津博奥新材料科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The CTF yield of this method can reach up to 96.8%. However, this method is carried out in a reactive distillation device, which requires two-step reactions of acetalization and acidolysis at different temperatures, and the process of acetalization m

Method used

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  • Preparation method of cyclic trimethylolpropane formaldehyde

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Embodiment 1

[0023] Add 1340g of trimethylolpropane and 300g of paraformaldehyde into a stirred tank reactor, add 400g of toluene as a solvent, heat to 100°C, rotate at 22r / min, add 10g of sulfuric acid as a catalyst, and add 5g of ZSM -5 is auxiliary agent. After reaction for about 2h, low-pressure evaporation is carried out at an absolute pressure of 5KPa. After evaporation, the solution in the kettle is filtered, after removing the auxiliary agent and other solid substances, it enters the distillation tower for low-pressure rectification, the pressure is about 3KPa , The reflux ratio is 1:6, and the top of the tower is CTF product. The product CTF yield is 98%, the product purity is 98.8%, the APHA color number is 10, the sodium content is 11 ppm, and the water content is 0.2%.

Embodiment 2

[0025] Add 1340g of trimethylolpropane and 811g of formaldehyde solution into a stirred tank reactor, add 200g of ethanol as solvent, heat to 85°C, rotate at 18r / min, add 12g of ammonium bisulfate as a catalyst, and add 8g of MCM-41 is an auxiliary agent. It is reacted while vacuuming at an absolute pressure of 7KPa. After reacting for about 4h, the solution in the kettle is filtered to remove the auxiliary agent and other solid materials, and then enter the rectification tower for low-pressure rectification, the pressure is about 5KPa , Reflux ratio is 1:5, and the top of the tower is CTF product. The CTF yield of the product is 97.8%, the product purity is 98.5%, the APHA color number is 15, the sodium content is 10 ppm, and the water content is 0.3%.

Embodiment 3

[0027] Add 670Kg trimethylolpropane and 406Kg formaldehyde solution into a stirred reactor, heat to 95°C, rotate at 12r / min, add 5Kg sodium hydrogen sulfate as a catalyst, and react while vacuuming at an absolute pressure of 6KPa. After about 3h, filter the solution in the kettle to remove solid matter, then enter the rectification tower for low-pressure rectification, the pressure is about 4KPa, the reflux ratio is 1:5, and the top of the tower is the CTF product. The product CTF yield is 99.2%, the product purity is 99%, the APHA color number is 10, the sodium content is 12 ppm, and the water content is 0.12%.

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Abstract

The invention relates to a preparation method of cyclic trimethylolpropane formaldehyde (CTF or MCF), mainly aiming at solving the problems in the prior art that synthetic conditions of trimethylolpropane formal are harsh, a process route is complicated, the purity of a product is low and the APHA color number is high. The preparation method comprises the following steps: taking trimethylolpropane(TMP) as a raw material, and mixing TMP, aldehyde, a solvent, a catalyst and an auxiliary agent according to a certain ratio; reacting at 60 to 120 DEG C for 0.1 to 6h; evaporating under low pressure, filtering and rectifying to obtain a cyclic trimethylolpropane formaldehyde product with the quality purity being greater than or equal to 98 percent and the color number APHA being less than or equal to 20. By adopting the preparation method provided by the invention, the problems are solved relatively well; a synthesis technology is simple and conditions are moderate, so that the preparation method can be widely applied to large-scale industrial production.

Description

Technical field [0001] The invention relates to a method for preparing cyclic trimethylolpropane formal, in particular to a method for preparing cyclic trimethylolpropane formal with simple process, mild conditions and high product quality. technical background [0002] Cyclic trimethylolpropane formal (hereinafter referred to as CTF), chemically named 5-ethyl-1,3-dioxane-5-methanol, CAS: 5187-23-5, is a monocyclic monohydric alcohol It is a colorless liquid with low odor and outstanding performance. It is suitable for the production of radiation-curable monomer esters. It is a monofunctional reactive diluent with lower shrinkage and better reactivity. It can be used to prepare low odor and high glass. Compared with traditional mono-acrylate monomers, it has the advantages of low viscosity, low odor, high reactivity and excellent adhesion, etc., which can make the curing speed faster. Faster and higher hardness. As a one-component monomer, it can improve the adhesion of coatings...

Claims

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Application Information

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IPC IPC(8): C07D319/06
CPCC07D319/06
Inventor 张舜光
Owner 天津博奥新材料科技有限公司
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