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A device and method for rectifying and purifying 3-isocyanatopropyltriethoxysilane

A technology of ester group propyltriethoxysilane and isocyanic acid, which is applied in the direction of silicon organic compounds, can solve the problems of cumbersome operation, highly toxic raw materials, and strict requirements for tail gas treatment, so as to improve extraction efficiency and avoid polymerization deterioration Effect

Active Publication Date: 2016-08-17
ASTATECH CHENGDU BIOPHARM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, this coupling agent is mainly prepared by the reaction of 3-aminopropyltriethoxysilane with phosgene, or the reaction of 3-aminopropyltriethoxysilane with solid phosgene (triphosgene) However, benzene or toluene is used as a solvent in the process. Because of its toxicity, the requirements for solvent recovery and tail gas treatment are harsh, and the operation is cumbersome; at the same time, phosgene or triphosgene is used as raw material, which has the disadvantages of highly toxic raw materials.

Method used

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  • A device and method for rectifying and purifying 3-isocyanatopropyltriethoxysilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025]Embodiment 1: In the first stage, feed cooling water at 50°C into the spiral tube 13, and at the same time adjust the vacuum to 2mmHg and raise the temperature of the kettle to 78°C. Prepare 392g of DMF solvent; in the second stage, feed cooling water at 85°C into the spiral tube 13, and simultaneously adjust the vacuum to 2mmHg and raise the temperature of the kettle to 98°C. After 9min, the former component accepts Make the DMF solvent of 98g in the tank 3; In the third stage, close the shut-off valve I9 ​​and open the shut-off valve II10, pass into the cooling water of 100 ℃ in the spiral pipe 13, simultaneously vacuum degree is adjusted to 2mmHg and still temperature is raised to After 15 minutes at 125°C, 390 g of 3-isocyanatopropyltriethoxysilane with a purity of 97% was obtained in the rear component receiving tank 4.

Embodiment 2

[0026] Embodiment 2: Pass into the cooling water of 53 ℃ in the helical tube 13, simultaneously adjust the vacuum to 2mmHg and raise the kettle temperature to 80 ℃, after 15min, make 400g of DMF solvent; in the second stage, feed 88°C cooling water into the spiral tube 13, simultaneously adjust the vacuum degree to 2mmHg and raise the temperature of the kettle to 100°C. Obtain the DMF solvent of 100g; In the third stage, close the shut-off valve I9 ​​and open the shut-off valve II10, pass into the cooling water of 103 DEG C in the helical pipe 13, simultaneously vacuum degree is adjusted to 2mmHg and still temperature is raised to 127 DEG C, through After 16 minutes, 390-410 g of 3-isocyanatopropyltriethoxysilane with a purity of 98% was prepared in the rear component receiving tank 4.

Embodiment 3

[0027] Example 3: In the first stage, feed cooling water at 55°C into the spiral tube 13, and at the same time adjust the vacuum to 2mmHg and raise the temperature of the kettle to 82°C. Prepare 409g of DMF solvent; in the second stage, feed 90°C cooling water into the spiral tube 13, and simultaneously adjust the vacuum to 2mmHg and raise the temperature of the kettle to 102°C. After 12min, the former component received Make the DMF solvent of 101g in the tank 3; In the third stage, close the shut-off valve I9 ​​and open the shut-off valve II10, pass into the cooling water of 105 ℃ in the spiral pipe 13, simultaneously vacuum degree is adjusted to 2mmHg and still temperature is raised to After 16 minutes at 130°C, 390-410 g of 3-isocyanatopropyltriethoxysilane with a purity of 99% was prepared in the rear component receiving tank 4.

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Abstract

The invention discloses a device for rectifying and purifying 3-isocyanatopropyl triethoxysilane, which comprises a distillation tower (1), a condenser (2), a front component receiving tank (3) and a rear component receiving tank The tank (4), the outlet port of the vacuum pump (5) is connected to the inlet of the front component receiving tank (3) and the rear component receiving tank (4), and the packing tower (6) is filled with Pall rings The filler (11), the spiral separator (8) is provided with a spiral tube (13), and the water inlet (14) and water outlet (15) of the spiral tube (13) are both arranged outside the spiral separator (8). It also includes a return pipe (16), and one end of the return pipe (16) is connected to the outlet port of the vacuum pump (5); it also discloses a purification method. The invention has the beneficial effects of simple process, no environmental pollution, high purity of 3-isocyanatopropyltriethoxysilane as high as 97-99%, high purification efficiency, and prevention of high-temperature materials from being polymerized and deteriorated.

Description

technical field [0001] The invention relates to the technical field of rectifying and purifying 3-isocyanatopropyl triethoxysilane under high vacuum and low temperature conditions, in particular to a device for rectifying and purifying 3-isocyanatopropyl triethoxysilane and its method. Background technique [0002] Principle of Rectify The basic principle of distillation is to partially vaporize the liquid mixture, and use the characteristics of different volatilities (relative volatility, α) of each component in it to realize the unit operation for the purpose of separation. Distillation can be divided into simple distillation, flash distillation, rectification and special distillation according to its operation method. [0003] 3-isocyanatopropyltriethoxysilane is one of the most important raw materials for polyurethane synthesis, and many varieties have been used in industry. The traditional phosgene production has the disadvantages of many process steps and complex equ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/20
Inventor 冉刚宁兆伦覃建华郭鹏
Owner ASTATECH CHENGDU BIOPHARM CORP