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Method for preparing stabilizing agent for silicon antifreeze

A technology of antifreeze and stabilizer, which is applied in the preparation of silicon-type antifreeze stabilizer and antifreeze stabilizer. Unable to obtain silicon-type antifreeze, phosphorus-silicon type stabilizer, etc., to achieve the effect of improving selectivity, increasing yield, and high yield

Active Publication Date: 2009-11-11
JIANGSU LOPALTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This type of stabilizer is mainly represented by phosphorus-silicon type coupling agent. For the known synthesis method of this type of substance, refer to the U.S. patent No. ORGANOPOLYSILOXANES CONTAINING PHOSPHONICGROUPS, METHOD FOR THE PRODUCTION AND USE THEREOF "U.S. patent, the above synthesis method usually uses organic amine as a catalyst, although it can prevent the gelation tendency of silicate, but the catalytic activity of organic amine is low, so it cannot be obtained High yield phosphorus silicon type stabilizer
Since the content of chloride ions in the antifreeze has a very high requirement (less than 80ppm), and the above synthesis method does not introduce how to deal with the by-product chloride, resulting in a large amount of chloride ions in the stabilizer during the later hydrolysis process Among them, it is impossible to obtain a phosphorus-silicon stabilizer suitable for the use of silicon-based antifreeze

Method used

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  • Method for preparing stabilizing agent for silicon antifreeze
  • Method for preparing stabilizing agent for silicon antifreeze
  • Method for preparing stabilizing agent for silicon antifreeze

Examples

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Effect test

Embodiment 1

[0025] In the present embodiment, the preparation method of silicon type antifreeze stabilizer comprises the following steps:

[0026] a. Add 800g of chloropropyltrimethylsilane, 500g of dimethyl phosphate, 6g of n-butylamine and 20g of benzyltriethylammonium chloride into a 2L, 312L stainless steel reaction kettle, press nitrogen to 0.15mpa, Check the airtightness of the equipment, heat and stir, raise the temperature to 120°C, and stir for 4 hours.

[0027] b. Sampling and analysis of the synthesized products. At this time, turn on the nitrogen switch and control the nitrogen flow rate at 0.6L / min. At this time, the temperature of the reactor is controlled at 150°C, and the time for nitrogen flow is 1 hour to remove some low-boiling chlorides and untreated raw materials for the reaction.

[0028] c. After completion of the chloride removal reaction, use a vacuum oil pump to flash-evaporate the synthesized product, and cut a fraction at 120±20° C. to obtain 800 g of the phos...

Embodiment 2

[0034] In the present embodiment, the preparation method of silicon type antifreeze stabilizer comprises the following steps:

[0035] a. Add 800g of chloropropyltrimethylsilane, 700g of diethyl phosphate, 6g of n-butylamine and 20g of benzyltriethylammonium chloride into a 2L, 312L stainless steel reaction kettle, press nitrogen to 0.15mpa, Check the airtightness of the equipment, heat and stir, raise the temperature to 180°C, and stir for 7 hours.

[0036] b. Sampling and analysis of the synthesized products. At this time, turn on the nitrogen switch and control the nitrogen flow rate at 1.0L / min. At this time, the temperature of the reactor is controlled at 170°C, and the time for nitrogen flow is 2 hours to remove some low-boiling chlorides and untreated raw materials for the reaction.

[0037] c. After completion of the chloride removal reaction, use a vacuum oil pump to flash-evaporate the synthesized product, and cut a fraction at 120±20° C. to obtain 920 g of phosphos...

Embodiment 3

[0043] In the present embodiment, the preparation method of silicon type antifreeze stabilizer comprises the following steps: a. Add 800g chloropropyltrimethylsilane, 1002g dimethyl phosphate, 6g n-butyl in 2L, 312L stainless steel reactor Amine and 20g of benzyltriethylammonium chloride, press nitrogen to 0.15mpa, check the airtightness of the equipment, heat and stir, raise the temperature to 150°C, stir for 6 hours,

[0044] b. Sampling and analysis of the synthesized products. At this time, turn on the nitrogen switch and control the nitrogen flow rate at 0.8L / min. At this time, the temperature of the reactor is controlled at 160°C, and the time for nitrogen flow is 1.5 hours to remove some low-boiling chlorides and untreated raw materials for the reaction.

[0045] c. After completion of the chloride removal reaction, use a vacuum oil pump to flash-evaporate the synthesized product, and cut a fraction at 120±20° C. to obtain 1020 g of the phosphosilane mixture. Yield is ...

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Abstract

The invention relates to a method for preparing a stabilizing agent for an antifreeze, in particular to a method for preparing a stabilizing agent for a silicon antifreeze, and belongs to the technical field of organic synthesis. The preparation method comprises the following steps: adopting a phase transfer catalyst as a catalyst accelerator to accelerate the reaction of halogenated silane and organic phosphonate, and removing chloride contents in a residual product through nitrogen and flash evaporation. The method has the advantages that the method can effectively improve the selectivity and yield of the reaction under the proper temperature, mainly can effectively reduce the content of chlorine hydride in the product to obtain the stabilizing agent applicable to the silicon antifreeze, and has high yield; and the purity of the obtained stabilizing agent for the silicon antifreeze is not less than 76 percent per mole.

Description

technical field [0001] The invention relates to a method for preparing a stabilizer for antifreeze, in particular to a method for preparing a silicon-type antifreeze stabilizer, and belongs to the technical field of organic synthesis. Background technique [0002] Antifreeze is a coolant containing special additives, mainly used in liquid-cooled engine cooling systems. Antifreeze has excellent properties such as antifreezing in winter, anti-boiling in summer, anti-scale and anti-corrosion throughout the year. In antifreeze technology, because its silicate component has excellent aluminum alloy protection ability, so the inorganic salt type antifreeze usually contains silicate component, but the alkaline aqueous solution of silicate at pH 7-9 It has a strong polymerization ability, and it is easy to produce silicate gel, which destroys the stability of antifreeze and has a great impact on the use of antifreeze. For this reason, a large number of scientific researchers have c...

Claims

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Application Information

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IPC IPC(8): C07F9/40C09K5/20B01J31/02
Inventor 石俊峰严军表江善钟陈甜
Owner JIANGSU LOPALTECH
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