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Overview and Production Process of Silane Coupling Agent

Mar 19, 2021

my country's glass fiber industry is a sunrise industry, and with the development of application fields such as construction, machinery, electronics and other glass fiber reinforced composite materials, my country's glass fiber industry is entering a new round of rapid development. It is estimated that during the "Eleventh Five-Year Plan" period, the growth rate of glass fiber production will be close to 10%. In 2010, my country's glass fiber production is expected to reach 1.3 million tons, and the demand for silane coupling agents will reach about 18,000 tons; plus the rubber industry In addition to the development of other industries, it is estimated that the total domestic demand for silane coupling agents in 2010 will reach more than 25,000 tons.

Although there are many silane coupling agent manufacturers in China, most of them have small production scales, lower product grades, and fewer varieties and specifications. Therefore, it is necessary for regions or enterprises with conditions to build larger multifunctional silane coupling agent production lines to improve the production level of silane coupling agents in my country.

Two overview
1 Basic situation:
Silane coupling agent is a kind of low molecular organic silicon compound with special structure. Its general formula is RSiX3, where R represents amino, mercapto vinyl, epoxy, chloropropyl, cyano and methacryloxy. Such groups, these groups and different matrix resins have strong reactivity, x represents a hydrolyzable group, such as halogen, alkoxy, acyloxy and so on.
The silane coupling agent is obtained by the addition of trichlorosilane (HSiCl3) and unsaturated olefins with reactive groups under the catalysis of platinic acid, followed by alcoholysis. Silane coupling agent can not only interact with the hydroxyl in the inorganic substance but also with the long molecular chain in the organic polymer, so that two materials with different properties can be coupled together, thereby improving the various properties of biological materials.
2 Purpose:
The application of silane coupling agent can be roughly summarized into three aspects;
(1) Used for surface treatment of glass fiber. Silane coupling agent can improve the bonding performance of glass fiber and resin, and improve the strength, water resistance and weather resistance of glass fiber reinforced composite materials. In 2004, the silane coupling agent used in glass fiber accounted for more than 50% of its total consumption. Among them, the more used varieties are vinyl silane, amino silane, methacryloxy silane and so on.
(2) Used for surface treatment of inorganic fillers. The silane coupling agent can pre-treat the surface of the filler when coupling the inorganic filler and resin, or directly add it to the resin. In order to improve the dispersibility and adhesion of the filler in the resin, improve the process performance and fill the plastic ( Including rubber) mechanical, electrical and weather resistance properties.
(3) Used as a sealant, adhesive and paint thickener. Silane coupling agents can improve their bonding strength, water resistance, weather resistance and other properties. Silane coupling agents can often solve the problem that certain materials cannot be bonded for a long time.
3 Varieties of silane coupling agent:

There are many varieties of silane coupling agents (see the table below for commonly used silane coupling agents), among which the largest output is bis-[3-(triethoxy)silylpropyl]tetrasulfide (Si-69 or KH-846) , It uses trichlorosilane and chloropropylene as raw materials to catalyze the synthesis of γ-chloropropyltrichlorosilane (it is an intermediate product for the production of a variety of silane coupling agents), and then undergo alcoholysis to obtain γ-chloropropyltriethyl Oxysilane is prepared by reacting with sulfide under certain conditions. It is a multifunctional silane coupling agent successfully used in the rubber industry and is widely used in radial tires and other rubber products.

Two production process
1 Production process
The production of silane coupling agent Si-69 requires intermediate γ-chloropropyltrichlorosilane. Since the intermediate is generally used by the manufacturer, its synthetic route is also given.
(1) Intermediate: Synthesis of γ-chloropropyltrichlorosilane
At present, the production of γ-chloropropyltrichlorosilane is a synthesis method of trichlorosilane and chloropropene under the catalysis of platinum compounds.
Brief description of the process flow: a certain amount of purified trichlorosilane (98%) and chloropropene (99%) are injected into the mixing kettle and mixed thoroughly, and then mixed with a batch of platinum compound in isopropanol solution under the protection of nitrogen. Into the addition kettle with a vacuum of 0.03-0.04Mpa and flushed with nitrogen, heat it in an oil bath, control the temperature at 50-60℃, and fully react for 5-6 hours. During the reaction, the catalyst is added in batches. After the addition, the reaction solution was gradually heated to 80°C and refluxed. When the reflux solution was gradually reduced until no reflux solution was seen, the reaction was terminated, and the reaction solution was pumped into the fractionation kettle for fractionation. The pressure in the kettle was 0.04Mpa and the temperature Control the temperature at 160°C, separate the low-boiling substances, and then further rectify the crude product to obtain the γ-chloropropyltrichlorosilane product.

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