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Method for preparing silane coupling agent Si-69 in water phase

A technology of silane coupling agent and si-69, which is applied in the field of compound preparation, can solve problems such as difficult process control, hydrolysis of raw materials and products, and expensive raw materials, and achieve easy control of process conditions, short production cycle, and shortened reaction the effect of time

Pending Publication Date: 2018-07-06
QINGDAO UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] The purpose of the present invention is to solve the traditional method for preparing silane coupling agent Si-69, which has long reaction time, low purity, expensive raw materials and difficult storage, high production cost, severe hydrolysis of raw materials and products, high requirements for operation, and technical process. Problems that are not easy to control, provide a method for preparing silane coupling agent Si-69 in the water phase, the silane coupling agent Si-69 obtained by this method is used to improve the dispersibility of inorganic fillers in rubber and improve the dispersibility of inorganic fillers. Combination with rubber, so as to improve the comprehensive performance of rubber

Method used

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  • Method for preparing silane coupling agent Si-69 in water phase
  • Method for preparing silane coupling agent Si-69 in water phase
  • Method for preparing silane coupling agent Si-69 in water phase

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Embodiment 1

[0025] A method for preparing silane coupling agent Si-69 in aqueous phase, comprising the steps:

[0026]One, dissolving sodium phosphate and sodium borate in water to make a buffer solution with a concentration of 0.05mol / L; two, dissolving sodium sulfide pentahydrate in water to make a sodium sulfide solution with a mass fraction of 12%; three, mixing Sodium sulfide solution is mixed with buffer solution, and elemental sulfur is added to it. The molar ratio of elemental sulfur to sodium sulfide is 2.75:1. Stir at 40°C at a speed of 280r / min until dissolved. The reaction time is 15min. Obtain the inorganic phase solution that contains polysulfide of reddish-brown; Four, dodecyltrimethylammonium bromide and KI are dissolved in water, and the total amount that dodecyltrimethylammonium bromide and KI add is γ - 1% of the mass of chloropropyltriethoxysilane to make a catalyst solution with a mass fraction of 2%; 5. Add the catalyst solution dropwise to the inorganic phase soluti...

Embodiment 2

[0029] A method for preparing silane coupling agent Si-69 in aqueous phase, comprising the steps:

[0030] One, dissolving sodium phosphate and sodium carbonate in water to make a buffer solution with a concentration of 0.05mol / L; two, dissolving sodium sulfide nonahydrate in water to make a sodium sulfide solution with a mass fraction of 12%; three, mixing Sodium sulfide solution is mixed with buffer solution, and elemental sulfur is added to it. The molar ratio of elemental sulfur to sodium sulfide is 3:1. Stir at 40°C at a speed of 280r / min until dissolved. The reaction time is 15min. Obtain a reddish-brown inorganic phase solution containing polysulfides; four, benzyltriethylammonium chloride and KI are dissolved in water, and the total amount of benzyltriethylammonium bromide and KI added is γ-chloropropyl 1% of triethoxysilane quality, make the catalyst solution that mass fraction is 2%; More than 98% of γ-chloropropyl triethoxysilane, the molar ratio of γ-chloropropyl ...

Embodiment 3

[0033] A method for preparing silane coupling agent Si-69 in aqueous phase, comprising the steps:

[0034] One, dissolving sodium phosphate and sodium hydrogen phosphate in water to make a buffer solution with a concentration of 0.06mol / L; two, dissolving sodium sulfide nonahydrate in water to make a sodium sulfide solution with a mass fraction of 14%; three, Mix the sodium sulfide solution with the buffer solution, and add elemental sulfur to it, the molar ratio of elemental sulfur to sodium sulfide is 2.6:1, stir at 50°C at a speed of 300r / min until dissolved, and the reaction time is 10min, that is A reddish-brown inorganic phase solution containing polysulfides can be obtained; four, benzyltriethylammonium chloride and KI are dissolved in water, and the total amount of benzyltriethylammonium chloride and KI added is γ- 1% of the mass of chloropropyltriethoxysilane is used to make a catalyst solution with a mass fraction of 2%. γ-chloropropyltriethoxysilane with a purity o...

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Abstract

The invention relates to a method for preparing a silane coupling agent Si-69 in a water phase, and relates to a preparation method of a compound. The problems that a traditional method for preparingthe silane coupling agent Si-69 is long in reaction time, low in product purity, expensive in raw material price, not easy to store, high in production cost, severe in raw material and product hydrolysis phenomenon, high in operation requirement, and not easy to control a process flow are solved. The method comprises the following steps of (1) preparing a buffer solution; (2) preparing a sodium sulfide solution; (3) synthesizing a polysulfide inorganic phase solution; (4) preparing a catalyst solution; (5) synthesizing the silane coupling agent Si-69; (6) filtering, separating, decoloring, impurity-removing, drying, and purifying the silane coupling agent Si-69. The method provided by the invention has the advantages of short reaction period, high product purity, easiness in storing raw materials, low price of the raw materials, easiness in getting the raw materials, simple operation flow, easiness in controlling process conditions, high yield, easiness in controlling average Sulphur content, and low production cost. The product prepared through the method provided by the invention is high in purity (99 percent or more), not hydrolyzed or sulfur-separated, and long in preservationtime.

Description

technical field [0001] The invention relates to a method for preparing a compound, in particular to a method for preparing a silane coupling agent—Si-69 in an aqueous phase. Background technique [0002] Silane coupling agent is a general term for compounds containing organic functional groups and hydrolyzable silane active groups in the molecule. The purpose of using a bifunctional coupling agent is to enhance the compatibility of polar fillers and non-polar rubbers, and to improve the interaction between fillers and rubbers. Adding a coupling agent to the compound can improve the dispersibility of the filler, and improve the processing performance, physical and mechanical properties, and dynamic properties of the compound. Materials that use these properties include rubber resin, coatings, adhesives, glass, and metal surfaces. treatment agent, etc. [0003] Automobile is the product of human civilization. While it brings progress to mankind, it also brings many sequelae....

Claims

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Application Information

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IPC IPC(8): C07F7/18
CPCC07F7/1892
Inventor 李志波姚彬彬阚泽沈勇贾维杰王滨
Owner QINGDAO UNIV OF SCI & TECH
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