Unlock instant, AI-driven research and patent intelligence for your innovation.

Thioester-bond-containing titanium ester coupling agent and preparing method thereof

A technology of titanate coupling agent and ester bond, which is applied in the field of titanate coupling agent and its preparation, can solve the problem of rubber scorching, Mooney viscosity increase, which is not conducive to the dispersion of white carbon black particles, rubber Problems such as high porosity, to achieve the effect of not easy rubber scorching, obvious coupling effect and simple production process

Inactive Publication Date: 2007-08-08
ZHEJIANG UNIV
View PDF0 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, polysulfide silane coupling agent needs a long time and high temperature to fully react with silica
When the mixing temperature is higher than 160°C, the polysulfide bond of the polysulfide silane coupling agent breaks, causing scorching of the rubber compound and increasing the Mooney viscosity, which is not conducive to the dispersion of silica particles in the rubber
The use of polysulfide silane coupling agent to modify silica also has disadvantages such as long mixing time, many mixing stages (3-6 stages), high porosity of the rubber material, and defective products due to scorch.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Thioester-bond-containing titanium ester coupling agent and preparing method thereof
  • Thioester-bond-containing titanium ester coupling agent and preparing method thereof
  • Thioester-bond-containing titanium ester coupling agent and preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0021] The preparation of the titanate coupling agent containing thioester bonds is carried out in two steps. The first step is to react the equimolar acid chloride compound and mercapto carboxylic acid in an organic solvent under the condition of nitrogen protection at low temperature under the action of an organic catalyst. A carboxylic acid compound containing a thioester bond is obtained. It is one of the keys of the present invention to slowly add mercaptocarboxylic acid dropwise to the acid chloride compound solution under low temperature and strong stirring conditions to control the reaction speed and avoid local overheating. The acid chloride compound is easy to be hydrolyzed, and the air and moisture in the medium need to be exhausted by nitrogen gas before the reaction. Acyl chloride compounds react violently with mercaptocarboxylic acids, releasing large amounts of hydrogen chloride. Simultaneously, hydrogen chloride reacts violently with the organic catalyst to re...

Embodiment 1

[0031] Using acetyl chloride, mercaptoacetic acid, and tetraethyl titanate as raw materials to prepare a titanate coupling agent containing a thioester bond:

[0032] 1) Weigh 0.2mol (15.7g) of acetyl chloride and 298g of chloroform, place them in a three-necked round-bottomed flask to make a 5% solution, add 0.18mol (15.3g) of pyridine and 1 magneton, cool to 0°C, at 0.1m 3Nitrogen gas is introduced from one side of the three-necked flask at a speed of / h, and the other side of the three-necked flask is connected to the waste gas receiver with built-in sodium hydroxide. liquid funnel, while magnetically stirring, add mercaptoacetic acid dropwise to a three-neck flask at a speed of 0.5ml / min. After the dropwise addition, continue to stir for 1h under nitrogen protection, filter, and carry out vacuum distillation on the filtrate to remove low-boiling fractions to obtain Carboxylic acid compounds with thioester bonds;

[0033] 2) Weigh 0.15mol (20g) of the carboxylic acid comp...

Embodiment 2

[0035] Using propionyl chloride, 2-mercaptopropionic acid, and tetrapropyl titanate as raw materials to prepare a titanate coupling agent containing a thioester bond:

[0036] Weigh 2mol (185g) of propionyl chloride and 740g of carbon tetrachloride, place them in a stainless steel container equipped with a stirring device, and make a 20% solution, add 2.4mol (213g) of triethylamine, cool to -20°C, and stir Mix the solution evenly, with 0.6m 3 Feed nitrogen gas at a speed of 1ml / min, use a dropping funnel to drop 2mol (212g) 2-mercaptopropionic acid at a speed of 1ml / min, continue to stir for 3h under nitrogen protection after the dropwise addition, filter, and carry out vacuum distillation to remove the low Boiling point fractions to obtain carboxylic acid compounds containing sulfur ester bonds;

[0037] 2) Take by weighing 1mol (168g) step 1) the carboxylic acid compound containing sulfur ester bond gained, be placed in the there-necked flask that agitator, condensation tub...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a polysilazane with butadiene and preparing method, which comprises the following steps: adding acyl chlorine compound into organic solvent; allocating solution with density at 5-20%; adding organic catalyst with molar number as 0.9-1.2 times as acyl chlorine; cooling; stirring; aerating nitrogen; dripping mercapto carboxyl acid with the same molar number as acyl chlorine; dripping; filtering to remove solid salt; decompressing; distilling to remove low-boiling point fraction; dripping titanium tetra-alkoxy; reacting for 0.5-2h; decompressing; distilling to remove low-boiling point fraction; obtaining the titanic acid ester coupler with thioester bond.

Description

technical field [0001] The invention relates to a titanate coupling agent containing sulfur ester bonds and a preparation method thereof. Background technique [0002] Compared with carbon black, silica has obvious advantages in terms of tread rubber wear resistance, wet road traction and rolling resistance, and is used as the main reinforcement of the new generation of low rolling resistance and low fuel consumption "green tires" agent. [0003] The surface of silica particles contains a large number of silanol groups, which are easy to agglomerate during the rubber mixing process, so the reinforcement effect of silica without surface treatment is poor. In tire tread rubber, silica, especially highly dispersed precipitated silica, and sulfur-containing bifunctional silane coupling agents such as γ-mercaptopropyltrimethoxysilane, γ-thiocyanopropyltriethyl Combined use of oxysilane, bis(3-triethoxysilylpropyl) disulfide (TESPD) or bis(3-triethoxysilylpropyl) tetrasulfide (T...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C08K5/56C07F7/28C08L21/00
Inventor 宋义虎郑强
Owner ZHEJIANG UNIV