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Preparation method of titanium complex with high catalytic activity

A high catalytic activity, titanium complex technology, applied in the preparation of organic compounds, the preparation of hydroxyl compounds, titanium organic compounds, etc., can solve the problems of product thermal stability and product appearance defects, high catalyst production cost, and achieve difficult crystallization. , the effect of low cost and long service life of catalyst

Active Publication Date: 2012-06-27
湖北新蓝天新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] Although existing titanium chelate catalysts have high catalytic activity, there are defects in product thermal stability and product appearance, and the production cost of the catalyst itself is relatively high

Method used

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  • Preparation method of titanium complex with high catalytic activity
  • Preparation method of titanium complex with high catalytic activity

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preparation example Construction

[0029] The preparation method of the highly catalytically active titanium complex provided by the embodiments of the present invention comprises the following steps:

[0030] A. Add tetraisopropyl titanate to the reaction kettle, add triethyl citrate dropwise under stirring, finish dropping in half an hour, and continue stirring for half an hour;

[0031] B. Add ethyl acetoacetate dropwise, drop it in 2 to 2.5 hours, keep the reaction temperature at 60°C to 70°C, and continue stirring for 1 hour;

[0032] C, steam the isopropanol that generates with negative pressure, then add 1,2-propylene glycol wherein, the mol ratio of tetraisopropyl titanate, triethyl citrate, ethyl acetoacetate and 1,2-propylene glycol is 1:0.1-0.5:1.5-1.9:0.5-1, preferably the molar ratio is 1:0.1-0.3:1.7-1.8:0.5-0.8. Stir the reaction for 1 hour, steam the remaining isopropanol with negative pressure, and obtain the titanium complex semi-finished product;

[0033] D. Add dibutyltin dilaurate to the t...

Embodiment 1

[0036] In a 500ml four-necked glass round bottom flask equipped with a stirrer, thermometer, condenser, heater and balance feeder, tetraisopropyl titanate, triethyl citrate, ethyl acetoacetate and 1,2- The molar ratio of propylene glycol is 1:0.1:1.5:1, add 200g of tetraisopropyl titanate, and start to add 20g of triethyl citrate dropwise under stirring condition. Stir for half an hour to complete the reaction. Then slowly add 138g of ethyl acetoacetate dropwise, keep the temperature at about 70°C, finish dropping in 2.5 hours, continue to stir for 1 hour; pump low boilers with negative pressure, distill the by-product isopropanol under reduced pressure, keep warm and pump until the flow is cut off Add 53g of 1,2-propanediol, and stir for 1 hour to react; extract low boilers with negative pressure, and steam the isopropanol remaining in the system under reduced pressure until the insulation is pumped to cut off the flow; then add 2.1g of dilauric acid Dibutyltin, and a compou...

Embodiment 2

[0038] In a 500ml four-necked glass round bottom flask equipped with a stirrer, thermometer, condenser, heater and balance feeder, tetraisopropyl titanate, triethyl citrate, ethyl acetoacetate and 1,2- The molar ratio of propylene glycol is 1:0.2:1.7:0.8, add 142g of tetraisopropyl titanate, and start to add 28g of triethyl citrate dropwise under stirring condition. Stir for half an hour to complete the reaction. Then slowly add 110g of ethyl acetoacetate dropwise, keep the temperature at about 65°C, drop it in 2 hours, continue to stir for 1 hour; pump low boilers with negative pressure, distill the by-product isopropanol under reduced pressure, keep warm and pump until the flow is cut off Add 30g of 1,2-propanediol, stir and react for 1 hour; extract low boilers with negative pressure, steam the isopropanol remaining in the system under reduced pressure, keep warm and pump until the flow is cut off; add 1.5g of dilauric acid to it Dibutyltin, and compound solvent: 40g methy...

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Abstract

The invention discloses a preparation method of a titanium complex with high catalytic activity. The preparation method comprises the steps of: adding tetraisopropyl titanate in an agitated reactor, finishing dropwise adding triethyl citrate under the condition of stirring within half of an hour, continuously stirring for half of an hour; finishing dropwise adding ethyl acetoacetate within 2-2.5hours, continuously stirring for reacting for 1hour; evaporating generated isopropanol under negative pressure, adding 1,2-propylene glycol in the evaporated generated isopropanol, stirring for reacting for 1 hour, and evaporating isopropanol remained in a system under the negative pressure to obtain a semi-finished product of the titanium complex; and adding organic tin in the semi-finished product of the titanium complex and compounding a solvent to obtain a finished product. The preparation method provided by the invention has the advantages of simplicity in operation, low cost, light product color, higher purity of the isopropanol as a side product, stable quality of the finished product, high catalytic activity, difficulty in crystallization, and longer service life of the catalyst.

Description

technical field [0001] The invention relates to the field of preparation of a dealcoholized room temperature vulcanized silicone rubber (RTV) catalyst, in particular to a preparation method of a titanium complex with high catalytic activity. Background technique [0002] Since its development in the 1950s, titanate has become one of the most widely used and best-performing organometallic catalysts. It is widely used as a coupling agent or catalyst for coatings, inks and polymers. Adding titanate to room temperature vulcanized silicone rubber can play the role of anti-corrosion and catalytic crosslinking. Short-chain titanate has disadvantages such as high activity, easy hydrolysis and difficult storage, so most of the market uses titanium chelate , This kind of chelate has good stability, no thickening, and the produced silica gel product has a long storage period, which can reach one year. Even if it is stored for a long time, it is not easy to crystallize and does not pro...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07F7/28C07C31/10C07C29/80C08J3/24C08L83/06
Inventor 王欣肖俊平高建秋彭汉华王成王度何仕凤
Owner 湖北新蓝天新材料股份有限公司
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