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Polytetrahydrofuran diol and its preparation and purification method

A technology of polytetrahydrofuran diol and tetrahydrofuran, which is applied in the field of polytetrahydrofuran diol and its preparation and purification, and can solve problems such as molecular weight deviation, molecular weight change, and misoperation

Active Publication Date: 2006-12-27
山东亚科环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, since the molecular weight of PTMG in the polymerization solution can only be determined after purification, the purification process will also cause molecular weight changes
If it is found that the molecular weight of the final PTMG changes, it is very difficult to determine the most direct cause. If only the water is adjusted, it may lead to misoperation and artificially increase the fluctuation of the molecular weight.
The third is that the molecular weight is actually determined by the polymerization of the lower layer solution (mainly the catalyst). Due to the presence of the catalyst, the water content of the lower layer solution is often more than 5 times higher than that of the upper layer. , when the water fluctuation is transmitted to the upper solution, the molecular weight has already deviated greatly, and it takes a long time to adjust back, and improper adjustment can easily cause molecular weight oscillation

Method used

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  • Polytetrahydrofuran diol and its preparation and purification method
  • Polytetrahydrofuran diol and its preparation and purification method
  • Polytetrahydrofuran diol and its preparation and purification method

Examples

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preparation example Construction

[0070] In the preparation method of the present invention, the tetrahydrofuran and the proton donor (preferably water) are completely mixed according to the proportion, continuously added to the polymerization reactor with a stirring device, and prepared under the action of the heteropolyacid catalyst. In the polytetrahydrofuran diol oligomer, the water is measured by weighing, and the accuracy requirement is greater than 0.1%.

[0071] The polymerization reactor is in a heterogeneous state, the upper layer is a solution containing polytetrahydrofuran diol and tetrahydrofuran, and the lower layer is a solution containing catalyst and tetrahydrofuran. Under the action of the stirring device, the upper and lower layers are fully mixed. The requirement for stirring the reactor is that the ratio of the displacement per minute to the effective volume of the polymerization reactor is in the range of 5-20, in other words, the number of cycles of the polymerization reactor is 5-20 tim...

Embodiment 1

[0110] Embodiment 1 (preparation of polytetrahydrofuran diol)

[0111] In this example, refined tetrahydrofuran was used, deionized water was used as the proton donor, and 12-tungstophosphoric acid (dried to 8 crystalline water) was used as the catalyst.

[0112] The refined tetrahydrofuran and deionized water are formulated into a homogeneous mixed solution at a molar ratio of 62.5:1, which is accurately measured to 0.1% by a balance. The solution is called tetrahydrofuran aqueous solution.

[0113] In addition, the refined tetrahydrofuran and the catalyst were formulated into a uniform mixed solution at a molar ratio of 42:1, which was called a catalyst solution.

[0114] The catalyst solution is added to the polymerization reactor, and then the tetrahydrofuran aqueous solution is continuously added into the reactor, and the mass ratio of the catalyst solution to the tetrahydrofuran aqueous solution in the reactor is 3:1. The polymerization reactor is equipped with a stirri...

Embodiment 2

[0122] Embodiment 2 (preparation of polytetrahydrofuran diol)

[0123] The preparation of polytetrahydrofuran diol was carried out in the same manner as in Example 1, except that the conversion rate of tetrahydrofuran was controlled at 29±0.5%.

[0124] The polymer product of gained adopts the method identical with embodiment 1 to carry out characterization, confirms that its structure is:

[0125] HO(CH 2 ) 4 O n h

[0126] The number-average molecular weight-time relation of gained polytetrahydrofuran diol is monitored in the same manner as in Example 1, and it is found that the number-average molecular weight of the polytetrahydrofuran diol product is stably controlled within the scope of 2000 ± 50 Daltons .

[0127] The viscosity of the obtained polytetrahydrofuran diol is measured in the same manner as in Example 1, and the viscosity of the polytetrahydrofuran diol prepared in this embodiment is 560-600 centipoise.

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Abstract

The invention discloses a ploytetrahydrofuran glycol, the construction formula is presented in I, the number average molecular weight is between 650-3500 and molecular weight distribution Mv / Mn is between 1.2-1.7. The invention also discloses the method for preparing said polymer, comprising following steps: tetrahydrofuran and proton donor reacting to generate ploytetrahydrofuran glycol under action of heteropoly acid catalyst in the polymerization reactor equipped with stirring device, monitoring the tetrahydrofuran polymerization rate, controlling the polymerization rate by adjusting proton donor adding amount and getting final product with needed number average molecular weight and molecular weight distribution. The invention also discloses the method for purifying ploytetrahydrofuran glycol. The number average molecular weight is accurately controlled on line in this invention, and the product is characterized by regular construction, narrow molecular weight distribution, low viscosity and good processing property. HO*(CH2)O4*nH (I)

Description

technical field [0001] The present invention relates to polytetrahydrofuran diol and its preparation and purification method. Background technique [0002] Polytetramethylene ether glycol (polytetramethylene ether glycol, abbreviated as PTMG, related literature is also known as polytetrahydrofuran, polytetramethylene ether glycol, polyoxytetramethylene glycol, polytetramethylene ether glycol, polyoxytetramethylene Diol, etc.) are the main raw materials of high-performance block polyether polyurethane, polyether amide, polyether ester elastomer, thermoplastic polyurethane and casting elastomer. It can be used to make artificial leather, elastic coatings and adhesives, etc. Recently, PTMG raw materials have also been used in the manufacture of polyester and polyamide series elastomers. [0003] PTMG acts as a soft segment component in polymer materials. Polymers made from PTMG have excellent elasticity, wear resistance, tensile properties, water resistance and low temperatu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/20
Inventor 张永梅
Owner 山东亚科环保科技有限公司
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