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A kind of preparation method of polycarbonate-polyether diol

A polyether diol and polycarbonate technology, which is applied in the field of polycarbonate-polyether diol synthesis, can solve the problems of prolonged reaction time, increased ratio of cyclic carbonate, and increased production cost of polymers, etc. Improve mass and heat transfer capacity and effect, improve activity and selectivity, optimize molecular weight distribution effect

Active Publication Date: 2021-11-09
合肥普力先进材料科技有限公司
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AI Technical Summary

Problems solved by technology

Otherwise, the catalyst has no application value due to the increase in production cost due to the excessive addition of the catalyst
An important means of controlling the molecular weight of polycarbonate-polyether diols with a smaller molecular weight is to add a higher proportion of initiators, generally 1 / 50 to 1 / 90 of the molar number of epoxy monomers. Under such conditions , most of the catalysts will lose activity; or although a very small number of catalysts still maintain weak activity, the reaction time is greatly prolonged (more than 12 hours) to obtain the polymer, which is due to the fact that the reaction time is actually due to a higher proportion of the initiator Leads to deactivation of the catalyst, prolonging the activation process of the catalyst on the reactants (by several hours)
It takes longer reaction time and more energy consumption, which increases the production cost
In addition, under the condition of the above-mentioned higher ratio of initiator addition, the structure ratio of polycarbonate in the polycarbonate-polyether diol structure obtained by synthesis will decrease (<50%), that is, the reaction to carbon dioxide fixed rate reduction
Because the addition of a higher proportion of initiator will cause a large number of catalyst active sites to be quenched or occupied, the macroscopic manifestation is that the catalyst activity is reduced or even deactivated
The reduction of the carbon dioxide fixation rate indicates that the proportion of the low-cost carbon dioxide raw material in the polymer is reduced, which means that the proportion of the higher-cost epoxide is increased, which leads to an increase in the production cost of the polymer on the one hand, and on the other hand, is beneficial to energy saving and emission reduction. (Consumption of CO2) is also less effective
If the temperature is too high, the content of carbonate chains will be low, the molecular weight distribution coefficient PDI will become wider, and the proportion of by-product cyclocarbonate will increase, which will reduce the quality of the product
Although a small number of continuous flow processes have been developed, there are problems: there is inevitably an amplification effect, which brings many uncertainties to further industrial applications; some continuous flow processes are not fully reacted in a short period of time, and need to increase The reaction time is used to increase the conversion rate, resulting in a decrease in production efficiency
However, due to the generation of product polycarbonate-polyether glycol, the reaction system becomes viscous, which makes it difficult to separate the catalyst from the polymerization system, which has caused prior art to produce polycarbonate-polyether glycol magnification effect
[0017] Compared with general polymers, the particularity of polycarbonate-polyether diols also lies in that the inventors have found that polycarbonate-polyether diols can increase the content of polycarbonate units, optimize polycarbonate When the molecular weight distribution of ester-polyether diol and the amplification effect of producing polycarbonate-polyether diol are solved, there is mutual entanglement, there is the situation of mutual restriction, and the catalyst activity of prior art is low, especially adding higher The proportion of the initiator is generally 1 / 50 to 1 / 90 of the molar number of epoxy monomers, and the product polycarbonate-polyether diol is formed, and the reaction system becomes viscous, which makes the catalyst separated from the polymerization reaction system. It becomes difficult to reduce the mass transfer and thermal conductivity of the reaction equipment, so that increasing the content of polycarbonate units is often accompanied by a wide molecular weight distribution, and it is reflected in the presence of amplification effects during production
[0018] In summary, those skilled in the art urgently need a kind of content that can improve polycarbonate unit and optimize the molecular weight distribution of polycarbonate-polyether diol, solve the amplification effect of producing polycarbonate-polyether diol , but there is no such technical solution

Method used

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  • A kind of preparation method of polycarbonate-polyether diol
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  • A kind of preparation method of polycarbonate-polyether diol

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Embodiment 1-11

[0043] A kind of preparation method of polycarbonate-polyether glycol, the structural formula of described polycarbonate-polyether glycol

[0044] as follows:

[0045]

[0046] The number average molecular weight of the polycarbonate-polyether diol is 500-5000, the molecular weight distribution coefficient PDI is 1.0-1.2, the hydroxyl value is 22.4-224.4 mgKOH / g, R' is selected from hydrogen atom, methyl group, ethyl alcohol group, chloromethyl group, R" is selected from hydrogen atom, methyl group, ethyl group, chloromethyl group, m1, m2, n1, n2 are positive numbers, 1≤(m1+m2):(n1+n2), 0≤ n3≤8 integers;

[0047] Include the following steps:

[0048] (1) Introduce epoxy, catalyst, initiator and carbon dioxide into the premixing tank for premixing. The premixing pressure is 0.1-2MPa, the premixing temperature is 0-50°C, and the premixing time is 0-3 hours. Then import in the pipelined continuous reactor, described pipelined continuous reactor comprises heating section gro...

Embodiment 12

[0087] Embodiment 12 with reference to embodiment 6, embodiment 12 adopts the raw material of embodiment 6 and catalyst and reaction technology, difference is, the initiator of embodiment 12: epoxy monomer mole is 1 / 50, and temperature of reaction is 80 ℃, and There are two sets of piped reactors than in Example 12, one set is a laboratory device, and the inner diameter of the pipeline is 10mm, and the other is a pilot plant, and the inner diameter of the pipeline is 100mm. The purpose is to view the present invention by enlarging the size of the pipeline Whether the method has amplifying effect.

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Abstract

The invention discloses a preparation method of polycarbonate-polyether diol, the number-average molecular weight of polycarbonate-polyether diol is 500-5000, comprising the following steps: (1) comprising epoxide, catalyst , initiator and carbon dioxide are imported into the premixing tank for premixing, and then introduced into the pipelined continuous reactor, and in the presence of the catalyst, the initiator, epoxy compound and carbon dioxide are contacted in the pipelined continuous reactor to carry out polymerization reaction; ( 2) The polymerization reaction product flow of step (1) is partly or completely flowed through the cooling section group, and part of the polycarbonate-polyether glycol is separated, and the remaining polymerization reaction product flow continues to be polymerized in a pipelined continuous reactor reaction, or cycle back to step (1); wherein, the catalyst is modified by mixed acid during synthesis, and obtained by reacting water-soluble metal salts of zinc and cobalt in a water-soluble solvent.

Description

technical field [0001] The invention relates to the field of polycarbonate-polyether diol synthesis, in particular to a preparation method of polycarbonate-polyether diol. Background technique [0002] The polycarbonate-polyether diol structure contains both polycarbonate chains and polyether chains generated by the homopolymerization of epoxy compounds, making it both high Young's modulus and flexible, making it suitable for preparing Raw material of polyurethane material. CO consumption due to the polymerization reaction to produce polycarbonate-polyether diols 2 , the transformation of greenhouse gas carbon dioxide as a raw material into polymer materials is very beneficial to environmental protection and energy reduction and emission reduction; the polymerization reaction is often accompanied by by-products of cyclocarbonate, which is a commonly used industrial product. It can be separated and purified for later sale. [0003] At present, the production of polycarbona...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G64/18C08G64/20C08G64/34
CPCC08G64/183C08G64/205C08G64/34
Inventor 罗铭毛红兵王自修
Owner 合肥普力先进材料科技有限公司
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