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CN-122003447-A - Method for producing polymer

CN122003447ACN 122003447 ACN122003447 ACN 122003447ACN-122003447-A

Abstract

The method for producing a polymer of the present invention comprises a polymerization step of polymerizing a polymerization initiator and a monomer in a liquid to obtain a polymerization product, and a further polymerization step of adding an additive component by performing at least one additional polymerization step. Wherein the additive component contains at least one component selected from the group consisting of monomers and polymerization initiators, and the addition of the additive component is performed while controlling the addition amount of the additive component.

Inventors

  • KITAMORI TAKEHIKO
  • SHIMIZU HISASHI
  • Adelina Tanaka
  • Iiyama Naoshi
  • Aratani Yoshinori
  • Sen Dushi

Assignees

  • 株式会社大赛璐

Dates

Publication Date
20260508
Application Date
20241009
Priority Date
20231010

Claims (15)

  1. 1. A method of making a polymer, the method comprising: A polymerization step of polymerizing a polymerization initiator and a monomer in a liquid to obtain a polymerization product, and An additional polymerization step of adding an additive component to perform a further polymerization reaction, the additional polymerization step being performed at least once, The additive component comprises at least one component selected from monomers and polymerization initiators, The addition of the additive component is performed while controlling the addition amount of the additive component.
  2. 2. The method for producing a polymer according to claim 1, wherein, The addition amount of the additive components is based on the mole.
  3. 3. The method for producing a polymer according to claim 1, wherein, When the additional polymerization step is performed n times (n≥1), the kth (1≥k≥n) additional polymerization step treats the liquid containing the polymerization reactant obtained in the polymerization step (in the case of k=1) or the liquid containing the polymerization reactant obtained in the kth-1 additional polymerization step (in the case of k≥2), The addition of the additive components in the kth additional polymerization step is performed while controlling M ki 、M ka 、M kf 、I ki 、I ka and I kf described below, M ki the total molar amount of the monomers contained in the liquid at the start time of the kth additional polymerization step; M ka the total molar amount of the monomers added in the kth additional polymerization step; m kf the total molar amount of the monomers contained in the liquid at the end of the kth additional polymerization step; I ki the total molar amount of the polymerization initiator contained in the liquid at the start time of the kth additional polymerization step; I ka the total molar amount of the polymerization initiator added in the kth additional polymerization step; I kf the total molar amount of the polymerization initiator contained in the liquid at the end of the kth additional polymerization step, Wherein M ka +I ka is not 0 mol, M ka is more than 0 mol, and I ka is more than 0 mol.
  4. 4. The method for producing a polymer according to claim 3, wherein, In the additional polymerization step, the addition of the additive component in the kth additional polymerization step is further performed while controlling the use of M represented by the following formula M by using the M ki 、M ka and the M kf , Formula M: m=m ki +M ka -M kf .
  5. 5. The method for producing a polymer according to claim 3 or 4, wherein, In the additional polymerization step, the addition of the additive component in the kth additional polymerization step is further performed while controlling the use of I ki 、I ka and I kf as represented by the following formula I, Formula I: i=i ki +I ka -I kf .
  6. 6. The method for producing a polymer according to claim 3 or 4, wherein, In the above additional polymerization step, the addition of the additive component in the kth additional polymerization step is further performed while controlling the ratio R represented by the following formula R using M represented by the following formula M and I represented by the following formula I, R is R=M/I M: m=m ki +M ka -M kf Formula I: i=i ki +I ka -I kf .
  7. 7. The method for producing a polymer according to claim 6, wherein, In the additional polymerization step, the control of the ratio R is performed so as to satisfy the following condition (1), The dispersion sigma 2 calculated according to the following expression sigma 2 is 300 or less, 。
  8. 8. The method for producing a polymer according to claim 1 or 2, wherein, As the monomer used in the polymerization step, at least two monomers are used.
  9. 9. The method for producing a polymer according to claim 1 or 2, wherein, As the monomer used in the above-mentioned polymerization step, at least one monomer selected from the group consisting of (meth) acryl-containing polymerizable monomer, isocyanate group-containing polymerizable monomer, carboxyl group-containing polymerizable monomer, hydroxyl group-containing polymerizable monomer, epoxy group-containing polymerizable monomer, and epoxy group-containing polymerizable monomer is used An oxazoline group-containing polymerizable monomer, a maleimide group-containing polymerizable monomer, an amino group-containing polymerizable monomer, a styrene-based monomer, a fluorine-containing vinyl monomer, a silicon-containing vinyl-based monomer, a vinyl ester-based monomer, a diene-based monomer, vinyl chloride, vinylidene chloride, allyl chloride, and vinyl ethyl ether.
  10. 10. The method for producing a polymer according to claim 1 or 2, wherein, In any additional polymerization step up to the nth time, when a monomer is added as the additive component, at least a part of the kind of the monomer and the kind of the monomer used in the polymerization step are repeated.
  11. 11. The method for producing a polymer according to claim 1 or 2, wherein, In the optional additional polymerization step up to the nth time, when a polymerization initiator is added as the additive component, the polymerization initiator and the polymerization initiator used in the polymerization step are radical polymerization initiators.
  12. 12. The method for producing a polymer according to claim 1 or 2, wherein, At least one step selected from the polymerization steps and the additional polymerization step performed at least once is performed using an instrument having a reaction channel for allowing the polymerization reaction of the monomer to proceed.
  13. 13. The method for producing a polymer according to claim 12, wherein, The device is a microfluidic reactor, and the reaction flow path is a microfluidic flow path.
  14. 14. A method of making a composition, the method comprising: a composition obtained using the polymer produced by the method for producing a polymer according to claim 1.
  15. 15. A method for producing a molded article, the method comprising: A step of molding a polymer produced by the method for producing a polymer according to claim 1 or a composition produced by the method for producing a composition according to claim 14.

Description

Method for producing polymer Technical Field The present disclosure relates to a method of manufacturing a polymer. Background In general, in the production of a polymer using a polymerization reaction, a monomer is polymerized in the presence of a polymerization initiator. Examples of the method for polymerizing the monomer include a batch polymerization method (batch polymerization method) in which a polymerization initiator and all monomers as raw materials are dissolved in a solvent, and the resulting solution is heated to polymerize at one time. However, in the batch polymerization method, it is difficult to control the reaction conditions in accordance with the progress of the reaction, and there are disadvantages that, for example, the reaction conditions vary with the action of the initiator on the monomer or the like due to a minute change in the reaction conditions, and the characteristics such as the molecular weight distribution of the resulting polymer are deviated. In addition, difficulty in controlling the reaction conditions is also related to quality differences between batches. One of the solutions to these problems is a method of mixing a monomer and a polymerization initiator or separately supplying them to a system maintained at respective temperatures to polymerize them, so-called a drop polymerization method (semi-batch polymerization method). As the dropping polymerization method, for example, a method of preheating and dropping a monomer and a method of dropping a monomer into a polymerization solvent maintained at a constant temperature are known (patent documents 1 and 2). The drop polymerization method is effective in obtaining a uniform polymer because the reaction system is smaller than the batch polymerization method, and therefore the component ratio in the reaction system can be easily controlled. However, in the dropping polymerization method, control of reaction conditions such as reaction temperature is difficult, and further improvement is expected from the viewpoint of controlling uniformity of the polymer. In view of this problem, patent document 3 discloses a technique of controlling uniformity (particularly molecular weight distribution) of a polymer obtained by using a microreactor having a1 st inlet for introducing a monomer component and another inlet located downstream from the 1 st inlet, and capable of introducing the monomer component into the 1 st inlet and the other inlets. Prior art literature Patent literature Patent document 1 Japanese patent application laid-open No. 2004-269855 Patent document 2 Japanese patent application laid-open No. 2004-355023 Patent document 3 Japanese patent application laid-open No. 2020-29518 Disclosure of Invention Problems to be solved by the invention Various methods have been studied for controlling the uniformity of polymers, particularly the molecular weight distribution. In recent years, a reactor has been developed which uses a reaction system in which monomers as raw materials are separately introduced into the reaction system to perform polymerization reaction, as disclosed in patent document 1. However, the limitation of the structure of the reactor is not preferable from the viewpoint of difficulty in flexibly coping with the change of the manufacturing environment, and a method of more easily controlling the molecular weight distribution of the polymer is desired. Accordingly, an object of the present disclosure is to provide a method for producing a polymer, which can easily control the molecular weight distribution of the polymer. Means for solving the problems As a result of intensive studies, the present inventors have found that, in a method of polymerizing a monomer in the presence of a polymerization initiator while adding at least one additive component selected from the group consisting of a monomer and a polymerization initiator, the above problems can be solved by allowing the addition of the additive component to proceed while controlling the addition amount of the additive component, and have completed the invention of the present disclosure. Namely, the gist of the present disclosure is as follows. < Mode 1> Mode 1 of the present disclosure relates to a method for producing a polymer, the method comprising: A polymerization step of polymerizing a polymerization initiator and a monomer in a liquid to obtain a polymerization product, and An additional polymerization step of adding an additive component to perform a further polymerization reaction, the additional polymerization step being performed at least once, The additive component comprises at least one component selected from monomers and polymerization initiators, The addition of the additive component is performed while controlling the addition amount of the additive component. < Mode 2> In the embodiment 1, the addition amount of the additive component may be a molar basis. < Mode 3> In embodiment 1 or 2, when the additional polymerization step