Method for setting polymerization condition and method for manufacturing optical material

Patent metadata

Field	Value
Publication number	US-12384870-B2
Application number	US-201817040136-A
Country	US
Kind code	B2
Filing date	Jun 6, 2018
Priority date	Mar 27, 2018
Publication date	Aug 12, 2025
Grant date	Aug 12, 2025

Abstract

A method for setting polymerization condition includes a physical property acquiring step of, when heating a composition including a polymerization-reactive compound and a polymerization catalyst and/or a polymerization initiator and retaining heat at a predetermined temperature, acquiring a physical property value a derived from a functional group before heating of the polymerization-reactive compound and a physical property value b derived from a remaining functional group after maintaining a temperature for a predetermined time; a remaining functional group ratio calculating step of calculating a remaining functional group ratio from the physical property value a and the physical property value b; a reaction rate coefficient calculating step of calculating a reaction rate coefficient from the remaining functional group ratio on the basis of a reaction rate equation; and a polymerization temperature calculating step of calculating a polymerization temperature on the basis of the reaction rate coefficient and conditions below.

First claim

The invention claimed is:

1. A method for manufacturing an optical material, comprising:
a physical property acquiring step comprising:
acquiring a physical property value A derived from a functional group before heating of a composition including a polymerization-reactive compound, a polymerization catalyst, and/or a polymerization initiator,
heating the composition and retaining heat at a plurality of predetermined temperatures, and
acquiring a physical property value B derived from a remaining functional group after maintaining each of the plurality of predetermined temperatures for predetermined times;

a remaining functional group ratio calculating step of calculating a remaining functional group ratio from the physical property value A and the physical property value B;
a reaction rate coefficient calculating step of calculating a reaction rate coefficient from the remaining functional group ratio on the basis of a reaction rate equation;
a polymerization temperature calculating step of back-calculating a plurality of polymerization temperatures at predetermined time intervals within a polymerization time based on the reaction rate equation using the reaction rate coefficient so as to satisfy the following conditions:
selecting and determining an average polymerization rate from a range of 0.4%/hr or more and 15%/hr or less in a range of 10% or more and 80% or less of a conversion ratio,
calculating multiple polymerization rates at predetermined time intervals within the time when the conversion ratio is in the range of 10% or more and 80% or less,
calculating a standard deviation by the positive square root of the variance of the multiple polymerization rates and the average polymerization rate, and
satisfying 2.3%/hr or less of the calculated standard deviation; and

a polymerization step of polymerizing a composition including the polyisocyanate compound, the active hydrogen compound, and the polymerization catalyst and/or the polymerization initiator to satisfy each polymerization temperature at predetermined time intervals obtained in the polymerization temperature calculating step.

2. The method for manufacturing an optical material according to claim 1 ,
wherein the polyisocyanate compound includes at least one kind selected from an aliphatic polyisocyanate, an aromatic polyisocyanate, a heterocyclic polyisocyanate, and an alicyclic polyisocyanate.

3. The method for manufacturing an optical material according to claim 1 ,
wherein the active hydrogen compound includes at least one kind selected from a group consisting of a polythiol compound having two or more mercapto groups, a hydroxythiol compound having one or more mercapto groups and one or more hydroxyl groups, a polyol compound having two or more hydroxyl groups, and an amine compound.

4. The method for manufacturing an optical material according to claim 1 ,
wherein the composition includes at least one kind of compound selected from an allyl carbonate compound, a (meth) acrylate compound, and an episulfide compound.

5. The method for manufacturing an optical material according to claim 4 ,
wherein the allyl carbonate compound is represented by General Formula (1),

wherein R 1 represents a chained or branched divalent to 20-valent group derived from an aliphatic polyol with 3 to 35 carbon atoms which may include a hetero atom, or a divalent to 20-valent group derived from a cycloaliphatic polyol with 5 to 40 carbon atoms which may include a hetero atom, m represents an integer of 2 to 10, and R 1 does not include an allyloxycarbonyl group.

6. The method for manufacturing an optical material according to claim 4 ,
wherein the (meth) acrylate compound is represented by General Formula (2),

and wherein R 2 represents a divalent to tetravalent organic group with 1 to 30 carbon atoms which may include a hetero atom or an aromatic group, R 3 represents a hydrogen atom or a methyl group, and n represents an integer of 2 to 4.

7. The method for manufacturing an optical material according to claim 4 ,
wherein the episulfide compound is represented by General Formula (3),

wherein General Formula (3), R 1 to R 7 may be the same or different and represent a hydrogen atom, a linear or branched alkyl group with 1 or more and 10 or less carbon atoms, or a substituted or unsubstituted aryl group with 6 or more and 18 or less carbon atoms, m represents an integer of 0 or more and 2 or less, and p represents an integer of 0 or more and 4 or less.

8. The method for manufacturing an optical material according to claim 1 ,
wherein the physical property values A and B are selected from the group consisting of a heat value, a specific gravity, a weight-average molecular weight, a number-average molecular weight, a spectral intensity in IR measurement, a 1 H-NMR spectral intensity, and a 13 C-NMR spectral intensity.

9. An apparatus for setting polymerization conditions comprising:
a storage unit;
a memory and instructions stored therein configured to:
acquire, from the storage unit, a physical property value A derived from a functional group before heating of a composition including a polymerization-reactive compound, a polymerization catalyst, and/or a polymerization initiator,
heat the composition and retaining heat at a plurality of predetermined temperatures, and
acquire, from the storage unit, a physical property value B derived from a remaining functional group after maintaining each of the plurality of predetermined temperatures for a predetermined times from a storage; and

a CPU and instructions stored therein configured to:
calculate a remaining functional group ratio from the physical property value A and the physical property value B,
calculate a reaction rate coefficient from the remaining functional group ratio on the basis of a reaction rate equation, and
back-calculate a plurality of polymerization temperatures at predetermined time intervals within a polymerization time based on the reaction rate equation using the reaction rate coefficient so as to satisfy the following conditions:
selecting and determining an average polymerization rate from a range of 0.4%/hr or more and 15%/hr or less in a range of 10% or more and 80% or less of a conversion ratio,
calculating multiple polymerization rates at predetermined time intervals within the time when the conversion ratio is in the range of 10% or more and 80% or less,
calculating a standard deviation by the positive square root of the variance of the multiple polymerization rates and the average polymerization rate, and
satisfying 2.3%/hr or less of the calculated standard deviation.

10. A non-transitory computer readable medium having stored thereon a computer program for setting polymerization conditions for a composition including a polymerization-reactive compound, a polymerization catalyst, and/or a polymerization initiator, the computer program causing a computer to implement functions of:
a storage unit;
a memory and instructions stored therein configured to:
acquire, from the storage unit, a physical property value A derived from a functional group before heating of the composition,
heat the composition and retaining heat at a plurality of predetermined temperatures, and
acquiring, from the storage unit, a physical property value B derived from a remaining functional group after maintaining a each of the plurali

Assignees

• Mitsui Chemicals Inc

Inventors

• Furuya Masayuki
• Nishimura Takeshi
• Ito Shinsuke
• Ogawa Tatsuya

Classifications

• G16C20/40

  Searching chemical structures or physicochemical data · CPC title

• G01N3/54

  Performing tests at high or low temperatures · CPC title

• C08G75/08

  from thiiranes · CPC title

• C08G18/72

  Polyisocyanates or polyisothiocyanates · CPC title

• C08F18/24

  Esters of carbonic or haloformic acids · CPC title