CN102794847B - The manufacture method of thermoset composition - Google Patents
The manufacture method of thermoset composition Download PDFInfo
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- CN102794847B CN102794847B CN201110137520.3A CN201110137520A CN102794847B CN 102794847 B CN102794847 B CN 102794847B CN 201110137520 A CN201110137520 A CN 201110137520A CN 102794847 B CN102794847 B CN 102794847B
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Abstract
The present invention provides the manufacture method for suppressing to solidify and produce the thermoset composition of the possibility of defect with composition.This method has the curing process for filling to the filling work procedure of mould and making after filling work procedure by hot briquetting mould composition to solidify the composition shunk with the solidification based on heat, and the curing process has following process：Heating process, makes composition be heated up from the temperature after filling work procedure by composition being heated up or being carried out the combination of liter mild temperature maintenance；Suppress process with departing from, stop heating composition after heating process, composition is set back and forth to change between the high and low temperature untill temperature of the temperature after heating process until the humidity province after reaching heating process again, so that the composition suppressed caused by being shunk caused by solidifying with composition departs from mould.
Description
Technical field
The present invention relates to the manufacture method of thermoset composition, more particularly to the group that will be shunk with the solidification based on heat
Compound is filled to mould and heats the manufacture method of the thermoset composition solidify said composition.In addition, this explanation
" composition " in book includes having or once has the composition of this characteristic of thermosetting.That is, the group before heat cure is represented sometimes
Compound, also represents the composition after heat cure sometimes.
Background technology
In recent years, in optical material, instead of glass lens, the popularization of plastic lens is promoted rapidly.Plastic lens has
The advantages of light weight, impact resistance, workability and easy dyeing.Therefore, plastic lens is in optical material, especially in eyeglass
Popularize rapidly in field.
During this popularization, this of the thickness of eyeglass is reduced in order to improve the aesthetic property of eyeglass
One requires to continue into the present from the glass lens epoch.Typically, the thickness for wanting to reduce eyeglass then needs to use high index of refraction
Material.
There is plastic lens to be better than the aspect of glass lens herein.For example if glass lens, then with refractive index into just
It can be dramatically increased than ground proportion, and the weight of eyeglass can be dramatically increased.If so, the comfortable wearing of eyeglass
Degree also can significantly be deteriorated.
On the other hand, if plastic lens, even if then refractive index is uprised, proportion is not also significantly increased, and eyeglass
Weight will not also be significantly increased.The wear comfort that therefore, it can suppress eyeglass is deteriorated.
It is used as the high plastics of refractive index, it is known to diallylcarbonate, epoxy methacrylates, phthalic acid two
Allyl ester (DAP：Di Allyl Phthalate, hereinafter also referred to " DAP ".) etc..On the other hand, plastic lens also have compared with
It is soft and its surface easily produces flaw this property compared with glass lens.If it is considered that the property selects high index of refraction
Plastic lens, then DAP is suitable.In addition, the DAP is also known as thermoset composition.
The technology of the thermoset composition (DAP) is taken as, for example Patent Document 1 discloses plastic lens molding
With the manufacture method of mould and plastic lens.Specifically, following method is disclosed：Using DAP as monomer, by the list
Body is filled to mould, its polymerization, solidification is then made by heating, so as to obtain lens.
In addition, being taken as the manufacture method of the plastic lens of thermoset composition, it is known to following technology：Using as
The basic composition injection moulding mould of plastic lens, hot briquetting mould (is for example joined so as to heat and solidify composition
According to patent document 2~5).
With 20 hours come heating combination in these patent documents, as a result, until terminating the solidification of composition needs
The time of 20 hours.
In addition, with above-mentioned requirements on the contrary, in order to manufacture high index of refraction and thicker plastic lens, it is known to following technology：
Polymerizable composition, polymerizable composition is filled to mould and enters trip temperature again and maintains or heat, then in order to prevent polymerization speed local
Rise and carry out refrigerating work procedure (referring for example to patent document 6).
In the patent document, until terminating the solidification of composition needs more than 20 hours (short again also to want more than 16 hours)
Time.
Prior art literature
Patent document
Patent document 1：Japanese Unexamined Patent Publication 6-339938 publications
Patent document 2：Japanese Unexamined Patent Publication 2005-107192 publications
Patent document 3：Japanese Unexamined Patent Publication 2005-131799 publications
Patent document 4：Japanese Unexamined Patent Publication 2007-261054 publications
Patent document 5：International publication number WO2009/017191 publications
Patent document 6：Japanese Unexamined Patent Publication 2009-226742 publications
The content of the invention
Problems to be solved by the invention
Such as the record also having in patent document 6, plastic lens is typically by making the composition in filling to mould
Solidify to be formed.However, making composition polymerization come in the case of solidifying, polymerization speed can change according to temperature.Therefore,
Slight temperature in composition, which is distributed with, may result in the rising for occurring partial polymerization speed, declines.
The molecular weight increase of rising, decline in the event of partial polymerization speed, the then such as part that polymerization speed rises
Other parts can be more than.The part can downwards settle or float upward in composition.And then, it is also possible in shaping mould
The inside (i.e. in composition) of tool produces convection current.Also, if composition solidifies in the state of above-mentioned vestige is remained, then mould
Material lens are possible to produce optical distortion, vein.
In order to suppress this optical distortion, the generation of vein, in patent document 2~5, so grown with more than 20 hours
Time carrys out heating combination.Even being provided with the patent document 6 of refrigerating work procedure in the midway of heating, until terminating composition
Solidify the short time for being also required to more than 16 hours again.
In this case, on the basis of the requirement from the side of wearer one as above-mentioned " aesthetic property ", " wear comfort "
On, in order to tackle " to increase production plastic lens " for the vigorous demand of plastic lens, in other words " shortening manufacturing time " this
The requirement from the side of plastic lens manufacturer one of sample also becomes strong.In order to meet this requirement, it is necessary to which shortening is consolidated to composition
Chemical industry sequence.
It is used as the gimmick for shortening curing process, it is contemplated that the hand of the curable temperature of composition is reduced using catalyst
Method.Shorten curing process using catalyst however, enabling, hard conating coating is being carried out to plastic lens resulting here
When (hard coat), dyeing, it is also possible to understand the compound to using in hard conating coating, dyeing used herein of catalyst
Produce harmful effect.
As a result, that is, enable and shorten curing process, it is also possible to hard conating coating, dyeing can not be carried out, so that institute can be caused
The scope of the end article of application narrows.
Even so, but if at will shortening curing process at a venture, then on the basis of above-mentioned optical distortion, vein also
It is possible to produce the plastic lens surface when composition is stripped from mould and uneven such defect occurs (below
The defect is referred to as " bumps ").
Worse, when wanting to shorten curing process, it is also possible to producing on the basis of " bumps ", " vein "
Defect, i.e. " malsegregation " produced before plastic lens is stripped from mould.It is somebody's turn to do " malsegregation " and refers to following production
Raw defect：During composition is solidified or after solidification, composition departs from mould, due to gravity with downside
Mould occurs to contact again, (is below also referred to as the defect " from mould " so as to produce malsegregation.Photo from mould is shown in meeting
The Fig. 5 illustrated in the project of embodiment described later.In addition, being shown in Fig. 6 described later from the mechanism that mould is produced).
Specifically, composition 4 departs from after mould 1 (Fig. 6 (c)), due to gravity, and said composition 4 at least can be with
The mould 1 (i.e. the use face 22a of the second mould 22) of downside occurs to contact again (Fig. 6 (d)).Thus, the even plastics of composition 4
The surface of lens can produce flaw, produce " from mould ".
Produced if in after curing process, although then to set other processes, these flaws can be by grinding, moving back
Fire or AR are coated with (antireflective coating, antireflection coating) to remove.However, just in case in the process of curing process
It is middle to produce, then it can produce flaw in the inside of plastic lens.
If so, these flaws be able to not can be removed by grinding etc., can only discard the plastic lens.As a result, only
Because wanting to shorten curing process and cause yield rate to reduce, it is impossible to meet above-mentioned requirements, this is present situation.
It is an object of the present invention to provide suppressing to solidify and produce the thermosetting composition of the possibility of defect with composition
The manufacture method of thing.
The solution used to solve the problem
The present inventor is in order to suppress the possibility that adjoint curing process shortens and produced defect, for existing curing process
Studied again.Now, the present inventor is especially conceived to " from mould " this defect to become the new temperature in curing process
Change method is studied.
By the research, the present inventor forms following understanding：" from mould " this defect is due to using with based on heat
Solidification and the composition that shrinks and produce.And speculate that " from mould " is produced as follows：Due to being combined in curing process
Thing is shunk so that composition departs from the surface of mould, so as to produce from mould.Also, at the same time also speculate, due to
Composition solidifies and make it that the surface of composition polishes, and it is also the original departed from that composition, which becomes to be easily separated from mould,
Cause.
Then, based on this supposition, the present inventor contemplates to set before heating process like that with patent document 6 and cooled down
The entirely different following gimmick of the gimmick of process：First the temperature of composition is dropped after the heating process that composition is solidified
It is low, then again so that the degree that the temperature of composition recovers the humidity province to cooling is heated up.
The composition shunk with the solidification based on heat would generally produce spontaneous heating.The heat of this spontaneous heating is in solidification
Increase in process, reach peak value, then reduce.It is essentially identical that this solidifies the degree carried out with composition.That is, with heat as above institute
Gradually changing for stating is same, and composition gradually solidifies, and its speed reaches peak value, and then curing rate is gradually reduced.
Then, the present inventor is conceived to the spontaneous heat of composition and reaches situation after peak value.Then the present inventor notes
Anticipate and arrive, on the one hand, the caloric value reduction, composition cooling of (i.e. composition) composition in mould, and on the other hand, with
The design temperature of past mould outer (i.e. thermoregulator) makes it heat up.As a result, temperature can be produced inside and outside mould
Degree is poor, and the composition that this temperature difference exactly makes surface polish departs from the main cause of mould, and the present inventor forms
As above recognize.
Based on this understanding, the present inventor speculates：If the solidification in composition in heating process has carried out more than half part
The temperature of composition is temporarily reduced such as the caloric value reduction for following composition afterwards, then at least is suppressing to produce this point from mould
On be effective.This is design with patent document 6, i.e. for structure that the increase with polymerization speed offseted and set refrigerating work procedure
Think entirely different design.
In addition, the present inventor forms following understanding：, can composite inhibiting by so temporarily reducing the temperature of composition
Depart from the possibility on the surface of mould.On this basis, by temporarily first suppressing solidification and then again so that the temperature of composition
The degree that degree recovers the humidity province to before cooling is heated up, and can maintain the adaptation between composition and mould
Solidify composition simultaneously.By the reciprocal change of this temperature, mould can be departed from composite inhibiting.As a result, this hair
A person of good sense forms following understanding：The solidification of composition can be completed while suppressing to produce from mould as described above, and made solid
Change degree is reached no less than conventional degree.
, then, then can be with 10 hours for example if if plastic lens using the composition containing DAP based on this understanding
Carry out curing process, and made plastic lens can significantly inhibit produce above-mentioned " bumps ", " vein ", " from mould " this
The possibility of the defect of sample.The fact that the experimental condition and result of embodiment 2~3 described later and comparative example 1~2 are being shown
Fig. 1 (a), also embodied in (b).
Further, since these defects can form shadow when to plastic lens irradiation light, thus it is following also by these defects
It is referred to as " shadow defect ".
It is as follows based on the embodiments of the present invention made are recognized above.
The first embodiment of the present invention is a kind of manufacture method of thermoset composition, it is characterised in that it has will
The composition shunk with the solidification based on heat is filled to the filling work procedure of the inside of mould and in foregoing filling work procedure
The curing process for afterwards solidifying by heating foregoing mould foregoing,
Said curing process has：
Heating process, it is foregoing to make by the combination for being heated up or being carried out to rise mild temperature maintenance to foregoing
Composition heats up from the temperature after foregoing filling work procedure；With
Depart from and suppress process, stop heating foregoing after foregoing heating process, make foregoing from foregoing
Temperature after heating process is set out until between the high and low temperature untill the temperature for reaching the humidity province after foregoing heating process again
Reciprocal change, so that the foregoing suppressed caused by being shunk caused by solidifying with foregoing departs from foregoing shaping
Mould.
Embodiment according to first embodiment, second embodiment of the present invention is characterised by that it enters one
The foregoing cooling of temperature of the step with the humidity province after foregoing heating process is up to after foregoing disengaging suppresses process,
And the stripping process for being stripped foregoing from foregoing mould.
Embodiment according to first or second embodiment, third embodiment of the present invention is characterised by,
Foregoing contains diallyl phthalate compound.
Embodiment according to the 3rd embodiment, the 4th embodiment of the invention is characterised by, foregoing solid
Chemical industry sequence was carried out within 10 hours.
Embodiment according to the 3rd or the 4th embodiment, the 5th embodiment of the invention is characterised by,
If be 100% from time of foregoing curing process start to finish, since foregoing curing process by least 80%
Time after start it is foregoing depart from suppress process.
The effect of invention
According to the present invention it is possible to suppress to solidify and produce the possibility of defect with composition.
Brief description of the drawings
Fig. 1 is the experimental condition and the figure of result for showing embodiment 2~3 and comparative example 1~2, and (a) is to show temperature adjustment
The figure of the design temperature of device and the relation of time, (b) is the glasses for showing to make in embodiment 2~3 and comparative example 1~2
The figure of the generation rate of shadow defect in plastic lens.
Fig. 2 be show the design temperature of the thermoregulator in embodiment 1 and time or composition actual temperature and when
Between relation figure.
Fig. 3 be show the design temperature of the thermoregulator in embodiment 4 and time, the actual temperature of thermoregulator with
The figure of the relation of the actual temperature and time of time or composition.
Fig. 4 is the design temperature and time or the actual temperature of composition for showing the thermoregulator in comparative example 1~2
With the figure of the relation of time.
Fig. 5 is the situation of shadow defect (from mould) extension in the plastic lens for show the glasses made in comparative example 2
Photo.
Fig. 6 be can be used for manufacture glasses plastic lens mould schematic diagram, be used for illustrate shadow defect (from
Mould) mechanism of production figure.
Description of reference numerals
1 mould
2 moulds (mold)
21 first moulds
21a (the first mould) uses face
22 second moulds
22a (the second mould) uses face
3 packing rings (gasket)
31 composition inlets
4 compositions
Embodiment
First, " focusing on the temperature change of thermoset composition in embodiment 1 " illustrates.
Then, " in embodiment 2 " to refinement " 1.C of embodiment 1 ") a) heating process and 1.C) b) depart from and press down
The Suitable examples of process processed are illustrated.
Hereafter, " focused in embodiment 3 " for the mould to being filled with thermoset composition inside it
The thermoregulator of temperature change, the i.e. design temperature of thermoregulator is assigned to illustrate.
Finally, " various modifications example is being illustrated in embodiment 4 ".
Embodiment 1
Describe embodiments of the present invention in detail referring to the drawings.
In the present embodiment, illustrated in the following order using Fig. 6.In addition, record below " stage I~V " is
Refer to the stage of the temperature change described in the Tables 1 and 2 of embodiment described later.
1. the manufacture method of thermoset composition
A thermoset composition) is prepared
B) filling work procedure
C) curing process (stage I~V)
A) heating process (stage I~III)
B) depart from and suppress process (stage IV~V)
I) cooling process (stage IV)
Ii) rewarming process (stage V)
D) stripping process
E) other processes
2. the effect obtained by embodiment
1. the manufacture method of thermoset composition
A thermoset composition) is prepared
In the present embodiment, as thermoset composition manufacture method an example, to manufacture glasses modeling
The situation of material lens is illustrated.In addition, as described above, " composition " in this specification includes having or once has thermosetting
The composition of this characteristic.That is, the composition (composition before heat cure) of the feed stage of plastic lens is represented sometimes, is also had
When represent after heat cure and D) composition (composition after heat cure) before stripping process.In addition, for convenience of description,
The plastic lens of glasses is referred to as " lens ".
In the present embodiment, as an example of composition, to containing diallyl phthalate compound
Composition is illustrated.The diallyl phthalate compound is therefore higher making due to higher refractive index
It is suitable during the lens of refractive index.In addition, diallyl phthalate compound is polymerize being used as monomer
In the case of form thermosetting resin.In addition, diallyl phthalate compound is shunk with the solidification based on heat.
It is of course also possible to be suitably added the compound in addition to diallyl phthalate compound in the composition.
And then, polymerization initiator etc. can also be suitably added into said composition.Detailed content " is carried out described later in embodiment 4 "
Explanation.In addition, in the present embodiment, the composition before curing process uses the material of liquid.
B) filling work procedure
Above-mentioned composition is thoroughly mixed, then filled said composition 4 to the mould 1 shown in Fig. 6 (a)
It is internal.The mould 1 is illustrated below.
Mould 1 has the first mould 21 and the second mould 22 and packing ring 3.In addition, also by the first mould 21 and the second mould 22
It is collectively referred to simply as " mould 2 ".The use face 21a of first mould 21 is preceding surface (i.e. from the point of view of the eyeglass wearer position to form lens
In front, target object side face) shape face.Also, the use face 22a of the second mould 22 is the rear table to form lens
The face of the shape in face (i.e. the face of eyeglass wearer side).First mould 21 and the second mould 22 are configured in mutually opposing mode.And
And, the packing ring 3 of ring-type is configured with around mould 2.Thus, the space of the die cavity as lens is formed by mould 2 and packing ring 3.And
And, composition 4 (Fig. 6 (b)) is injected from the composition inlet 31 being arranged in a part for packing ring 3 to the space.
In addition, in the present embodiment, the shape of the first mould 21 is so that the preceding surface of made lens has convex surface
Mode set.Conversely, the shape of the second mould 22 is set with making the rear surface of made lens have mode with concave surfaces
's.In addition, packing ring 3 both plays a role as the periphery maintaining part of mould 2, the effect for determining lens thickness is played again.
In addition, as mould 2 and the material of packing ring 3, as long as can by the injection moulding mould 1 of above-mentioned composition 4, make combination
The material that thing 4 polymerize is to use.But, as mould 2, preferably use in order that its is not easily damaged and be scratched and carry out
Cross the glass molding of chemical intensification treatment.
C) curing process (stage I~V in table 1)
Composition 4 is filled to mould 1, thermoregulator hot briquetting mould 1 is then used in this process, so that
Said composition 4 is set to polymerize, solidify.In this process, heating process (stage I~III in table 1) is carried out in first half term, rear
Half way, which depart from, suppresses process (stage IV~V in table 1).Curing process is illustrated below.
A) heating process (stage I~III)
In heating process, make combination by composition 4 being heated up or being carried out the combination of liter mild temperature maintenance
Thing 4 is from B) temperature heating after filling work procedure.In this process, make the gelation of composition 4 of liquid, then make it gradually solid
Change.In addition, " heating " in present embodiment is to instigate temperature continuously to rise, " temperature maintenance " refers to not carry out temperature change.
Therefore, " rise the combination that mild temperature is maintained " to refer to periodically be heated up, refer to " in the heating of a certain stage, and then
Next stage enter trip temperature maintenance " situation, also refer in contrast " enter in a certain stage trip temperature maintenance, and then
Next stage heating " situation.Sum it up, this process refers to the process without cooling.
B) depart from and suppress process (stage IV~V)
In the case where using monomers of the DAP as lens as in this embodiment, due to solidification, composition 4 itself
It can shrink.If so, as shown in Fig. 6 (c), despite before composition 4 is stripped from mould 1,
But composition 4 departs from mould 1 (i.e. composition 4 departs from the use face 21a of the first mould 21 and the use face 22a of the second mould 22)
Possibility can also increase.Especially, if its molding shrinkage is less than 1% if the monomer of conventional lens, and DAP has
Molding shrinkage is up to the high shrinkage of nearly 10% degree.Therefore, if using DAP, can produce it is compared with the past very
Easily occurs the situation that composition 4 departs from mould 1.
Composition 4 departs from after mould 1, and such as shown in Fig. 6 (d), said composition 4 at least can be with downside due to gravity
Mould 1 (i.e. the use face 22a of the second mould 22) occurs to contact again.Firstly, since this is contacted again, composition 4 can produce the flaw
Defect.
And then, in the formation lens of composition 4, the curvature of lens back-surface side part can be varied from due to contraction
The curvature (Fig. 6 (c)) of the curved surface of second mould 22 of mould 1.Then, if in the state for occurring this disengaging and contacting again
Lower carry out curing process, then can carry out curing process (Fig. 6 (d)) in the state of composition 4 is in contact with the second mould 22.If
Like this, the inside of composition 4 can form the flaw (flaw for being printed on a part of shape of the second mould 22) of circular die.
Incidentally, should be that can become significantly more defect when wanting and shortening curing process from mould.This is due to contracting
Short curing process this operation meaning：If assuming that the range of temperature of whole curing process is set into as in the past,
The rate of temperature change for composition 4 must then be improved.If so, it is necessary to steep temperature rise composition 4 and similarly
Drastically cool.If so, concavo-convex, vein is not only, and can all be increased from the possibility that mould is produced.
Therefore, in the present embodiment, for composite inhibiting 4, to depart from mould 2 such so as not to form Fig. 6 (c), (d)
State, so as to carry out this process.
In this process, first, stop heating composition 4.Then, said composition 4 is made from C) a) after heating process
Temperature is set out until reaching C again) back and forth change between high and low temperature untill the temperature of humidity province a) after heating process.Specifically
For, this process is by i) cooling process and ii) rewarming process the two processes are formed.
I) cooling process (stage IV)
In this process, depart from the surface of mould 1 come composite inhibiting 4 by temporarily reducing the temperature of composition 4.
Due to until the C that carries out before this process) a) heating process, composition 4 solidifying.
As described above, if composition 4 is solidified, the caloric value of composition 4 can reach peak value, then reduce, group
Compound 4 itself can tend to cooling.However, conventional, even in this in a flash, the temperature adjustment for hot briquetting mould 1
Device is still operated in the way of composition 4 is heated up.Therefore, in this process, in order to make up now produced temperature difference
And reduce the temperature of composition 4.That is, the reciprocal change of temperature is proceeded by from low temperature side.
Solidify composition 4 by carrying out above-mentioned operation, it is possible thereby to which the surface of composite inhibiting 4 becomes excessively light
It is sliding, it might even be possible to which that composite inhibiting 4 becomes prone to depart from mould 1, it can suppress to produce from mould.
Ii) rewarming process (stage V)
In the present embodiment, desuperheated composition 4 is made to recover again to original after above-mentioned i) cooling process is carried out
The temperature come.That is, the temperature of composition 4 is made to recover again to C) temperature of humidity province a) after heating process is (if this reality
Mode is applied, then is also that will carry out C) temperature b) i) before cooling process).It is this reciprocal between high and low temperature by carrying out
Change, can solidify composition 4 while the adaptation between composition 4 and mould 1 is maintained.That is, by i) dropping
Warm process temporarily to suppress solidification, and the surface of composite inhibiting 4 becomes excessively smooth so that between composition 4 and mould 1
There is a certain degree of adaptation.But, it is not enough there is also curing degree if composition 4 is cooled and is stripped like this
Possibility.Therefore, this process is carried out no less than conventional degree also for reaching curing degree.
In addition, be not that simple heating is carried out to composition 4 in this process, but having makes the temperature of composition 4 extensive
Again to " temperature of the humidity province after heating process " this feature., not only will not be due to excessively rising by so recovering temperature
Temperature and increase the possibility produced from mould again, and curing degree can be made to reach no less than conventional journey as described above
Degree.
Here, " temperature of the humidity province after heating process " preferably with the temperature after heating process to be mutually synthermal, can be with
It is accurately mutually synthermal not to be, can allow have when being stripped in stripping process described later by composition 4, be manufactured into lens
The curing degree of practicality can be stood and the temperature amplitude of the degree of flaw caused by from mould is not produced.In such as this embodiment party
In the case that formula so uses DAP as monomer, if being in a ratio of about ± 3 DEG C with the temperature after heating process, it can allow.
I more than) cooling process and ii) in rewarming process the two processes, by making the temperature of composition 4 back and forth become
Change, mould 1 can be departed from composite inhibiting 4.As a result, as set forth above, it is possible to be completed while can suppress and be produced from mould
The solidification of composition 4, and curing degree is reached no less than conventional degree.
In addition, as in this embodiment use DAP in the case of, C) b) depart from suppress process in temperature it is reciprocal
Change is preferably carried out with the temperature amplitude more than 3 DEG C.If temperature amplitude is more than 3 DEG C, fully it can consolidate composite inhibiting 4
Change, and can effectively suppress to produce from mould.
In addition, C) b) depart from suppress process preferably at least in C) a) solidify with above-mentioned composition 4 in heating process and carry out
Above-mentioned composition 4 spontaneous heating reach after peak value start.Thus, it is possible in C) a) solidification of composition 4 is entered in heating process
The reduction of the caloric value that composition 4 is positively followed after more than half part is gone, and can effectively suppress to produce from mould.
In addition, the contraction that the generation from mould occurs due to composition 4 with solidification.Therefore, molding shrinkage is higher,
Should easier generation composition 4 disengaging mould 1.However, by carrying out C as present embodiment) b) depart from suppression
Process, can also the generation disengaging of composite inhibiting 4 even if molding shrinkage height.Therefore, in the past due to molding shrinkage
The high and compound avoided, can also make lens etc. if present embodiment is used.I.e., it is possible to expand molding shrinkage
Application of the high material in product.
In addition, molding shrinkage is higher, the value for the effect that present embodiment is brought is bigger.As a result, if this implementation
The molding shrinkage of the composition 4 used in mode be more than 1%, then can improve composite inhibiting 4 depart from mould 1,
Even suppress to produce such effect from mould.
And then, for the thickness of lens, lens center part and the difference of the thickness of rims of the lens part are bigger, this implementation
The effect of mode is bigger.For example lens center part is very thin, rims of the lens part it is relatively thicker by comparison in the case of, even if
The overall molding shrinkage of lens is identical, and the amount of contraction of lens center part and rims of the lens part is also varied considerably.That is, with it is saturating
Mirror middle body is compared, and the amount of contraction of rims of the lens part is very big.As a result, equivalent to lens in use face 21a, 22a of mould 2
The part of marginal portion, the possibility that composition 4 departs from mould 1 can become very large.In this regard, by carry out this implementation
The C of mode) b) depart from suppression process, even so the lens of shape can also suppress to produce while system from mould
Make.If in addition, the thickness of lens center part (optic central part or geometric center part) is thinner than rims of the lens part
Thickness, then can more play the effect.
In addition, in C) b) ii) rewarming process when, the stage for the temperature for maintaining composition 4 can also be formed.That is, holding group
The temperature of compound 4 is substantially certain within a certain period of time, the temperature of composition 4 is recovered to C) temperature a) after heating process
Degree.Wherein, due to C) b) depart from the purpose for suppressing process also with the solidification of temporary transient composite inhibiting 4, therefore it is somebody's turn to do " certain time "
Being preferably set to the curing degree of the lens for finally manufacturing does not have the time of the length of effect.
In addition, setting from C) time of curing process start to finish as 100% when, C) b) depart from and suppress process and preferably exist
Since C) curing process begin to pass through at least 80% time after.If be said differently, setting from C) curing process
When the time of start to finish is 100%, C) a) heating process is preferably from C) curing process proceed by least 80% time.
As it was previously stated, a meaning of this process is to suppress by C) composition 4 shrinks caused combination in curing process
Thing 4 departs from use face 21a, 22a of mould 1.That is, this process can be on the surface whether composition 4 departs from mould 1
A certain degree of stage progress has been carried out for the stage of problem, i.e. solidification.In addition, the solidification of composition 4 is entered in heating process
After row is a greater part of, the caloric value of composition 4 reaches and carried out when being reduced after peak value in the way of following the temperature of composition 4 and reducing
Thermoregulator design temperature reduction it is also relevant with the condition setting of above-mentioned time.
As described above, in the present embodiment, being carried out after the time for preferably beginning to pass through at least 80% from curing process
C) b) depart from and suppress process.Thus, it is possible to which more effectively composite inhibiting 4 departs from mould 1.
And then, C) curing process carries out preferably within 10 hours.In addition, even in 10 hours progress C) curing process
Under the conditions of this, it is also preferred that ensuring C) time b) i) spent by cooling process is more than 1 hour.Also, now preferably with super
The temperature amplitude for crossing 3 DEG C carries out cooling process.This is because, by the composition 4 that so can fully cool, and can suppress
The surface of composition 4 becomes excessively smooth, can further suppress to produce from mould.
In addition, C) curing process can not be carried out within 10 hours, and alternatively shown in embodiment as be described hereinafter
Fig. 1, Fig. 2 and Fig. 3 shown in, by from whole C) from the point of view of curing process when rate of temperature change be set as 40 DEG C of (i.e. compositions 4
The difference of 40 DEG C of 80 DEG C of temperature maximum in temperature change and temperature minimum value) it is more than/more than 10 hours, i.e. 4.0 DEG C/h.
D) stripping process
Hereafter, the stripping process of the mold release compositions 4 from mould 1 is carried out.Now, preferably by C) b) depart from suppression work
Reach that the composition 4 of the temperature of the humidity province after heating process cools and the mold release compositions 4 from mould 1 after sequence.
E) other processes
After above-mentioned operation is carried out, composition 4 is surface-treated, is annealed, is cut or washed if necessary.
So manufacture the lens as product.
2. the effect obtained by embodiment
According to present embodiment, following effect can be played.That is, when manufacturing lens, 20 hours will can be needed conventional
The curing process of composition 4 more than (short again also to want 16 hours) is significantly foreshortened to less than 10 hours.And then, even if significantly shortening
Curing process, can also suppress the possibility that lens produce shadow defect (especially from mould).
As a result, can meet manufacture with high index lens when reduce lens edge thickness this for
The requirement of " aesthetic property " and weight increased " wear comfort " this requirement from the side of wearer one for suppressing lens, and
And can also meet in order to tackle " to increase production plastic lens " for the thriving demand of lens this come from lens manufacturers one
The requirement of side.
And then, if present embodiment, then catalysis need not be used to reduce the curable temperature of composition 4
Gained lens can successfully be carried out hard conating coating, dyeing by agent.As a result, curing process can be shortened, and can also be expanded
The application of big manufactured lens.
Embodiment 2
In the present embodiment, to refinement " 1.C of embodiment 1 ") a) heating process and 1.C) b) depart from and suppress work
The Suitable examples of sequence are illustrated.First, by C) a) heating process be divided into at least two stages illustrate heat up composition 4 feelings
Condition.Hereafter, by C) b) depart from the i for suppressing process) cooling process is divided into the feelings of publicly price-reduction temperature composition 4 at least two stages
Condition.
C) a) heating process (stage I~III)
I) the first heating process (stage II)
First, rate of temperature change is set as more than 2.5 DEG C/h and less than 5 DEG C/h in the first heating process.
By carrying out this temperature setting, it can suppress to produce the bumps produced due to the temperature change of the first half term of curing process.
Ii) the second heating process (stage III)
Make rate of temperature change higher than above-mentioned first heating process come the above-mentioned composition 4 that heats up after the first heating process.This
When, rate of temperature change is set at less than 12 DEG C/h.Set by carrying out this temperature after the first heating process is carried out
It is fixed, can be with the excessive convection current of generation in composite inhibiting 4.As a result, can also further it press down on the basis of bumps are inhibited
System is produced also due to the temperature change of the first half term of curing process and the vein that produces.
The heating process at least two stages is so set more than, can suppress to produce from mould, and can suppress
In addition shadow defect, the i.e. concavo-convex, generation of vein.
In addition, in addition to the first heating process and the second heating process, as long as make composition 4 after filling work procedure
Temperature heats up, then can set another process (such as stage I of table 1) being made up of heating and/or temperature maintenance.However, i.e.
Make stage by stage to be heated up, it is also preferred that followed by carrying out ii in above-mentioned i) the first heating process) the second heating process.
In addition, using rate of temperature change is set as more than 2.5 DEG C/h and temperature change stage less than 5 DEG C/h as
I) the first heating process, the heating process followed by carried out using this is ii) the second heating process, to meet said temperature rate of change
The mode of condition set be preferred.In addition, if by C) rate of temperature change of maximum a) is reached in heating process
Heating process is used as ii) the second heating process, then it can more effectively suppress the concavo-convex, generation of vein.
And then, never making from the viewpoint of composition 4 departs from mould 1, preferably in a) ii) the second heating process is followed by
Carry out b) and depart from suppression process.It is however also possible to which being taken place without between the two processes makes composition 4 depart from mould
The heating of 1 degree and/or temperature maintain process.
If in addition, from the viewpoint of fully being solidified, shortening hardening time, preferably in whole C) a) heating process
In persistently overheating composition 4.
C) b) depart from and suppress process
I) cooling process
1) the first cooling process
First, the rate of temperature change of composition 4 is set as more than 0 DEG C/h and less than 4 in the first cooling process
DEG C/h.As long as the original condition for meeting embodiment 1 can suppress the generation of shadow defect, but it can not be expected from generation is reduced
Shadow defect risk from the viewpoint of, more preferably in C) b) i) drastically cool in cooling process composition 4 not too much.By entering
The such temperature setting of row, can suppress to produce the shadow defect as caused by temperature change drastically.
2) the second cooling process
Make rate of temperature change higher than above-mentioned first cooling process come the above-mentioned composition 4 that cools after the first cooling process.This
When, rate of temperature change is set as the degree more than the first cooling process.By carrying out this temperature setting, it can reach original
Purpose, i.e. suppress from mould produce.
As above, the cooling process for being divided into two stages is set, is initially slowly cooled, then carries out phase therewith
Relatively quickly cooling, it is possible thereby to suppress can not expected shadow defect produce, and can also more effectively reach original
Purpose, i.e. suppression are produced from mould.
In addition, in addition to the first cooling process and the second cooling process, as long as from C) temperature a) after heating process
Cooling above-mentioned composition 4 is played, then another process being made up of cooling and/or temperature maintenance can be set.Wherein, come stage by stage
In the case of being cooled, preferably 2) the second cooling process is followed by carried out in above-mentioned 1) the first cooling process.
In addition, rate of temperature change to be set as more than 0 DEG C/h and less than 4 DEG C/h temperature change stages is 1) the
One cooling process, the cooling process followed by carried out using this is 2) the second cooling process, to meet the bar of said temperature rate of change
It is preferred that the mode of part, which set,.
And then, never make from the viewpoint of composition 4 departs from mould 1, preferably b) i) 2) after the second cooling process
Then b) ii is carried out) rewarming process.It is however also possible to carry out that the drop of the degree of shadow defect will not be produced between the two processes
Temperature and/or temperature maintain process.
If in addition, from the viewpoint of over-curing, the disengaging mould 1 of effective composite inhibiting 4 is suppressed, preferably existed
Whole C) b) i) continued down composition 4 in cooling process.Furthermore, it is understood that it is preferred that in C) b) depart from suppress process before it is not right
Composition 4 is cooled.
Embodiment 3
In the present embodiment, it is not as " from the temperature change from the point of view of composition 4 embodiment 1 ", but focused on
In for making setting for the thermoregulator of the internal generation temperature change of mould 1 filled with composition 4, i.e. thermoregulator
Constant temperature degree is illustrated.
Substantially, the temperature of thermoregulator is carried out in the way of composition 4 is reached the temperature conditionss of above-mentioned embodiment
Degree setting.But, in actually manufacture lens, sometimes the temperature of the design temperature of thermoregulator and actual composition 4 it
Between can produce difference.In the present embodiment, consider this difference and set to carry out the temperature of thermoregulator.
The temperature of this thermoregulator is set especially in C) b) i) in cooling process it is important.In above-mentioned embodiment
In, have been described that it is effective to carry out that cooling process is divided into two stages for composition 4.On the other hand, for this
The thermoregulator of embodiment, as shown in figure 3, being excellent to enter trip temperature setting in the way of carrying out the cooling process in a stage
Choosing.More specifically, by the rate of temperature change of the cooling process in a stage be set at less than 20 DEG C and with 1 hour with
On come the composition 4 that cools be preferred.
As described above, difference can be produced between the temperature of the design temperature of thermoregulator and actual composition 4.At this
In the case of kind, if the rate of temperature change of the design temperature of thermoregulator be set to too drastically, composition 4 can be with not
The state fully cooled is moved to next rewarming process.If so, the solidification carried out, knot can not can fully be suppressed
Really, it is impossible to suppress to produce from mould.
Therefore, in the present embodiment, the rate of temperature change of the design temperature of the thermoregulator in cooling process is set
It is set to and is less than 20 DEG C, was cooled composition 4 with more than 1 hour.Thus, it is possible to take time fully to suppress to solidify, and then can be with
More effectively suppress to produce from mould.
This is for wanting C) curing process control is particularly effective in the case of within 10 hours.Typically, if it is desired to contract
Short whole C) curing process, normally tend to shorten C therein) b) i) cooling process.However, just so-called " haste brings no success ",
Present embodiment is gone around, and the rate of temperature change of the design temperature of thermoregulator is set at less than into 20 DEG C, with 1 hour
Fully to cool composition 4 above.
In addition, the condition of the rate of temperature change and time are applicable not only to the design temperature of thermoregulator, it is also applied for
Composition 4.That is, in C) b) i) in cooling process, the rate of temperature change of composition 4 is set at less than 20 DEG C, with more than 1 hour
The composition 4 that fully to cool is also preferred.At this point it is possible to as " being divided into two stages embodiment 2 " is cooled
Process or the cooling process in a stage.
Embodiment 4
In addition, the technical scope of the present invention is not limited to above-mentioned embodiment, being also included within can draw by invention
Embodiment obtained from various changes, improvement is added in the scope of certain effects obtained from technical characteristic, its combination.
DAP is used in above-mentioned embodiment as monomer, but as long as being the composition shunk with the solidification based on heat
4, then it can also use material in addition.If for example, it is contemplated that composition 4 is solidified by polymerizeing or being crosslinked
Situation.
In addition, as the thermosetting resin in addition to DAP, phenolic resin, urea resin, ureaformaldehyde tree can be exemplified
Fat, melmac, polyester-melamine resin, melamine formaldehyde resin, alkyd resin, epoxy resin, epoxy-three
Cymel, unsaturated polyester resin, polyimide resin, acrylic resin, polyorganosiloxane resin, polyurethane resin,
Urethane methacylate resins, methacrylate resin, diallylcarbonate resin, PMMA resins (poly- methyl-prop
E pioic acid methyl ester resin), general double of thioxanthamide system resin, polycarbonate resin, episulfide system resin, resin
Curing components type acrylic resin (acrylic polyol solidfied material) etc..
In addition, in addition, such as can also include phenol resol resins, cresol novolac resin, bisphenol-A
The novolak phenolics such as novolac resin, the phenolic resin, bisphenol A epoxide resin, Bisphenol F ring such as bakelite
The bisphenol-type epoxy resins such as oxygen tree fat, the nobolak type epoxy such as phenolic resin varnish, cresol novolac epoxy
Resin, biphenyl type epoxy resin, 1,2- Stilbene-baseds epoxy resin, triphenol methane type epoxy resin, alkyl-modified triphenol first
The epoxy resin, urea such as alkane type epoxy resin, the epoxy resin containing triazine core, dicyclic pentylene modified phenol type epoxy resin
The resin containing triazine ring such as resin, melmac, unsaturated polyester resin, bimaleimide resin, organosilicon tree
Fat, the resin containing benzoxazine ring, cyanate ester resin, epoxide modified siloxanes etc., can use one kind in these or incite somebody to action
It is used in combination.
And then, further it can add ultra-violet absorber in monomer as DAP.If enumerating as ultraviolet radiation absorption
The example of agent, then can include selected from least one of benzophenone series and enumerate BTA system.Also, it is used as the benzophenone
It is ultra-violet absorber, 2,4-DihydroxyBenzophenone, 2- hydroxyl -4- acetoxyethoxies benzophenone, 2- can be included
Hydroxyl -4- methoxy benzophenones, 2,2 '-dihydroxy -4- methoxy benzophenones, 2,2 '-dihydroxy -4,4 '-dimethoxy
Benzophenone, 2-hydroxy-4-n-octoxybenzophenone, 2,2 '-dihydroxy -4,4 '-dimethoxy -5,5 '-disulfo hexichol
The sodium salt of ketone 2,2- hydroxyl -4- octyloxybenzophenones, 2,2 ', 4,4 '-tetrahydroxy -4- octyloxybenzophenones and 2,2 ',
4 '-trihydroxy -4- octyloxybenzophenones etc.；As enumerate BTA system ultra-violet absorber, 2- (2,4- dihydroxy can be included
Phenyl)-BTA, 2- (2,4,6- trihydroxy phenyl)-BTA, 2- (2 '-hydroxyl -5- octyl phenyls) BTA,
The chloro- 2- of 5- (2,4- dihydroxy phenyl)-BTA, the chloro- 2- of 5- (2,4,6- trihydroxy phenyl)-BTA, the bromo- 2- of 5-
(2,4- dihydroxy phenyl)-BTA, the bromo- 2- of 5- (2,4,6- trihydroxy phenyl)-BTA, two chloro- 2- (2,4- dihydroxies
Base phenyl)-BTA, Dibromo-dichloro -2- (2,4- dihydroxy phenyl)-BTA etc..Wherein, 2- hydroxyls are preferably selected from
Base -4- octyloxybenzophenones, 2,2 ', 4,4 '-tetrahydroxy -4- octyloxybenzophenones, 2,2 ', 4 '-trihydroxy -4- octyloxies
At least one of benzophenone and 2- (2 '-hydroxyl -5- octyl phenyls) BTA, particularly preferred 2,2 ', 4 '-trihydroxy -
4- octyloxybenzophenones.Certainly, can also be according to thermosetting composition even known ultra-violet absorber than that described above
The species of thing 4 is suitably selected.
Now, in order to adjust tone, known metallic particles or metal with the function for adjusting tone can be added
Compound.If for example, can include with composition, i.e. CoOAl2O3And/or CoAl2O4Cobalt compound, the Au of expression
Particulate etc..
And then, polymerization initiator can also be added in monomer as DAP.As polymerization initiator, as long as list can be made
Body polymerization is not particularly limited, and can use known material, be preferably selected from organic peroxide and organic azo chemical combination
At least one of thing.As the organic peroxide, benzoyl peroxide, methyl ethyl, peroxidating can be included
MEK, di-t-butyl peroxide, lauroyl peroxide, acetyl peroxide, di-isopropyl peroxydicarbonate, the carbon of peroxidating two
Sour double (4- t-butylcyclohexyls) ester, tert-butyl hydroperoxide -2 ethyl hexanoic acid ester, tertiary hexyl peroxidating -2 ethyl hexanoic acid esters etc.；Make
For organic azo compound, 2 can be included, 2 '-azo double bis-isobutyronitrile, 2,2 '-azo double (2 Methylpropionic acid methyl), 2,
2 '-azo double (2- methylbutyronitriles), 2,2 '-azo double (2,4- methyl pentane nitrile), 4,4 '-azo double (4- cyanopentanoic acids) etc..
Among these, benzoyl peroxide, di-isopropyl peroxydicarbonate and tert-butyl hydroperoxide -2- ethyl hexyls are preferably selected from
At least one of acid esters.
In addition, making C in the above-described embodiment) composition 4 before curing process is liquid, and can also use liquid or
The composition 4 of solid-state.As long as the composition 4 for making into liquid in mould 1 solidifies, does not hereafter make mould 1 and group
The situation that compound 4 departs from, you can the application present invention.That is, even in B) it is, for example, solid-state in filling work procedure, can also be in B) filling
C is carried out after the processing that fusing composition 4 is carried out after process) curing process.
In addition, for above-mentioned embodiment, in C) b) depart from suppress process in carried out a temperature change back and forth, and
Two temperature changes back and forth above can also be carried out.However, in this case, being needed after composition 4 is cooled once
Make it restore to C) temperature of humidity province a) after heating process.And need again to drop composition 4 from the temperature
Temperature, and equally make it restore to C) humidity province a) after heating process temperature.
In addition, setting the first mould in the way of the preceding surface for making made lens has convex surface in the above-described embodiment
21 shape, and can also have mode with concave surfaces in contrast with the preceding surface for making made lens and set the first mould 21
Shape.Equally, for the second mould 22, the shape opposite with above-mentioned embodiment can also be set to.In addition, the He of the first mould 21
Second mould 22 can be set in the way of so that the two sides of made lens has convex surface, can also be so that made
The two sides of lens has mode with concave surfaces and set.
In addition, in order to assign photochromism to the lens made in above-mentioned embodiment, following methods can be used：
The method that the coating (photochromic films) comprising photochromic pigment is set on lens substrate, is coated to photic by lens substrate
The method of color-changing membrane, configures method of photochromic films etc. between two panels lens substrate.
In addition, being illustrated in above-mentioned embodiment to glasses with plastic lens, but as long as being with consolidating based on heat
The composition changed and shunk can be using the present invention.Can be except glasses plastics are saturating if for example enumerating applicable example
The equimultiple type used in plastic optical component or duplicator, facsimile machine, LED printers beyond mirror etc.
Read the such folding of achromatic lens, variable focal length lens, the viewing lens (finder lens) of lens or camera
Penetrate rate profile plastic lens.
Embodiment
Then embodiment is provided to illustrate the present invention.Certainly, the present invention is not limited to following examples.
Embodiment 1
A thermoset composition) is prepared
The IPP-27 (Japanese grease manufacture) as polymerization initiator is added in diallyl phthalate, and is added
As the UV-5411 (SUN CHEMICAL COMPANT LTD. manufactures) of ultra-violet absorber, stir at normal temperatures, and subtracting
Pressure is de-gassed while stirring.Hereafter, stirred liquid is filtered, the composition used in the present embodiment is made.
B) filling work procedure
Filtered liquid is filled into the mould 1 shown in Fig. 6 (a).Specifically, from the note of composition inlet 31
Enter above-mentioned composition to be filled with to mould 1.In addition, making it under air atmosphere during injection, it will be used to be adjusted to
The design temperature of the thermoregulator of the temperature of pattern tool 1 is set as 42 DEG C.
C) curing process
For so filling to the composition 4 in mould 1, the temperature carried out in each stage as described in Table 1 becomes
Change.In addition, for the temperature change of table 1, the design temperature and time or the actual temperature of composition 4 of thermoregulator will be shown
Degree and the chart of the relation of time are shown in Fig. 2.In addition, carrying out needing 20 hours this process conventional with 10 hours.
In addition, for each stage, design temperature, the time needed for each stage, the temperature drawn by design temperature and time
Rate of change (DEG C/h) is different in each stage.In addition, for the temperature and rate of temperature change in following stage, showing
Numerical value in the setting of thermoregulator.For the temperature and rate of temperature change of actual composition 4, especially record every time.
Table 1
| Stage | Reach temperature setting (DEG C) | The time (hour) in stage | Rate of temperature change (DEG C/h) |
| Before curing process | 42 | - | - |
| I | 53 | 5 | 2.2 |
| II | 60 | 1.5 | 4.7 |
| III | 80 | 2 | 10 |
| IV | 70 | 0.5 | -20 |
| V | 85 | 1 | 15 |
A) heating process
In the present embodiment, as heating process, stage I~III is set.In addition, in the present embodiment, the rank in table 1
Section II (4.7 DEG C/h of rate of temperature change) is equivalent to i) the first heating process.In addition, stage III (10 DEG C of rate of temperature changes/small
When) equivalent to ii) the second heating process.
B) depart from and suppress process
In the present embodiment, as suppression process is departed from, stage IV~V is set.In addition, in the present embodiment, in table 1
Stage IV (- 20 DEG C/h of rate of temperature change) is i) cooling process, stage V (15 DEG C/h of rate of temperature change) is ii) rewarming
Process.
D) stripping process
Terminating above-mentioned C) after curing process, the composition 4 for being up to the temperature of the humidity province after heating process cools.
Then, mould 2 and packing ring 3 are pulled down, composition 4 is stripped.
E) other processes
Said composition 4 is made annealing treatment.Thus the glasses plastic lens in the present embodiment is obtained.
Embodiment 2~3
Embodiment 2~3 is in C) temperature change as shown in Fig. 1 (a) is carried out in curing process.In addition carry out with implementing
The same process of example 1.
Embodiment 4
Embodiment 4 is in C) in each stage temperature change as described in Table 2 is carried out in curing process.In addition, for table 2
Temperature change, the design temperature of thermoregulator and the actual temperature and the relation of time of time or composition 4 will be shown
Chart is shown in Fig. 3.In addition process similarly to Example 1 is carried out.
Table 2
| Stage | Reach temperature setting (DEG C) | The time (hour) in stage | Rate of temperature change (DEG C/h) |
| Before curing process | 42 | - | - |
| I | 53 | 5 | 2.2 |
| II | 60 | 1.5 | 4.7 |
| III | 77 | 1.5 | 11.3 |
| IV | 70 | 1 | -7 |
| V | 85 | 1 | 15 |
In addition, in example 4, for composition 4,1) the first cooling process and 2) i) b) are being carried out in cooling process
Two cooling process.On the other hand, the cooling process in a stage is set in thermoregulator, rate of temperature change is set as
It is set as more than 1 hour less than 20 DEG C, and by temperature fall time.
Comparative example 1~2
Comparative example 1 is in C) in each stage temperature change as described in Table 3 is carried out in curing process.And then, comparative example 2
Temperature change as described in Table 4 is carried out in each stage.In addition, for the temperature change of table 3 and table 4, will show that temperature is adjusted
The design temperature and time or the actual temperature of composition 4 and the chart of the relation of time for saving device are shown in Fig. 4.In addition enter
The process of row similarly to Example 1.
Table 3
| Stage | Reach temperature setting (DEG C) | The time (hour) in stage | Rate of temperature change (DEG C/h) |
| Before curing process | 40 | - | - |
| I | 40 | 1.5 | 0 |
| II | 50 | 4.5 | 2.2 |
| III | 55 | 1 | 5 |
| IV | 75 | 1.5 | 13.3 |
| V | 85 | 0.5 | 20 |
| VI | 85 | 1 | 0 |
Table 4
| Stage | Reach temperature setting (DEG C) | The time (hour) in stage | Rate of temperature change (DEG C/h) |
| Before curing process | 40 | - | - |
| I | 40 | 1.5 | 0 |
| II | 50 | 3 | 3.3 |
| III | 55 | 1 | 5 |
| IV | 75 | 2.5 | 8 |
| V | 85 | 1 | 10 |
| VI | 85 | 1 | 0 |
Evaluate
For the glasses plastic lens made in embodiment 1~4 and comparative example 1~2, the situation for examining shadow defect to produce
Or shadow defect generation rate.In addition, for shadow defect, being examined using high-pressure sodium lamp.Specifically, it will be thrown by above-mentioned high-pressure sodium lamp
The light penetrated is thrown on glasses plastic lens and is projected on curtain.Visually to observe the transmission picture.In addition, being produced for shadow defect
Raw rate, is calculated by the following method：Examined by above-mentioned visual observation in the glasses plastic lens made with same hand method
How is the quantity of the lens of generation shadow defect, so as to calculate.
It is unconfirmed to be produced to shadow defect firstly, for embodiment 1.Equally, it is also unconfirmed to arrive shadow defect for embodiment 4
Produce.
And then, shadow defect generation rate is examined to embodiment 2~3, shown in such as Fig. 1 (b), shadow defect generation rate be about 1% with
Under, shadow defect has obtained extremely effective suppression.
On the other hand, in comparative example 1~2, such as shown in Fig. 1 (b), shadow defect generation rate is about 10% or higher.Fig. 5 shows
The reason for having gone out this shadow defect generation rate increase.Fig. 5 is shown in the glasses plastic lens made in comparative example 2 from mould production
The figure of raw situation.Understand by Fig. 5 (a) sequentially into (e) from the situation that mould gradually extends.
As described previously for embodiment, although with needed for curing process conventional time (20 hours, it is short again
Want 16 hours) compared to the curing process for foreshortening to about 1/2~5/8 (10 hours), it also can effectively suppress shadow defect.On the other hand can
Know, in the comparative example of the present embodiment is not applied, it 10 hours is that can not suppress shadow defect simply just to foreshorten to curing process
Produce.
Other are attached below preferred embodiment.
Note 1
A kind of manufacture method of thermoset composition, it is characterised in that foregoing disengaging suppresses the reciprocal of the temperature in process
Change and carried out with the temperature amplitude more than 3 DEG C.
Note 2
A kind of manufacture method of thermoset composition, it is characterised in that foregoing disengaging suppresses process at least in foregoing heating
The spontaneous heating of the foregoing solidified in process with foregoing reaches to be started after peak value.
Note 3
A kind of manufacture method of thermoset composition, it is characterised in that the molding shrinkage of foregoing be 1% with
On.
Note 4
A kind of manufacture method of thermoset composition, it is characterised in that persistently overheating foregoing group in foregoing heating process
Compound.
Note 5
A kind of manufacture method of thermoset composition, it is characterised in that foregoing disengaging, which suppresses process, to be had to aforementioned combinatorial
The cooling process of thing and foregoing is set to recover to the rewarming work of the temperature after foregoing heating process after foregoing cooling process
Sequence,
Foregoing cooling process further has the first cooling process of cooling foregoing and in the foregoing first cooling work
Make rate of temperature change higher than foregoing first cooling process come the second cooling process of the foregoing that cools after sequence.
Note 6
A kind of manufacture method of thermoset composition, it is characterised in that foregoing heating process has heating foregoing
The first heating process and make after foregoing first heating process rate of temperature change higher than foregoing first heating process come before heating up
The second heating process of composition is stated,
The rate of temperature change of foregoing first heating process is more than 2.5 DEG C/h and less than 5 DEG C/h, foregoing second heating
The rate of temperature change of process is less than 12 DEG C/h,
Wherein, it regard the process that maximum temperature rate of change is reached in foregoing heating process as the second heating process.
Note 7
A kind of manufacture method of glasses plastic lens, it is characterised in that followed by carried out in foregoing first heating process
Foregoing second heating process.
Note 8
A kind of manufacture method of thermoset composition, it is characterised in that the foregoing cooling process of progress more than 1 hour, with
Temperature amplitude cooling foregoing more than 3 DEG C.
Note 9(below in relation to the design temperature of thermoregulator)
A kind of manufacture method of thermoset composition, it is characterised in that said curing process by will be used to making it is foregoing into
Pattern has the thermoregulator for occurring temperature change and is set to defined temperature conditionss to carry out,
The foregoing suppression process that departs from has the cooling process of cooling aforementioned temperature adjuster and made after foregoing cooling process
Aforementioned temperature adjuster recovers to the rewarming process of the temperature after foregoing heating process,
Foregoing cooling process by the rate of temperature change of the design temperature of aforementioned temperature adjuster be set at less than 20 DEG C/it is small
When, carried out with more than 1 hour.
Note 10
A kind of manufacture method of thermoset composition, it is characterised in that said curing process by will be used to making it is foregoing into
Pattern has the thermoregulator for occurring temperature change and is set to defined temperature conditionss to carry out,
The persistently overheating aforementioned temperature adjuster in foregoing heating process.
Note 11
A kind of manufacture method of thermoset composition, it is characterised in that said curing process by will be used to making it is foregoing into
Pattern has the thermoregulator for occurring temperature change and is set to defined temperature conditionss to carry out,
Foregoing heating process has the first heating process of heating aforementioned temperature adjuster and in foregoing first heating process
Make rate of temperature change higher than foregoing first heating process come the second heating process of the aforementioned temperature adjuster that heats up afterwards,
The rate of temperature change of foregoing first heating process is less than 5 DEG C/h, the rate of temperature change of foregoing second heating process
Less than 12 DEG C/h.
Note 12(following for summary)
A kind of manufacture method of thermoset composition, it is characterised in that it, which has, to be shunk with the solidification based on heat
Composition fill to the filling work procedure of the inside of mould and after foregoing filling work procedure by heating foregoing mould
To make the curing process that foregoing solidifies,
Said curing process has following process：
Heating process, it is foregoing to make by the combination for being heated up or being carried out to rise mild temperature maintenance to foregoing
Composition heats up from the temperature after foregoing filling work procedure；With
Depart from and suppress process, stop heating foregoing after foregoing heating process, make foregoing from foregoing
Temperature after heating process is set out until between the high and low temperature untill the temperature for reaching the humidity province after foregoing heating process again
Reciprocal change, so that the foregoing suppressed caused by being shunk caused by solidifying with foregoing departs from foregoing shaping
Mould,
Foregoing contains diallyl phthalate compound,
Said curing process was carried out within 10 hours,
The foregoing reciprocal change for departing from the temperature in suppression process is carried out with the temperature amplitude more than 3 DEG C, and then, if in the past
State curing process start to finish time be 100% when, have passed through since foregoing heating process more than 80% when
Between when carry out it is foregoing depart from suppress process.
Claims (7)
1. a kind of manufacture method of thermoset composition, it is characterised in that it, which has, to be shunk with the solidification based on heat
Composition fill to the filling work procedure of the inside of mould and after the filling work procedure by heat the mould come
Make the curing process of the composition solidification,
The curing process has following process：
Heating process, makes the combination by the composition being heated up or being carried out the combination of liter mild temperature maintenance
Thing is from the temperature heating after the filling work procedure, so that the composition gels, solidification；With
Depart from and suppress process, suppress the institute caused by being shunk caused by solidifying with the composition after the heating process
State composition and depart from the mould,
The suppression process that departs from has：Cooling process, the caloric value of composition reaches peak value described in the heating process
The temperature of the mould is reduced in the way of following the temperature of the composition and reduce when reducing afterwards, thus makes described group
Compound cools；Rewarming process, makes the temperature of the desuperheated composition recover again to described after the cooling process
The temperature of humidity province after heating process.
2. the manufacture method of thermoset composition according to claim 1, it is characterised in that it further has described
Depart from the composition cooling for the temperature for suppressing to be up to the humidity province after the heating process after process and by the combination
The stripping process that thing is stripped from the mould.
3. the manufacture method of thermoset composition according to claim 1 or 2, it is characterised in that the composition contains
Diallyl phthalate compound.
4. the manufacture method of thermoset composition according to claim 3, it is characterised in that the curing process is small 10
When within carry out.
5. the manufacture method of thermoset composition according to claim 3, it is characterised in that set from the curing process and open
When the time begun to end is 100%, since the curing process after at least 80% time it is described
Depart from and suppress process.
6. the manufacture method of thermoset composition according to claim 4, it is characterised in that set from the curing process and open
When the time begun to end is 100%, since the curing process after at least 80% time it is described
Depart from and suppress process.
7. the manufacture method of thermoset composition according to claim 1, it is characterised in that the cooling process has：
Make the first cooling process of the composition cooling；
Make rate of temperature change higher than first cooling process come the of the composition that cools after first cooling process
Two cooling process.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110137520.3A CN102794847B (en) | 2011-05-24 | 2011-05-24 | The manufacture method of thermoset composition |
| JP2012001831A JP5926561B2 (en) | 2011-05-24 | 2012-01-10 | Method for producing thermosetting composition |
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| CN201110137520.3A CN102794847B (en) | 2011-05-24 | 2011-05-24 | The manufacture method of thermoset composition |
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| CN102794847B true CN102794847B (en) | 2017-08-29 |
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| US20210079151A1 (en) | 2018-03-27 | 2021-03-18 | Mitsui Chemicals, Inc. | Method for setting polymerization condition and method for manufacturing optical material |
| KR102474121B1 (en) | 2018-07-24 | 2022-12-06 | 미쯔이가가꾸가부시끼가이샤 | Method for setting polymerization conditions, method for manufacturing optical materials |
| CN112612175B (en) * | 2020-12-16 | 2022-08-09 | 深圳市光科数字科技有限公司 | Miniature projection curtain and preparation process thereof |
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| JP2002069133A (en) * | 2000-06-16 | 2002-03-08 | Showa Denko Kk | Plastic lens material, method for producing the material, composition for plastic lens, plastic lens obtained by curing the composition and method for producing the plastic lens |
| JP2004209968A (en) * | 2002-12-18 | 2004-07-29 | Seiko Epson Corp | Method for producing plastic lens and raw material storage/supply apparatus |
| US20060192306A1 (en) * | 2005-02-25 | 2006-08-31 | The Microoptical Corporation | Manufacturing methods for embedded optical system |
| JP2006239977A (en) * | 2005-03-02 | 2006-09-14 | Seiko Epson Corp | Manufacturing method of plastic lens |
| JP2009226742A (en) * | 2008-03-24 | 2009-10-08 | Seiko Epson Corp | Manufacturing method of plastic lens |
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|---|---|---|---|---|
| CN1427767A (en) * | 2000-03-30 | 2003-07-02 | Q2100有限公司 | Apparatus and system for production of plastic lenses |
| CN1489706A (en) * | 2001-11-09 | 2004-04-14 | 大日本印刷株式会社 | Optical element |
| CN101321616A (en) * | 2005-12-21 | 2008-12-10 | 埃西勒国际通用光学公司 | Method for coating an ophthalmic lens within an injection molding machine |
| CN101765494A (en) * | 2007-07-25 | 2010-06-30 | Hoya株式会社 | Method for producing plastic lens |
| CN101339301A (en) * | 2008-08-06 | 2009-01-07 | 上海康耐特光学股份有限公司 | Shock resistance optical resin lens and method of manufacture |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102794847A (en) | 2012-11-28 |
| JP5926561B2 (en) | 2016-05-25 |
| JP2012240414A (en) | 2012-12-10 |
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