CN100417982C - A recycled method of mixed liquid crystal reclaimed from production line - Google Patents

A recycled method of mixed liquid crystal reclaimed from production line Download PDF

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Publication number
CN100417982C
CN100417982C CNB2005100219289A CN200510021928A CN100417982C CN 100417982 C CN100417982 C CN 100417982C CN B2005100219289 A CNB2005100219289 A CN B2005100219289A CN 200510021928 A CN200510021928 A CN 200510021928A CN 100417982 C CN100417982 C CN 100417982C
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liquid crystal
mixed liquid
vth
production surplus
reclaimed
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CN1952743A (en
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黄洪健
林秦
李铁
何志奇
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Shenzhen Holitech Optoelectronics Co Ltd
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BYD Co Ltd
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Abstract

The invention discloses a re-used method for the produced and recycled mixed liquid crystal. The produced and recycled mixed liquid crystal which is the same series of liquid crystal contains four kinds of monomer liquid crystal,recycles the residue after filled, and calculates the parameters(Deltn and Vth) needed for allocating liquid crystal using the common thickness tester and the electric measuring instrument which is widely used on the product line,and reuses it as the monomer with other monomer liquid crystal. The invention is convenient to use, low cost, and doesn't need expensive equipment, can improve the availability ratio of liquid crystal by 25%, and has high economic benefit.

Description

A kind of production surplus is reclaimed mixed liquid crystal and is utilized method again
Technical field
The present invention relates to a kind of production surplus recovery mixed liquid crystal and utilize method again, be used for mixed liquid crystal cycling and reutilization surplus on the production line and recovery.
Background technology
In production of liquid crystal displays, liquid crystal need be poured in the liquid crystal sylphon, be commonly called as and be " filling liquid ".Existing filling liquid mode mostly is slot type and sponge strip is irritated liquid.Sponge strip is irritated liquid because liquid crystal pollution is seriously replaced by slot type gradually.
The principle of slot type perfusion liquid crystal is: with the liquid crystal of single variety, perhaps by the liquid crystal after the different liquid crystal of multiple (as 4 kinds) homologous series are allocated according to desired parameters, inject liquid crystal utensil, put liquid crystal utensil, liquid crystal sylphon into the filling liquid chamber together, to irritate liquid chamber and the liquid crystal sylphon be contacted with liquid crystal after being evacuated, conveying N 2(nitrogen) pours into liquid crystal in the sylphon by capillary principle and pressure reduction.
The feature that slot type is irritated liquid is: the cleanliness of liquid crystal are higher, contaminated degree is lighter, but it can produce a certain proportion of surplus liquid crystal, as: the liquid crystal (4 bottles are mixed) of preparation 10 grams, the surplus liquid crystal of residual 4 grams of meeting in liquid crystal utensil, the surplus liquid crystal that will produce One's name is legion repeatedly like this.In order to reduce production costs, need carry out recycling to it.
At present the liquid crystal recovery method mainly contains two kinds: if one be the liquid crystal that has adopted single variety when irritating liquid, then can reclaim at the liquid crystal of single variety, its Δ n (optical anisotropy) and Vth (threshold voltage) are known, need only filter and to utilize again, its advantage is that Δ n and Vth are known, so can allocate accurately.But its range of adjustment is little, and owing to generally all adopt many bottles when at present irritating liquid and be mixed, the use of this kind method has significant limitation; Two, the plurality of liquid crystals at same series of products reclaims, because be mixed liquid crystal, its Δ n and Vth are unknown, after therefore filtering, need test key parameters such as Δ n and Vth by exact instrument.Its advantage is that the adjustable extent of this Δ n and Vth is big, and is easy to use.But it needs expensive exact instrument, and expense is higher.
Summary of the invention
The present invention needs the expensive higher shortcoming of exact instrument, expense in order to overcome in the prior art when mixed liquid crystal recycled, propose a kind of production surplus recovery mixed liquid crystal and utilize method again, can reclaim many bottles of mixed liquid crystals, do not need expensive exact instrument again, just can finish all test jobs in general LCD factory.
For achieving the above object, production surplus recovery mixed liquid crystal of the present invention utilizes method to comprise the steps: again
The raffinate that A irritates the different liquid crystal of homologous series behind the liquid reclaims, and obtains the production surplus and reclaims mixed liquid crystal;
The production surplus that B fails to understand above-mentioned composition, parameter is reclaimed mixed liquid crystal and is filtered;
C adopts the electrical measurement machine that generally uses on common thick tester of box and the production line to measure allotment liquid crystal desired parameters Δ n and Vth; Wherein Δ n is the optical anisotropy of liquid crystal, and Vth is the threshold voltage of liquid crystal;
D utilizes above-mentioned parameter Δ n and the Vth that records, and mixed liquid crystal is reclaimed in the production surplus utilize once again with other monomer liquid crystals as a monomer.
The present invention also comprises following improvement:
In steps A, the homologous series liquid crystal that will reclaim a period of time mixes, and carries out batch then and filters.
Filter type in step B is by adopting suitable suction flask and funnel to filter.
The method of measurement parameter Vth is in step C: adopt LCD electrical measurement machine by regulation voltage, when transferring to the picture sudden change, promptly negativity by blackly bleach, positivity when black, writes down this point voltage by leucismus, this voltage is reference voltage V1; Be approximately equal to Vth according to V1 then and draw the Vth value.
Method with the thick tester test of box Δ n in step C comprises the steps:
C-1 uses known mixed liquid crystal, adopts the standard sylphon of the thick d of known box to irritate liquid, as standard model;
C-2 carries out the test of Δ n*d to this standard model;
C-3 uses production surplus mixed liquid crystal, adopts as above method to irritate liquid, tests Δ n*d simultaneously;
C-4 calculates the Δ n of production surplus mixed liquid crystal according to following formula:
Δn1=Δn2*C1/C2
Wherein: Δ n1 is the optical anisotropy numerical value that liquid crystal has been filtered in the production surplus; Δ n2 is the optical anisotropy numerical value of standard monomer liquid crystal; C1 is the d* Δ n1 numerical value that liquid crystal has been filtered in the production surplus; C2 is the d* Δ n2 numerical value of standard monomer liquid crystal, and * represents multiplication sign.
Resistivity>10 of the mixed liquid crystal that obtains at step B 9Ω cm.
The vacuum tightness of filtering in step B is not less than 30 mm Hg (mmHg); And the uncovered perfusion case of putting into of the liquid crystal that will reclaim in steps A vacuumizes vacuum tightness<10 -2Mm Hg (mmHg), and kept 1 hour.
When in step D, utilizing liquid crystal once again, the mixed liquid crystal of known parameters Δ n and Vth is treated as monomer liquid crystal, allocated, so just have a plurality of Vth and Δ n with other many monomer liquid crystals, during allotment, be deployed into needed Vth and Δ n by linear relationship as required.
After adopting said method, the present invention can use and adopt the electrical measurement machine that generally uses on common thick tester of box and the production line to obtain allotment liquid crystal desired parameters (Δ n and Vth), utilizes once again with other monomer liquid crystals as a kind of monomer.The present invention is simple and practical, and cost is low, does not need expensive instrument and equipment, can make the liquid crystal utilization factor improve 25%, has high economic benefit.And through experiment confirm, it is feasible fully that the recovery of mixed liquid crystal is reclaimed in this produced in series surplus.
Embodiment
Method of testing of the present invention mainly is divided into three steps: 1. the filtration of liquid crystal is reclaimed in the production surplus; 2. the mensuration of optical anisotropy Δ n; 3. the mensuration of reference voltage V1.Wherein
Figure C20051002192800061
Wherein: n//for being parallel to the refractive index of molecular long axis; Be refractive index perpendicular to molecular long axis.The Vth threshold voltage is the voltage that penetrating light intensity changed 10% o'clock, and Vth is generally 1~3V.As described below, for fear of using expensive apparatus measures Vth, use V1 (reference voltage) among the present invention as the dosing parameter, this value approaches theoretical Vth.
Illustrate respectively below:
One, the 1. filtration of production surplus recovery liquid crystal;
The selection principle of equipment:
Select suitable suction flask and funnel according to the amount of liquid crystal of required processing, avoid the waste and the secondary pollution of liquid crystal.
Key instrument equipment:
1. G4 sand core funnel, (φ 50mm, φ 30mm, φ 80mm).
2. hard (borosilicate) glass suction flask (50ml, 100ml, 250ml, 500ml).
3. vacuum filtration system: vacuum pump, vacuum meter, safety flack, pressure pipe and perforated rubber stopper (cooperating) with the funnel suction flask.
Basic operation:
1. the instrument of all contact liquid crystal must clean dry no any residue, and again with high purity water flushing three times, oven dry was stand-by in the baking oven of cleaning after the suggestion container was cleaned; Reusable funnel, the organic solvent such as the washing with acetone of available Mos level (electron level) are clean.
2. select suitable apparatus for use according to the amount of liquid crystal of required processing, install vacuum apparatus.
3. the unlatching vacuum pump requires vacuum tightness can not be lower than 30mmHg, and liquid crystal is poured in the G4 funnel, filters, and liquid crystal enters suction flask.After waiting to have filtered, remove vacuum.
4. bubble in a large number before the can for preventing, the uncovered perfusion case of putting into of liquid crystal that needs to reclaim vacuumizes.Vacuum tightness<10 -2MmHg, and kept 1 hour.
5. whether the combination property parameter original with it of checking liquid crystal compares, can use with decision.
This recovery liquid crystal is necessary for color is not had significant change, does not mix moisture content, solvent and other impurity and the resistivity of liquid crystal>10 in the use significantly 9Ω cm.
Two, the mensuration of optical anisotropy Δ n:
Test philosophy:
Use the standard sylphon, use known parameters liquid crystal and production surplus to reclaim liquid crystal respectively and irritate liquid, measure the Δ n*d of two kinds of schemes respectively with the thick tester of box, wherein the thick d value of box identical (identical sylphon) can be obtained mixed liquid crystal Δ n thus.
Major equipment:
The thick tester of box, precision prescribed: ± 0.05.
Basic operation and computing formula:
1. use known mixed liquid crystal, adopt the thick standard sylphon of known box to irritate liquid, as mark
Accurate sample.
2. this standard model is carried out the test of Δ n*d.
3. use production surplus mixed liquid crystal, adopt as above method to irritate liquid, test Δ n*d simultaneously.
4. repeat above (1-3) step 3 time, obtain its mean value.
5. calculate the Δ n of production surplus mixed liquid crystal according to formula (1).
Computing formula (1):
d.Δn1/(d.Δn2)=C1/C2
So: Δ n1=Δ n2*C1/C2
Wherein: Δ n1: the optical anisotropy numerical value of liquid crystal has been filtered in the production surplus;
Δ n2: the optical anisotropy numerical value of standard monomer liquid crystal;
C1: the d* Δ n1 numerical value of liquid crystal has been filtered in the production surplus;
C2: the d* Δ n1 numerical value of standard monomer liquid crystal;
Three, the mensuration of reference voltage V1
Test philosophy:
Adopt LCD electrical measurement machine by regulation voltage, when transferring to picture sudden change (being bleached by black of negativity, positivity is black by leucismus), write down this point voltage, this voltage is reference voltage V1.Attention: V1 is a voltage of measuring, and is used for the approximate Vth that regards as and uses (dispense liquid parameter).Vth is meant threshold voltage, and it is the intrinsic parameter of liquid crystal, and the voltage when penetrance is suddenlyd change is the intrinsic attribute of liquid crystal exactly.Among the present invention, Vth the unknown of mixed liquid crystal.Show that according to experiment V1 is approximately equal to Vth, and V1 is easy to measure, therefore, the present invention utilizes measurement V to measure Vth's.
The electrical measurement machine was used to measure Von originally, and the present invention then surveys V1 with special use-pattern with it.Von generally is that penetrance is 50% o'clock a voltage, and we are that the employing penetrance is 10% o'clock a voltage for V1, therefore we can say that we determine V1 according to VON.The implication of Von is: in when work, some lines are arranged by gating at display, some are by gating, by gating be called the selection attitude, this voltage is for selecting voltage VON, non-state selection voltage is VOFF.And electrical measurement machine of the present invention is to measure whole the screen when all being gating, the voltage when normally showing.
Major equipment:
LCD Tester (comprising signal generator and power supply) is used to test VON, precision prescribed: ± 0.01V.
Basic operation:
1. according to the known parameters of production surplus mixed liquid crystal, estimate the minimum as far as possible scope of Vth earlier.
2. must select a suitable product to test V1, its requirement is to adopt the production surplus mixed liquid crystal that has filtered to irritate after the liquid, and the display effect of its glass when electrical measurement be normal (more approaching with the production standard product) relatively.
3. after using above-mentioned product to use production surplus mixed liquid crystal to irritate liquid at the 2nd it is tested, measure the V1 of a reference earlier.
4. use the 3rd reference V1, regard mixed liquid crystal as a new monomer, allocate (will carry out appropriate selection with reference to parameter in the selection of these three liquid crystal) propping up liquid crystal then with other three isonomic lists, select a suitable product or above-mentioned sylphon then at the 2nd, irritate liquid.
5. the 4th product is carried out electrical measurement, mainly investigate its display effect and V1, if with standardized product Vth certain difference is arranged, can reach institute by fine setting must an effect.
6. the 5th product is carried out reliability and the photoelectric characteristic aspect is measured, excessive to verify the difference of its performance and standardized product as difference, should consider its purposes carefully.
7. unclear owing to its Dopant (chirality agent) content, thus also must repeatedly finely tune it, so that obtain optimal display result.If the liquid crystal to Undopant reclaims, then need not carry out this step.(annotate: the direction of setting by us for the nematic liquid crystal that makes in the box is the shape aligned twisted in the shape of a spiral, and we often will add the cholesteric liquid crystal that a spot of hand of spiral and frictional direction are complementary, purpose be lure into mutually the row liquid crystal from the bottom of the box to box jacking row aligned twisted.A small amount of cholesteric liquid crystal of this adding, we just are referred to as the chirality agent, or are adjuvant, and its english name is called dopant.)
Case study on implementation: be that these mixed liquid crystals of four sections of mixed liquid crystals " C " " C " that the color liquid crystal C-STN process production surplus of certain company is reclaimed are comprised " C1 ", " C2 ", " C3 ", " C4 ", four kinds of monomers.
Following table is listed some correlation parameters of each monomer:
Liquid crystal parameter C(%) Δn V th(V)
C1 0.733 0.1285 1.27
C2 0.745 0.1597 1.32
C3 0.952 0.1281 2.07
C4 0.952 0.1597 2.12
4 sections of above liquid crystal belong to the homologous series liquid crystal, and through repeatedly reclaiming the surplus liquid crystal of producing, its composition and various parameter are all failed to understand.By this department being used the situation of this model liquid crystal, can be greatly to estimating its correlation parameter:
Mixed liquid crystal " C ":
C(%):0.80%-0.95%;
Δn:0.1400-0.1570;
V th(V):1.80V-2.10V;
By above correlation parameter, (appropriate sylphon is meant: select Vth or the sylphon of Δ n in its parameter area under the situation of the parameter of known general mixed liquid crystal to have selected an appropriate sylphon, can obtain higher precision when so accurately measuring), its correlation parameter is as follows:
Cell gap (the box degree of liquid crystal cell between two glass): 5.4UM;
Twist angle (twist angle of liquid crystal): 250 °;
Δ n*d: about 800;
Vth: 1.920V;
Test by repeatedly draws mixed liquid crystal " C ": some correlation parameters:
C(%): 0.80%-0.95%;
Δn: 0.154;
V th(V): 1.905V;
The mixed liquid crystal of known parameters Δ n and Vth treated as single liquid crystal prop up liquid crystal with other three lists and allocate, so just have 4 Vth and Δ n.During allotment, can be deployed into needed Vth and Δ n by linear relationship as required.
In this example, allocate by these parameters and this serial monomer " C2 ", " C3 ", " C4 ", its mixed ratio and correlation parameter see the following form.
Figure C20051002192800101
Use the product that above-mentioned liquid crystal filling produces and the comparison of its critical nature of standardized product, test data such as following table:
Figure C20051002192800111
Voltage Vop when wherein, so-called contrast is best is exactly the voltage of complete white or complete shiny black degree ratio when maximum.
By analyze top data as can be known the product of its crucial technical parameter and standard liquid crystal hardly differ, can reach requirement fully.The yield of its reliability and short run test manufacture simultaneously can both reach requirement, and its white, stain fraction defective<2% show that its filter effect is good.
From above analysis as can be known: it is feasible fully that the recovery of mixed liquid crystal is reclaimed in this produced in series surplus, allocate liquid crystal desired parameters Δ n and V1 also has enough precision can carry out utilizing once again with other liquid crystal as a monomer then in inferior use by filtering, use common LCD electrical measurement machine (being used to survey V1) and the thick tester of box (being used to test Δ n) to obtain it.This invention can bring bigger economy and technical benefits.
In sum, the present invention utilizes fixing liquid crystal cell, and mixed liquid crystal is reclaimed in the production surplus, promptly comprises the mixing composition of multiple monomer liquid crystal with a series of liquid crystal, behind the filling liquid raffinate process is reclaimed, and the liquid crystal that will repeatedly reclaim mixes; Through filtering, adopt the electrical measurement machine that generally uses on common thick tester of box and the production line to obtain allotment liquid crystal desired parameters (Δ n and Vth), utilize once again with other monomer liquid crystals as a monomer.The present invention is simple and practical, and cost is low, does not need expensive instrument and equipment, can make the liquid crystal utilization factor improve 25%, has high economic benefit.

Claims (9)

1. a production surplus is reclaimed mixed liquid crystal and is utilized method again, it is characterized in that comprising the steps:
A, the raffinate that the different liquid crystal of homologous series are irritated behind the liquid reclaim, and obtain the production surplus and reclaim mixed liquid crystal;
B, the production surplus recovery mixed liquid crystal that above-mentioned composition, parameter are failed to understand filter;
C, adopt the electrical measurement machine that generally uses on common thick tester of box and the production line to measure allotment liquid crystal desired parameters Δ n and Vth; Wherein Δ n is the optical anisotropy of liquid crystal, and Vth is the threshold voltage of liquid crystal;
D, utilize above-mentioned parameter Δ n and the Vth that records, mixed liquid crystal is reclaimed in the production surplus utilize once again with other monomer liquid crystals as a monomer.
2. production surplus according to claim 1 is reclaimed mixed liquid crystal and is utilized method again, and it is characterized in that: in steps A, the homologous series liquid crystal that will reclaim a period of time mixes, and carries out batch then and filters.
3. production surplus according to claim 1 and 2 is reclaimed mixed liquid crystal and is utilized method again, and it is characterized in that: the filter type in step B is by adopting suitable suction flask and funnel to filter.
4. production surplus according to claim 1 and 2 is reclaimed mixed liquid crystal and is utilized method again, it is characterized in that: the method for measurement parameter Vth is in step C: adopt LCD electrical measurement machine to pass through regulation voltage, when transferring to the picture sudden change, be negativity by black bleach, positivity is by leucismus when black, write down this point voltage, this voltage is reference voltage V1; Be approximately equal to Vth according to V1 then and draw the Vth value.
5. production surplus according to claim 1 and 2 is reclaimed mixed liquid crystal and utilized method again, it is characterized in that: the method with the thick tester test of box Δ n in step C comprises the steps:
C-1 uses known mixed liquid crystal, adopts the standard sylphon of the thick d of known box to irritate liquid, as standard model;
C-2 carries out the test of Δ n*d to this standard model;
C-3 uses production surplus mixed liquid crystal, adopts as above method to irritate liquid, tests Δ n*d simultaneously;
C-4 calculates the Δ n of production surplus mixed liquid crystal according to following formula:
Δn1=Δn2*C1/C2
Wherein: Δ n1 is the optical anisotropy numerical value that liquid crystal has been filtered in the production surplus; Δ n2 is the optical anisotropy numerical value of standard monomer liquid crystal; C1 is the d* Δ n1 numerical value that liquid crystal has been filtered in the production surplus; C2 is the d* Δ n2 numerical value of standard monomer liquid crystal.
6. production surplus according to claim 1 and 2 is reclaimed mixed liquid crystal and is utilized method again, it is characterized in that: resistivity>10 of the mixed liquid crystal that obtains at step B 9Ω cm.
7. production surplus according to claim 1 and 2 is reclaimed mixed liquid crystal and is utilized method again, and it is characterized in that: the vacuum tightness of filtering in step B is not less than 30 mm Hg.
8. production surplus according to claim 1 and 2 is reclaimed mixed liquid crystal and utilized method again, it is characterized in that: the uncovered perfusion case of putting into of the liquid crystal that will reclaim in steps A vacuumizes vacuum tightness<10 -2Mm Hg, and kept 1 hour.
9. production surplus according to claim 1 and 2 is reclaimed mixed liquid crystal and is utilized method again, it is characterized in that: when in step D, utilizing liquid crystal once again, the mixed liquid crystal of known parameters Δ n and Vth is treated as monomer liquid crystal, allocate with other many monomer liquid crystals, so just have a plurality of Vth and Δ n, during allotment, be deployed into needed Vth and Δ n by linear relationship as required.
CNB2005100219289A 2005-10-18 2005-10-18 A recycled method of mixed liquid crystal reclaimed from production line Expired - Fee Related CN100417982C (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI471159B (en) * 2011-09-02 2015-02-01 Ind Tech Res Inst Methods for recycling a recovery liquid crystal

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5540857A (en) * 1992-12-16 1996-07-30 Hitachi Chemical Co., Ltd. Purification of liquid crystals and liquid crystal composition
US6056892A (en) * 1997-03-06 2000-05-02 Mitsubishi Gas Chemical Company, Inc. Method for purifying liquid crystal
JP2002166259A (en) * 2000-11-30 2002-06-11 Sony Corp Recovery method of liquid crystal
JP2002244114A (en) * 2001-02-13 2002-08-28 Toray Eng Co Ltd Exfoliating method of bonded liquid crystal panel by solvent, and device thereof
JP2002254059A (en) * 2001-02-28 2002-09-10 Mitsubishi Materials Corp Material recovery method from liquid crystal display panel
CN1497036A (en) * 2002-09-26 2004-05-19 大日本油墨化学工业株式会社 Treatment method of reused liquid crystal material

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5540857A (en) * 1992-12-16 1996-07-30 Hitachi Chemical Co., Ltd. Purification of liquid crystals and liquid crystal composition
US6056892A (en) * 1997-03-06 2000-05-02 Mitsubishi Gas Chemical Company, Inc. Method for purifying liquid crystal
JP2002166259A (en) * 2000-11-30 2002-06-11 Sony Corp Recovery method of liquid crystal
JP2002244114A (en) * 2001-02-13 2002-08-28 Toray Eng Co Ltd Exfoliating method of bonded liquid crystal panel by solvent, and device thereof
JP2002254059A (en) * 2001-02-28 2002-09-10 Mitsubishi Materials Corp Material recovery method from liquid crystal display panel
CN1497036A (en) * 2002-09-26 2004-05-19 大日本油墨化学工业株式会社 Treatment method of reused liquid crystal material

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI471159B (en) * 2011-09-02 2015-02-01 Ind Tech Res Inst Methods for recycling a recovery liquid crystal

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