CN105255621A - Preparation method of semi water-based liquid crystal cleaning compound - Google Patents
Preparation method of semi water-based liquid crystal cleaning compound Download PDFInfo
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- CN105255621A CN105255621A CN201510620702.4A CN201510620702A CN105255621A CN 105255621 A CN105255621 A CN 105255621A CN 201510620702 A CN201510620702 A CN 201510620702A CN 105255621 A CN105255621 A CN 105255621A
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Abstract
The invention discloses a preparation method of a semi water-based liquid crystal cleaning compound, and belongs to the technical field of cleaning. According to the preparation method, polyoxyethylene polyoxypropylene block polyether is taken as a surfactant; additives such as an emulsifier, a chelating agent, an organic base, and sodium metasilicate pentahydrate are added so as to obtain the semi water-based liquid crystal cleaning compound. Toxicity of the polyoxyethylene polyoxypropylene block polyether surfactant is low, and the surfactant possesses acidic and basic stability, and excellent decontamination effects; adding of the chelating agent and the organic base is capable of removing metal ions on liquid crystal surfaces; a cleaning method is simple; operation is simple; and the semi water-based liquid crystal cleaning compound is friendly to the environment.
Description
Technical field
The invention discloses a kind of preparation method of half aq. type liquid crystal cleaning agent, belong to cleaning technique field.
Background technology
Current most enterprise uses fluorine Lyons (CFC-113), 1,1, and the ozone consuming substances such as 1-trichloroethane, tetracol phenixin (being called for short ODS) cleans as electronic cleaning agent.Due to them, to have chemical stability good, toxicity is little, do not burn, and surface tension is less, do not damage by cleaning material and strong many advantageous characteristic such as perviousness, rapid-drying properties can be kept, being widely used as the clean-out system of kinescope, printed circuit board (PCB), semi-conductor, electronic machine, precision component, liquid-crystal display etc.But they exist following defect: there is the material damaged the ozone layer in (1) clean-out system, to limit and replace their use at present; (2) pollutent remained in LCD micro slit is not easily removed; (3) efficiency of existing clean-out system cleaning is not high; (4) effectively can not remove the metal ion of LCD remained on surface, cause electrode corrode by the metal ion that remains and cause serious consequence.So this emerging industry of ODS substitute is arisen at the historic moment, and develop rapidly.
The non-ODS cleaning technique used at LCD production industry in the world at present has: aq. type cleaning technique, half aq. type cleaning technique, solvent-borne type cleaning technique.Developing efficient aq. type clean-out system or half aq. type clean-out system, replace leaning solvent as much as possible, is the developing direction of clean-out system.Although the associated problem that leaning solvent faces in Environment protection and safety problem are more, the advantages such as it has, and cleaning efficiency is high, the recyclable recycling of solvent, technique are simple, aqueous cleaning agent can not replace leaning solvent completely.But research and develop novel
Efficient water base metal cleaning agent or semi-aqueous cleaning agent, improve it and recycle value, and replacing solvent cleaner as much as possible has become a kind of trend.
Research purpose of the present invention, be want to develop a kind of milk sap i.e. half aq. type clean-out system, not only cleaning performance is good, environmentally friendly, and merge the advantage of leaning solvent, cleaning is simple to operation simultaneously, and this clean-out system will have broad mass market prospect.
Summary of the invention
The technical problem that the present invention mainly solves: effectively can not remove the residual metal ion of liquid crystal surfactant for current liquid crystal cleaning agent, electrode is caused to be remained the drawback of corrosion, provide a kind of preparation method of half aq. type liquid crystal cleaning agent, the present invention utilizes and prepares polyoxyethylene polyoxypropylene block polyether for tensio-active agent, add emulsifying agent wherein again, sequestrant, organic bases, a kind of half aq. type liquid crystal cleaning agent prepared by the auxiliary agents such as metasilicate pentahydrate sodium, use polyoxyethylene polyoxypropylene block polyether tensio-active agent toxicity little in scavenging solution of the present invention, to ph stability, there is better soil-removing action, add the metal ion that sequestrant and organic bases effectively can remove liquid crystal surfactant, and cleaning is simple to operation, environmentally friendly.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
A preparation method for half aq. type liquid crystal cleaning agent, is characterized in that concrete preparation process is:
(1) count by weight, choose 10 ~ 15 parts of sodium lauryl sulphate respectively, 10 ~ 20 parts of polyoxyethylene polyoxypropylene block polyethers, the fatty alcohol-polyoxyethylene ether of 5 ~ 8 parts and 10 ~ 15 parts of trihydroxy ethylamine oleate soaps are added in there-necked flask, add in flask again in the deionized water of 40 ~ 50 parts, be warming up to 50 ~ 60 DEG C, use magnetic stirrer 30 ~ 40min simultaneously, solution is mixed;
(2) the above-mentioned solution mixed first is warming up to 80 ~ 90 DEG C, take the thanomin of total mass 5 ~ 8% more respectively as emulsifying agent, the butyl glycol ether of total mass 15 ~ 20% joins in mixing solutions as the EDTA of solubility promoter and total mass 0.2 ~ 0.3% as sequestrant, and continue stirring 20 ~ 25min, stir rear standing solution 5 ~ 6min;
(3) metasilicate pentahydrate sodium of total mass 5% is added in the solution after above-mentioned leaving standstill, at maintaining the temperature at 80 ~ 90 DEG C, massfraction 20 ~ 30% thanomin organic bases is slowly dripped again in mixing solutions, regulator solution pH to 11 ~ 12, carry out stirring reaction 30 ~ 40min afterwards, mixing speed is 400 ~ 500r/min;
(4) in above-mentioned reacted solution, then add total mass 5 ~ 10% dehydrated alcohol, after continuing stirring 10 ~ 20min, solution is cooled to room temperature, obtains a kind of half aq. type liquid crystal cleaning agent.
Described fatty alcohol-polyoxyethylene ether general formula is RO (CH
2cH
2o) nH, R=C
8~ C
10, n=4 ~ 8.
The preparation process of described polyoxyethylene polyoxypropylene block polyether is:
(1) propylene glycol first adding 100 ~ 200g in 1L stainless steel autoclave is initiator, the KOH of total quality of material 0.3 ~ 0.5g is added as catalyzer after being warming up to 100 ~ 120 DEG C, and nitrogen is passed in reactor, the oxyethane of 100 ~ 200g is slowly added, reaction 10 ~ 15min in reactor;
(2) reactor is warming up to 160 ~ 180 DEG C after terminating by above-mentioned reaction, and continues to pass into nitrogen, keeps still internal pressure to be 0.2MPa, then in reactor, slowly adds the propylene oxide of 100 ~ 200g, reaction 30 ~ 40min under the condition stirred;
(3) above-mentioned reaction slowly adds the oxyethane of 100 ~ 200g again after terminating, and by reactor inside holding at 180 ~ 200 DEG C, still internal pressure is 0.3Mpa, and reaction is cooled to room temperature, then discharging after aging, obtains polyoxyethylene polyoxypropylene block polyether.
Application method of the present invention: the present invention is prepared half aq. type liquid crystal cleaning agent and be applied in liquid crystal cleaning, first 27mm × 23mm size, the liquid crystal display 10 of thick 7 μm is got, use 50 ~ 70kHZ, 120 ~ 140W small-scale ultrasonic cleaning clean, scavenging period 5 ~ 10min, liquid crystal display is put into before start, shut down after getting screen, take out rear range estimation and use polaroid to check degree of cleaning, discovery liquid crystal display surface non-metallic ion is residual
1.the invention has the beneficial effects as follows:
(1) the polyoxyethylene polyoxypropylene block polyether tensio-active agent toxicity that uses of the present invention is little, to ph stability, has preferably wetting, emulsification, soil-removing action;
(2) half aq. type liquid crystal cleaning agent of the present invention adds the metal ion that sequestrant and organic bases effectively can remove liquid crystal surfactant, and cleaning is simple.
Embodiment
First count by weight, choose 10 ~ 15 parts of sodium lauryl sulphate respectively, 10 ~ 20 parts of polyoxyethylene polyoxypropylene block polyethers, the fatty alcohol-polyoxyethylene ether of 5 ~ 8 parts and 10 ~ 15 parts of trihydroxy ethylamine oleate soaps are added in there-necked flask, add in flask again in the deionized water of 40 ~ 50 parts, be warming up to 50 ~ 60 DEG C, use magnetic stirrer 30 ~ 40min simultaneously, solution is mixed; The solution mixed first is warming up to 80 ~ 90 DEG C, take the thanomin of total mass 5 ~ 8% more respectively as emulsifying agent, the butyl glycol ether of total mass 15 ~ 20% joins in mixing solutions as the EDTA of solubility promoter and total mass 0.2 ~ 0.3% as sequestrant, and continue stirring 20 ~ 25min, stir rear standing solution 5 ~ 6min; The metasilicate pentahydrate sodium of total mass 5% is added in solution after leaving standstill, at maintaining the temperature at 80 ~ 90 DEG C, massfraction 20 ~ 30% thanomin organic bases is slowly dripped again in mixing solutions, regulator solution pH to 11 ~ 12, carry out stirring reaction 30 ~ 40min afterwards, mixing speed is 400 ~ 500r/min; In solution after the reaction, then add total mass 5 ~ 10% dehydrated alcohol, after continuing stirring 10 ~ 20min, solution is cooled to room temperature, obtains a kind of half aq. type liquid crystal cleaning agent.
Described fatty alcohol-polyoxyethylene ether general formula is RO (CH
2cH
2o)
nh, R=C
8~ C
10, n=4 ~ 8.
The preparation process of described polyoxyethylene polyoxypropylene block polyether is:
First the propylene glycol first adding 100 ~ 200g in 1L stainless steel autoclave is initiator, the KOH of total quality of material 0.3 ~ 0.5g is added as catalyzer after being warming up to 100 ~ 120 DEG C, and nitrogen is passed in reactor, the oxyethane of 100 ~ 200g is slowly added, reaction 10 ~ 15min in reactor; After reaction terminates, reactor is warming up to 160 ~ 180 DEG C, and continues to pass into nitrogen, keep still internal pressure to be 0.2MPa, then in reactor, slowly add the propylene oxide of 100 ~ 200g, reaction 30 ~ 40min under the condition stirred; Again slowly add the oxyethane of 100 ~ 200g after reaction terminates, and by reactor inside holding at 180 ~ 200 DEG C, still internal pressure is 0.3Mpa, reaction is cooled to room temperature, then discharging after aging, obtains polyoxyethylene polyoxypropylene block polyether.
Example 1
First count by weight, choose 10 parts of sodium lauryl sulphate respectively, 20 parts of polyoxyethylene polyoxypropylene block polyethers, the fatty alcohol-polyoxyethylene ether of 5 parts and 15 parts of trihydroxy ethylamine oleate soaps are added in there-necked flask, add in flask again in the deionized water of 50 parts, be warming up to 50 DEG C, use magnetic stirrer 30min simultaneously, solution is mixed; The solution mixed first is warming up to 80 DEG C, take the thanomin of total mass 5% more respectively as emulsifying agent, the butyl glycol ether of total mass 15% joins in mixing solutions as the EDTA of solubility promoter and total mass 0.2 ~ % as sequestrant, and continue stirring 20 ~ 25min, stir rear standing solution 5min; The metasilicate pentahydrate sodium of total mass 5% is added in solution after leaving standstill, at maintaining the temperature at 80 DEG C, then in mixing solutions, slowly drip massfraction 20% thanomin organic bases, regulator solution pH to 11, carry out stirring reaction 30min afterwards, mixing speed is 400r/min; In solution after the reaction, then add total mass 5% dehydrated alcohol, after continuing to stir 10min, solution is cooled to room temperature, obtains a kind of half aq. type liquid crystal cleaning agent.
Described fatty alcohol-polyoxyethylene ether general formula is RO (CH
2cH
2o)
nh, R=C
8, n=4.
The preparation process of described polyoxyethylene polyoxypropylene block polyether is:
First the propylene glycol first adding 100g in 1L stainless steel autoclave is initiator, the KOH of total quality of material 0.3g is added as catalyzer after being warming up to 100 DEG C, and nitrogen is passed in reactor, in reactor, slowly add the oxyethane of 100g, reaction 10min; After reaction terminates, reactor is warming up to 160 DEG C, and continues to pass into nitrogen, keep still internal pressure to be 0.2MPa, then in reactor, slowly add the propylene oxide of 100g, under the condition stirred, react 30min; Again slowly add the oxyethane of 100g after reaction terminates, and by reactor inside holding at 180 DEG C, still internal pressure is 0.3Mpa, reaction is cooled to room temperature, then discharging after aging, obtains polyoxyethylene polyoxypropylene block polyether.
The present invention being prepared half aq. type liquid crystal cleaning agent is applied in liquid crystal cleaning, first 27mm × 23mm size, the liquid crystal display 10 of thick 7 μm is got, 50kHZ, 120W small-scale ultrasonic cleaning is used to clean, scavenging period 5min, liquid crystal display is put into before start, shut down after getting screen, take out rear range estimation and use polaroid to check degree of cleaning, discovery liquid crystal display surface non-metallic ion is residual
Example 2
First count by weight, choose 15 parts of sodium lauryl sulphate respectively, 15 parts of polyoxyethylene polyoxypropylene block polyethers, the fatty alcohol-polyoxyethylene ether of 7 parts and 15 parts of trihydroxy ethylamine oleate soaps are added in there-necked flask, add in flask again in the deionized water of 48 parts, be warming up to 55 DEG C, use magnetic stirrer 35min simultaneously, solution is mixed; The solution mixed first is warming up to 85 DEG C, take the thanomin of total mass 6% more respectively as emulsifying agent, the butyl glycol ether of total mass 17% joins in mixing solutions as the EDTA of solubility promoter and total mass 0.25% as sequestrant, and continue to stir 23min, stir rear standing solution 5min; The metasilicate pentahydrate sodium of total mass 5% is added in solution after leaving standstill, at maintaining the temperature at 85 DEG C, then in mixing solutions, slowly drip massfraction 25% thanomin organic bases, regulator solution pH to 11 ~ 12, carry out stirring reaction 35min afterwards, mixing speed is 450r/min; In solution after the reaction, then add total mass 7% dehydrated alcohol, after continuing to stir 15min, solution is cooled to room temperature, obtains a kind of half aq. type liquid crystal cleaning agent.
Described fatty alcohol-polyoxyethylene ether general formula is RO (CH
2cH
2o)
nh, R=C
9, n=4 ~ 8.
The preparation process of described polyoxyethylene polyoxypropylene block polyether is:
First the propylene glycol first adding 150g in 1L stainless steel autoclave is initiator, the KOH of total quality of material 0.4g is added as catalyzer after being warming up to 110 DEG C, and nitrogen is passed in reactor, in reactor, slowly add the oxyethane of 150g, reaction 13min; After reaction terminates, reactor is warming up to 170 DEG C, and continues to pass into nitrogen, keep still internal pressure to be 0.2MPa, then in reactor, slowly add the propylene oxide of 150g, under the condition stirred, react 35min; Again slowly add the oxyethane of 150g after reaction terminates, and by reactor inside holding at 190 DEG C, still internal pressure is 0.3Mpa, reaction is cooled to room temperature, then discharging after aging, obtains polyoxyethylene polyoxypropylene block polyether.
Application method of the present invention: the present invention is prepared half aq. type liquid crystal cleaning agent and be applied in liquid crystal cleaning, first 27mm × 23mm size, the liquid crystal display 10 of thick 7 μm is got, 60kHZ, 130W small-scale ultrasonic cleaning is used to clean, scavenging period 7min, liquid crystal display is put into before start, shut down after getting screen, take out rear range estimation and use polaroid to check degree of cleaning, discovery liquid crystal display surface non-metallic ion is residual
Example 3
First count by weight, choose 13 parts of sodium lauryl sulphate respectively, 15 parts of polyoxyethylene polyoxypropylene block polyethers, the fatty alcohol-polyoxyethylene ether of 8 parts and 15 parts of trihydroxy ethylamine oleate soaps are added in there-necked flask, add in flask again in the deionized water of 49 parts, be warming up to 60 DEG C, use magnetic stirrer 40min simultaneously, solution is mixed; The solution mixed first is warming up to 90 DEG C, take the thanomin of total mass 8% more respectively as emulsifying agent, the butyl glycol ether of total mass 20% joins in mixing solutions as the EDTA of solubility promoter and total mass 0.3% as sequestrant, and continue to stir 25min, stir rear standing solution 6min; The metasilicate pentahydrate sodium of total mass 5% is added in solution after leaving standstill, at maintaining the temperature at 90 DEG C, then in mixing solutions, slowly drip massfraction 30% thanomin organic bases, regulator solution pH to 12, carry out stirring reaction 40min afterwards, mixing speed is 500r/min; In solution after the reaction, then add 10% dehydrated alcohol, after continuing stirring 10 ~ 20min, solution is cooled to room temperature, obtains a kind of half aq. type liquid crystal cleaning agent.
Described fatty alcohol-polyoxyethylene ether general formula is RO (CH
2cH
2o)
nh, R=C
10, n=4 ~ 8.
The preparation process of described polyoxyethylene polyoxypropylene block polyether is:
First the propylene glycol first adding 200g in 1L stainless steel autoclave is initiator, the KOH of total quality of material 0.5g is added as catalyzer after being warming up to 120 DEG C, and nitrogen is passed in reactor, in reactor, slowly add the oxyethane of 200g, reaction 15min; After reaction terminates, reactor is warming up to 180 DEG C, and continues to pass into nitrogen, keep still internal pressure to be 0.2MPa, then in reactor, slowly add the propylene oxide of 200g, under the condition stirred, react 40min; Again slowly add the oxyethane of 200g after reaction terminates, and by reactor inside holding at 200 DEG C, still internal pressure is 0.3Mpa, reaction is cooled to room temperature, then discharging after aging, obtains polyoxyethylene polyoxypropylene block polyether.
The present invention being prepared half aq. type liquid crystal cleaning agent is applied in liquid crystal cleaning, first 27mm × 23mm size, the liquid crystal display 10 of thick 7 μm is got, 70kHZ, 140W small-scale ultrasonic cleaning is used to clean, scavenging period 10min, liquid crystal display is put into before start, shut down after getting screen, take out rear range estimation and use polaroid to check degree of cleaning, discovery liquid crystal display surface non-metallic ion is residual.
Claims (3)
1. a preparation method for half aq. type liquid crystal cleaning agent, is characterized in that concrete preparation process is:
(1) count by weight, choose 10 ~ 15 parts of sodium lauryl sulphate respectively, 10 ~ 20 parts of polyoxyethylene polyoxypropylene block polyethers, the fatty alcohol-polyoxyethylene ether of 5 ~ 8 parts and 10 ~ 15 parts of trihydroxy ethylamine oleate soaps are added in there-necked flask, add in flask again in the deionized water of 40 ~ 50 parts, be warming up to 50 ~ 60 DEG C, use magnetic stirrer 30 ~ 40min simultaneously, solution is mixed;
(2) the above-mentioned solution mixed first is warming up to 80 ~ 90 DEG C, take the thanomin of total mass 5 ~ 8% more respectively as emulsifying agent, the butyl glycol ether of total mass 15 ~ 20% joins in mixing solutions as the EDTA of solubility promoter and total mass 0.2 ~ 0.3% as sequestrant, and continue stirring 20 ~ 25min, stir rear standing solution 5 ~ 6min;
(3) metasilicate pentahydrate sodium of total mass 5% is added in the solution after above-mentioned leaving standstill, at maintaining the temperature at 80 ~ 90 DEG C, massfraction 20 ~ 30% thanomin organic bases is slowly dripped again in mixing solutions, regulator solution pH to 11 ~ 12, carry out stirring reaction 30 ~ 40min afterwards, mixing speed is 400 ~ 500r/min;
(4) in above-mentioned reacted solution, then add total mass 5 ~ 10% dehydrated alcohol, after continuing stirring 10 ~ 20min, solution is cooled to room temperature, obtains a kind of half aq. type liquid crystal cleaning agent.
2. the preparation method of a kind of half aq. type liquid crystal cleaning agent according to claim 1, is characterized in that: described fatty alcohol-polyoxyethylene ether general formula is RO (CH
2cH
2o)
nh, R=C
8~ C
10, n=4 ~ 8.
3. the preparation method of a kind of half aq. type liquid crystal cleaning agent according to claim 1, is characterized in that: the preparation process of described polyoxyethylene polyoxypropylene block polyether is:
(1) propylene glycol first adding 100 ~ 200g in 1L stainless steel autoclave is initiator, the KOH of total quality of material 0.3 ~ 0.5g is added as catalyzer after being warming up to 100 ~ 120 DEG C, and nitrogen is passed in reactor, the oxyethane of 100 ~ 200g is slowly added, reaction 10 ~ 15min in reactor;
(2) reactor is warming up to 160 ~ 180 DEG C after terminating by above-mentioned reaction, and continues to pass into nitrogen, keeps still internal pressure to be 0.2MPa, then in reactor, slowly adds the propylene oxide of 100 ~ 200g, reaction 30 ~ 40min under the condition stirred;
(3) above-mentioned reaction slowly adds the oxyethane of 100 ~ 200g again after terminating, and by reactor inside holding at 180 ~ 200 DEG C, still internal pressure is 0.3Mpa, and reaction is cooled to room temperature, then discharging after aging, obtains polyoxyethylene polyoxypropylene block polyether.
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Cited By (6)
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| CN107245387A (en) * | 2017-05-19 | 2017-10-13 | 合肥市惠科精密模具有限公司 | A kind of TFT LCD displays water-base cleaning liquid and preparation method thereof |
| CN107354018A (en) * | 2017-05-20 | 2017-11-17 | 合肥市惠科精密模具有限公司 | A kind of high-efficiency environment friendly LCDs cleaning agent |
| CN108570683A (en) * | 2018-06-28 | 2018-09-25 | 广东剑鑫科技股份有限公司 | A kind of steel mesh aqueous cleaning agent and preparation method thereof |
| CN108690742A (en) * | 2018-06-25 | 2018-10-23 | 安徽全兆光学科技有限公司 | A kind of optical mirror slip cleaning agent |
| CN108690747A (en) * | 2018-06-25 | 2018-10-23 | 安徽全兆光学科技有限公司 | A kind of photovoltaic chip detergent |
| CN113214915A (en) * | 2021-04-26 | 2021-08-06 | 深圳市恒享表面处理技术有限公司 | Oil removing agent and preparation method thereof |
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| CN108690742A (en) * | 2018-06-25 | 2018-10-23 | 安徽全兆光学科技有限公司 | A kind of optical mirror slip cleaning agent |
| CN108690747A (en) * | 2018-06-25 | 2018-10-23 | 安徽全兆光学科技有限公司 | A kind of photovoltaic chip detergent |
| CN108570683A (en) * | 2018-06-28 | 2018-09-25 | 广东剑鑫科技股份有限公司 | A kind of steel mesh aqueous cleaning agent and preparation method thereof |
| CN113214915A (en) * | 2021-04-26 | 2021-08-06 | 深圳市恒享表面处理技术有限公司 | Oil removing agent and preparation method thereof |
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