CN108865173A - A kind of preparation method of self assembly liquid crystal new material - Google Patents
A kind of preparation method of self assembly liquid crystal new material Download PDFInfo
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- C09K19/00—Liquid crystal materials
- C09K19/04—Liquid crystal materials characterised by the chemical structure of the liquid crystal components, e.g. by a specific unit
- C09K19/06—Non-steroidal liquid crystal compounds
- C09K19/08—Non-steroidal liquid crystal compounds containing at least two non-condensed rings
- C09K19/10—Non-steroidal liquid crystal compounds containing at least two non-condensed rings containing at least two benzene rings
- C09K19/14—Non-steroidal liquid crystal compounds containing at least two non-condensed rings containing at least two benzene rings linked by a carbon chain
- C09K19/16—Non-steroidal liquid crystal compounds containing at least two non-condensed rings containing at least two benzene rings linked by a carbon chain the chain containing carbon-to-carbon double bonds, e.g. stilbenes
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
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- C09K19/00—Liquid crystal materials
- C09K19/04—Liquid crystal materials characterised by the chemical structure of the liquid crystal components, e.g. by a specific unit
- C09K19/06—Non-steroidal liquid crystal compounds
- C09K19/08—Non-steroidal liquid crystal compounds containing at least two non-condensed rings
- C09K19/10—Non-steroidal liquid crystal compounds containing at least two non-condensed rings containing at least two benzene rings
- C09K19/14—Non-steroidal liquid crystal compounds containing at least two non-condensed rings containing at least two benzene rings linked by a carbon chain
- C09K19/16—Non-steroidal liquid crystal compounds containing at least two non-condensed rings containing at least two benzene rings linked by a carbon chain the chain containing carbon-to-carbon double bonds, e.g. stilbenes
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Abstract
The present invention relates to field of new material preparation, particularly with regard to a kind of preparation method of self assembly liquid crystal new material；Its technical solution is：Intermediate 1 with tetraphenylethylene structure is connect with rod shaped liquid crystal primitive intermediate 2, has synthesized a kind of liquid crystal molecule with self assembly characteristic；This programme uses the tetraphenylethylene with rotation paddle configuration as activated centre core, induced by changing liquid crystal unit, Length of spacer the luminous primitive of distortion in a limited space in be self-assembly of liquid crystalline phase, existing contradiction between solving liquid crystal and shining, turns waste into wealth the accumulation process of spontaneous liquid crystal molecule.
Description
Technical field
The present invention relates to field of material preparation, particularly with regard to a kind of preparation method of self assembly liquid crystal new material.
Background technique
Since liquid crystal is found, thousands of kinds of substances have shown the property of liquid crystal.As scientist is to substance
The further investigation and heightened awareness of state, it is believed that liquid crystal state is a kind of between isotropism liquid and solid new substance
State, and it is characterized in that order between solid-state and liquid；Liquid crystal material is in LCD industry using quite wide
It is general.
CN101046586A discloses a kind of liquid crystal material distributor：Spacer height measurement unit, to survey
Measure the spacer height on substrate；Liquid crystal material distributor, to be assigned to substrate according to surveyed spacer height determination
On liquid crystal material amount, and the liquid crystal material is assigned on substrate.
CN102836802A disclose it is a kind of can it is micro and the drippage of liquid crystal material is carried out with small spacing, result can make
The liquid crystal material drippage device and liquid crystal material coating method of the liquid crystal material layer thin thickness of liquid crystal display panel.The liquid crystal of the invention
Material applying device, liquid crystal material is coated on substrate, has the liquid crystal material stocking mechanism and liquid crystal of storage liquid crystal material
The internal pressure control mechanism and liquid that material stocking mechanism connects and is maintained within a predetermined range the internal pressure of liquid crystal material stocking mechanism
The applying mechanism of brilliant material stocking mechanism connection and the ink-jet mode being coated to liquid crystal material on substrate.Internal pressure control mechanism packet
It is born containing the gas supply part for supplying atmosphere or arbitrary gas to liquid crystal material stocking mechanism and to the supply of liquid crystal material stocking mechanism
The negative pressure feeding portion of pressure.
CN1497036A, which is provided, a kind of to be recycled from used liquid crystal board and recycles with reusable in the pure of liquid crystal board
The processing method of the liquid crystal material of degree and physical parameter.This method includes：(1) work for extracting liquid crystal material from liquid crystal board
Sequence, the process for the liquid crystal material that (2) purification extracts, the process of the physical parameter of the liquid crystal material of (3) measurement purification, and
(4) process of the physical parameter of the liquid crystal material is adjusted.
Traditional luminescent liquid crystal molecules generally have the characteristics that one, i.e. the characteristics of luminescence and liquid crystal liquid crystal property is total by the same big conjugation
The molecule of plane undertakes, and π-π is easily generated when gathering and stacks interaction and leads to fluorescent quenching, this phenomenon limits liquid crystal
The application of material.
Summary of the invention
To solve the above-mentioned problems, the present invention provides a kind of preparation methods of self assembly liquid crystal new material.
A kind of preparation method of self assembly liquid crystal new material, technology of preparing scheme are as follows：
According to mass fraction, by 4.2-6.2 parts of intermediate 1,11.2-15.5 parts of intermediate 2,9.6-10.6 parts of potassium carbonate
Acetonitrile with 80-100 parts is added in reaction kettle, is then vacuumized, and then uses the air in high pure nitrogen replacement reaction kettle, often
The secondary pumpdown time is 10-15min, is finally filled with high pure nitrogen, keeps normal pressure；It is warming up to 75-95 DEG C after the completion, reacts 70-
85h；Add 0.1-0.6 parts of trifluoro propyl dimethyl silicone polymer/vinyl trifluoro propyl dimethyl silicone polymer/silicon
Sesquioxyalkane cross-linked polymeric, 0.1-0.6 part polydimethyl diallyl ammonium chloride, 0.01-0.06 parts of dimethyl fluorene -2 9,9-,
7- hypoboric acid, 0.03-0.09 parts of lanthanum isopropoxide, reacts 1-5h by 60-85 DEG C；Solvent is evaporated after completing reaction, is then added
30-55 parts of diluted hydrochloric acid dissolution product collects organic phase, is then divided 5-10 times with 200-300 parts of methylene chloride and extracted,
A kind of self assembly liquid crystal green wood will can be obtained after drying, filtering in the anhydrous sodium sulfate of 30-40 parts of addition after filtrate solvent evaporated
Material.
The intermediate 1 is prepared according to following scheme：
According to mass fraction, 4, the 4- dihydroxy benaophenonel of 3.5-5.5 parts of zinc powder and 5-10 parts is added to reaction kettle
In, it then vacuumizes, then with the air in high pure nitrogen replacement reaction kettle, each pumpdown time is 10-15min, finally
It is filled with high pure nitrogen, keeps normal pressure；80-90 parts of tetrahydrofuran is added after completion into reaction kettle, uses liquid nitrogen after mixing evenly
System is cooled to subzero 65-75 DEG C, 2.8-3.6 parts of titanium tetrachloride is then slowly added dropwise into reaction kettle, is added dropwise
After stirring 20-30min afterwards, make system be warming up to naturally room temperature it is subsequent it is continuous be warming up to 70-90 DEG C, react 10-15h；Complete reaction
10-15 parts of dilute hydrochloric acid is added afterwards, is extracted after stirring 10-20min with water and methylene chloride, then be can be obtained after solvent evaporated
Intermediate 1.
The intermediate 2 is prepared according to following scheme：
According to mass fraction, by 2.5-3.5 parts of cyanobiphenyl phenol, 4.5-5.5 parts of bromododecane, 5.0-6.5 parts of carbon
Sour potassium and 70-90 parts of acetonitrile are added in reaction kettle, are then vacuumized, then with the sky in high pure nitrogen replacement reaction kettle
Gas, each pumpdown time are 10-15min, are finally filled with high pure nitrogen, keep normal pressure；It is warming up to 70-90 DEG C after the completion, instead
Answer 60-80h；Solvent is evaporated after completing reaction, 30-55 parts of diluted hydrochloric acid dissolution product is then added, then uses 200-300 parts
Methylene chloride divide 5-10 times and extracted, collect organic phase, being added after 30-40 part of anhydrous sodium sulfate dries, filters will filter
Intermediate 2 can be obtained after liquid solvent evaporated.
The solvent acetonitrile and tetrahydrofuran is all by stringent dry except water process.
The dilute hydrochloric acid concentration is 1%-5%.
A kind of preparation method of self assembly liquid crystal new material disclosed in the method for the present invention, this programme, which uses, has rotation paddle configuration
Tetraphenylethylene as activated centre core, induce the luminous primitive of distortion to exist by changing liquid crystal unit, Length of spacer
Be self-assembly of liquid crystalline phase in limited space, solve liquid crystal and shine between existing contradiction, spontaneous liquid crystal molecule
Accumulation process is turned waste into wealth.
Specific embodiment
The invention is described further below by specific embodiment：
Embodiment 1
A kind of preparation method of self assembly liquid crystal new material, technology of preparing scheme are as follows：
According to mass fraction, 1,13 parts of intermediate of 5.1 parts of 2,9.9 parts of intermediate of potassium carbonate and 85 parts of acetonitrile are added
Into reaction kettle, then vacuumize, then with the air in high pure nitrogen replacement reaction kettle, each pumpdown time is 12min,
It is finally filled with high pure nitrogen, keeps normal pressure；It is warming up to 79 DEG C after the completion, reacts 76h；Add 0.2 part of trifluoro propyl poly- two
Methylsiloxane/vinyl trifluoro propyl dimethyl silicone polymer/silsesquioxane cross-linked polymeric, 0.3 part of poly dimethyl diene
Propyl ammonium chloride, 0.03 part of 9,9- dimethyl fluorene -2,7- hypoboric acid, 0.06 part of lanthanum isopropoxide, react 2h by 67 DEG C；It completes
Solvent is evaporated after reaction, 38 parts of diluted hydrochloric acid dissolution product is then added, organic phase is collected, then with 260 parts of dichloromethane
Alkane, which divides 7 times, to be extracted, and one kind will can be obtained certainly in the anhydrous sodium sulfate of 35 parts of addition after filtrate solvent evaporated after drying, filtering
Assemble liquid crystal new material.
The intermediate 1 is prepared according to following scheme：
According to mass fraction, 4, the 4- dihydroxy benaophenonel of 4.5 parts of zinc powder and 8 parts is added in reaction kettle, then
It vacuumizes, then with the air in high pure nitrogen replacement reaction kettle, each pumpdown time is 13min, is finally filled with High Purity Nitrogen
Gas keeps normal pressure；85 parts of tetrahydrofuran is added after completion into reaction kettle, system is cooled to zero with liquid nitrogen after mixing evenly
Lower 70 DEG C, 3.2 parts of titanium tetrachloride is then slowly added dropwise into reaction kettle, after stirring 25min after being added dropwise, makes system certainly
So be warming up to room temperature it is subsequent it is continuous be warming up to 80 DEG C, react 13h；The dilute hydrochloric acid for completing 13 parts of addition after reacting, is used after stirring 15min
Water and methylene chloride extraction, then can be obtained intermediate 1 after solvent evaporated.
The intermediate 2 is prepared according to following scheme：
According to mass fraction, by 2.9 parts of cyanobiphenyl phenol, 5.0 parts of bromododecane, 5.7 parts of potassium carbonate and 80 parts
Acetonitrile is added in reaction kettle, is then vacuumized, then with the air in high pure nitrogen replacement reaction kettle, each pumpdown time
For 13min, it is finally filled with high pure nitrogen, keeps normal pressure；It is warming up to 80 DEG C after the completion, reacts 70h；Solvent is steamed after completing reaction
It is dry, 45 parts of diluted hydrochloric acid dissolution product is then added, is then extracted, is collected organic with methylene chloride point 8 times of 250 parts
After drying, filtering intermediate 2 will can be obtained after filtrate solvent evaporated in phase, the anhydrous sodium sulfate of 35 parts of addition.
The solvent acetonitrile and tetrahydrofuran is all by stringent dry except water process.
The dilute hydrochloric acid concentration is 3%.
Sample number into spectrum is CA-1.
Embodiment 2
A kind of preparation method of self assembly liquid crystal new material, technology of preparing scheme are as follows：
According to mass fraction, 1,11.2 parts of intermediate of 4.2 parts of 2,9.6 parts of intermediate of potassium carbonate and 80 parts of acetonitrile are added
Enter into reaction kettle, then vacuumize, then with the air in high pure nitrogen replacement reaction kettle, each pumpdown time is
10min is finally filled with high pure nitrogen, keeps normal pressure；It is warming up to 75 DEG C after the completion, reacts 70h；Add 0.1 part of trifluoropropyl
Base dimethyl silicone polymer/vinyl trifluoro propyl dimethyl silicone polymer/silsesquioxane cross-linked polymeric, 0.1 part of poly- diformazan
Base diallyl ammonium chloride, 0.01 part of 9,9- dimethyl fluorene -2,7- hypoboric acid, 0.03 part of lanthanum isopropoxide, 60 DEG C, reaction
1h；Solvent is evaporated after completing reaction, 30 parts of diluted hydrochloric acid dissolution product is then added, organic phase is collected, then with 200 parts
Methylene chloride, which divides 5 times, to be extracted, and the anhydrous sodium sulfate of 30 parts of addition will can be obtained after drying, filtering after filtrate solvent evaporated
A kind of self assembly liquid crystal new material.
The intermediate 1 is prepared according to following scheme：
According to mass fraction, 4, the 4- dihydroxy benaophenonel of 3.5 parts of zinc powder and 5 parts is added in reaction kettle, then
It vacuumizes, then with the air in high pure nitrogen replacement reaction kettle, each pumpdown time is 10min, is finally filled with High Purity Nitrogen
Gas keeps normal pressure；80 parts of tetrahydrofuran is added after completion into reaction kettle, system is cooled to zero with liquid nitrogen after mixing evenly
Lower 65 DEG C, 2.8 parts of titanium tetrachloride is then slowly added dropwise into reaction kettle, after stirring 20min after being added dropwise, makes system certainly
So be warming up to room temperature it is subsequent it is continuous be warming up to 70 DEG C, react 10h；The dilute hydrochloric acid for completing 10 parts of addition after reacting, is used after stirring 10min
Water and methylene chloride extraction, then can be obtained intermediate 1 after solvent evaporated.
The intermediate 2 is prepared according to following scheme：
According to mass fraction, by 2.5 parts of cyanobiphenyl phenol, 4.5 parts of bromododecane, 5.0 parts of potassium carbonate and 70 parts
Acetonitrile is added in reaction kettle, is then vacuumized, then with the air in high pure nitrogen replacement reaction kettle, each pumpdown time
For 10min, it is finally filled with high pure nitrogen, keeps normal pressure；It is warming up to 70 DEG C after the completion, reacts 60h；Solvent is steamed after completing reaction
It is dry, 30 parts of diluted hydrochloric acid dissolution product is then added, is then extracted, is collected organic with methylene chloride point 5 times of 200 parts
After drying, filtering intermediate 2 will can be obtained after filtrate solvent evaporated in phase, the anhydrous sodium sulfate of 30-40 parts of addition.
The solvent acetonitrile and tetrahydrofuran is all by stringent dry except water process.
The dilute hydrochloric acid concentration is 1%.
Sample number into spectrum CA-2.
Embodiment 3
A kind of preparation method of self assembly liquid crystal new material, technology of preparing scheme are as follows：
According to mass fraction, by 1,15.5 parts of intermediate of 6.2 parts of 2,10.6 parts of intermediate of potassium carbonate and 100 parts of acetonitrile
It is added in reaction kettle, then vacuumizes, then with the air in high pure nitrogen replacement reaction kettle, each pumpdown time is
15min is finally filled with high pure nitrogen, keeps normal pressure；It is warming up to 95 DEG C after the completion, reacts 85h；Add 0.6 part of trifluoropropyl
Base dimethyl silicone polymer/vinyl trifluoro propyl dimethyl silicone polymer/silsesquioxane cross-linked polymeric, 0.6 part of poly- diformazan
Base diallyl ammonium chloride, 0.06 part of 9,9- dimethyl fluorene -2,7- hypoboric acid, 0.09 part of lanthanum isopropoxide, 85 DEG C, reaction
5h；Solvent is evaporated after completing reaction, 55 parts of diluted hydrochloric acid dissolution product is then added, organic phase is collected, then with 300 parts
Methylene chloride, which divides 10 times, to be extracted, and the anhydrous sodium sulfate of 40 parts of addition will can obtain after drying, filtering after filtrate solvent evaporated
To a kind of self assembly liquid crystal new material.
The intermediate 1 is prepared according to following scheme：
According to mass fraction, 4, the 4- dihydroxy benaophenonel of 5.5 parts of zinc powder and 10 parts is added in reaction kettle, so
After vacuumize, then with the air in high pure nitrogen replacement reaction kettle, each pumpdown time is 15min, is finally filled with high-purity
Nitrogen keeps normal pressure；90 parts of tetrahydrofuran is added after completion into reaction kettle, is after mixing evenly cooled to system with liquid nitrogen
Subzero 75 DEG C, 3.6 parts of titanium tetrachloride is then slowly added dropwise into reaction kettle makes system after stirring 30min after being added dropwise
Naturally be warming up to room temperature it is subsequent it is continuous be warming up to 90 DEG C, react 15h；The dilute hydrochloric acid for completing 15 parts of addition after reacting, stirs 10-
It is extracted after 20min with water and methylene chloride, intermediate 1 then can be obtained after solvent evaporated.
The intermediate 2 is prepared according to following scheme：
According to mass fraction, by 3.5 parts of cyanobiphenyl phenol, 5.5 parts of bromododecane, 6.5 parts of potassium carbonate and 90 parts
Acetonitrile is added in reaction kettle, is then vacuumized, then with the air in high pure nitrogen replacement reaction kettle, each pumpdown time
For 15min, it is finally filled with high pure nitrogen, keeps normal pressure；It is warming up to 90 DEG C after the completion, reacts 80h；Solvent is steamed after completing reaction
It is dry, 55 parts of diluted hydrochloric acid dissolution product is then added, is then extracted, is collected organic with methylene chloride point 10 times of 300 parts
After drying, filtering intermediate 2 will can be obtained after filtrate solvent evaporated in phase, the anhydrous sodium sulfate of 40 parts of addition.
The solvent acetonitrile and tetrahydrofuran is all by stringent dry except water process.
The dilute hydrochloric acid concentration is 5%.
Sample number into spectrum CA-3.
Comparative example 1
Lanthanum isopropoxide, the other the same as in Example 1, obtained sample number into spectrum CA-4 is not added.
Comparative example 2
Bromododecane, the other the same as in Example 1, obtained sample number into spectrum CA-5 is not added.
Comparative example 3
Zinc powder, the other the same as in Example 1, sample number into spectrum CA-6 is not added.
Comparative example 4
It is poly- that trifluoro propyl dimethyl silicone polymer/vinyl trifluoro propyl dimethyl silicone polymer/silsesquioxane crosslinking is not added
It closes, the other the same as in Example 1, obtained sample number into spectrum CA-7.
Comparative example 5
Polydimethyl diallyl ammonium chloride, the other the same as in Example 1, obtained sample number into spectrum CA-8 is not added.
Comparative example 6
It is not added, 9,9- dimethyl fluorene -2,7- hypoboric acid, it is the same as embodiment 1, sample number into spectrum CA-9.
Table：The performance for the test specimen that different process is made compares.
Claims (5)
1. a kind of preparation method of self assembly liquid crystal new material, technology of preparing scheme are as follows：
According to mass fraction, by 4.2-6.2 parts of intermediate 1,11.2-15.5 parts of intermediate 2,9.6-10.6 parts of potassium carbonate
Acetonitrile with 80-100 parts is added in reaction kettle, is then vacuumized, and then uses the air in high pure nitrogen replacement reaction kettle, often
The secondary pumpdown time is 10-15min, is finally filled with high pure nitrogen, keeps normal pressure；It is warming up to 75-95 DEG C after the completion, reacts 70-
85h；Add 0.1-0.6 parts of trifluoro propyl dimethyl silicone polymer/vinyl trifluoro propyl dimethyl silicone polymer/silicon
Sesquioxyalkane cross-linked polymeric, 0.1-0.6 part polydimethyl diallyl ammonium chloride, 0.01-0.06 parts of dimethyl fluorene -2 9,9-,
7- hypoboric acid, 0.03-0.09 parts of lanthanum isopropoxide, reacts 1-5h by 60-85 DEG C；Solvent is evaporated after completing reaction, is then added
30-55 parts of diluted hydrochloric acid dissolution product collects organic phase, is then divided 5-10 times with 200-300 parts of methylene chloride and extracted,
A kind of self assembly liquid crystal green wood will can be obtained after drying, filtering in the anhydrous sodium sulfate of 30-40 parts of addition after filtrate solvent evaporated
Material.
2. a kind of preparation method of self assembly liquid crystal new material according to claim 1, it is characterised in that：The centre
Body 1 is prepared according to following scheme：
According to mass fraction, 4, the 4- dihydroxy benaophenonel of 3.5-5.5 parts of zinc powder and 5-10 parts is added to reaction kettle
In, it then vacuumizes, then with the air in high pure nitrogen replacement reaction kettle, each pumpdown time is 10-15min, finally
It is filled with high pure nitrogen, keeps normal pressure；80-90 parts of tetrahydrofuran is added after completion into reaction kettle, uses liquid nitrogen after mixing evenly
System is cooled to subzero 65-75 DEG C, 2.8-3.6 parts of titanium tetrachloride is then slowly added dropwise into reaction kettle, is added dropwise
After stirring 20-30min afterwards, make system be warming up to naturally room temperature it is subsequent it is continuous be warming up to 70-90 DEG C, react 10-15h；Complete reaction
10-15 parts of dilute hydrochloric acid is added afterwards, is extracted after stirring 10-20min with water and methylene chloride, then be can be obtained after solvent evaporated
Intermediate 1.
3. a kind of preparation method of self assembly liquid crystal new material according to claim 1, it is characterised in that：The centre
Body 2 is prepared according to following scheme：
According to mass fraction, by 2.5-3.5 parts of cyanobiphenyl phenol, 4.5-5.5 parts of bromododecane, 5.0-6.5 parts of carbon
Sour potassium and 70-90 parts of acetonitrile are added in reaction kettle, are then vacuumized, then with the sky in high pure nitrogen replacement reaction kettle
Gas, each pumpdown time are 10-15min, are finally filled with high pure nitrogen, keep normal pressure；It is warming up to 70-90 DEG C after the completion, instead
Answer 60-80h；Solvent is evaporated after completing reaction, 30-55 parts of diluted hydrochloric acid dissolution product is then added, then uses 200-300 parts
Methylene chloride divide 5-10 times and extracted, collect organic phase, being added after 30-40 part of anhydrous sodium sulfate dries, filters will filter
Intermediate 2 can be obtained after liquid solvent evaporated.
4. a kind of preparation method of self assembly liquid crystal new material according to claim 1, it is characterised in that：The solvent
Acetonitrile and tetrahydrofuran are all by stringent dry except water process.
5. a kind of preparation method of self assembly liquid crystal new material according to claim 1, it is characterised in that：Dilute salt
Acid concentration is 1%-5%.
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2018
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| CN101512397A (en) * | 2006-08-25 | 2009-08-19 | 新日本石油株式会社 | Retardation film, and liquid crystal display device using the same |
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