Embodiment
Protection screen red cloth curtain instrument, as shown in Figure 1, comprise fixed head 15, the first set casing 1 is installed in the side of fixed head 15, the opposite side of fixed head 15 installs the second set casing 17, fixed head 15 is installed the first stationary shaft 5 and the second stationary shaft 14, the first roll shaft 2 is installed in one end of first stationary shaft 5, first roll shaft 2 is positioned at the first set casing 1, first roll shaft 2 is installed the first cloth curtain 3, the other end of the first stationary shaft 5 installs the first gear 6, first gear 6 is positioned at the second set casing 17, the second roll shaft 11 is installed in one end of second stationary shaft 14, second roll shaft 11 is positioned at the first set casing 1, second roll shaft 11 is installed the second cloth curtain 12, the other end of the second stationary shaft 14 installs the 3rd gear 16, 3rd gear 16 is positioned at the second set casing 17, push-rod electric machine 8 is installed in second set casing 17 inside, drive motor 10 is installed in the pull bar end of push-rod electric machine 8, the output shaft of drive motor 10 installs the second gear 7, second gear 7 can coordinate with the first gear 6 or the 3rd gear 16, the first described cloth curtain (3) and the second cloth curtain (12) scribble the high temperature resistant dye composite of the redness formed by following components by weight percent: 1-phenyl-3-methyl-5-pyrazolone 30 ~ 40 parts, 5,8-dihydroxy-1,4-naphthoquinones 20 ~ 30 parts, 1-(4-sulfonic group phenyl)-3-carboxyl-5-pyrazolone 20 ~ 30 parts, sodium lauroyl sarcosine 5 ~ 8 parts, sorbitan monostearate 4 ~ 7 parts, polyglyceryl fatty acid ester 2 ~ 5 parts, colouring stabilizer IFI-85112 ~ 4 part, polyvinyl alcohol (PVA) 3 ~ 6 parts and microcrystalline cellulose 2 ~ 5 parts.
The invention provides the protection screen red cloth curtain instrument that red cloth curtain is changed in a kind of automatic realization.Push-rod electric machine 8 of the present invention can drive drive motor 10 to move up and down; make the 3rd gear 16 can respectively with the first gear 6 or the second gear 7; make drive motor 10 that the first roll shaft 2 can be driven to rotate or drive the second roll shaft 11 to rotate; thus realize the switching of different red cloth curtain, thus make protection screen red cloth curtain instrument, without the need to staff is manual, red cloth curtain be taken off the replacing that just can realize red cloth curtain.
The first counterweight 4 is installed in the bottom of described first cloth curtain 3.First counterweight 4 of the present invention can facilitate the first cloth curtain 3 under the gravity sag of the first counterweight 4.
The second counterweight 13 is installed in the bottom of described second cloth curtain 12.Second counterweight 13 of the present invention can facilitate the second cloth curtain 12 under the gravity sag of the second counterweight 13.
The preparation method of described redness is high temperature resistant dye composite, comprise the steps: with parts by weight, by 1-phenyl-3-methyl-5-pyrazolone 30 ~ 40 parts, 5, 8-dihydroxy-1, 4-naphthoquinones 20 ~ 30 parts, 1-(4-sulfonic group phenyl)-3-carboxyl-5-pyrazolone 20 ~ 30 parts, sodium lauroyl sarcosine 5 ~ 8 parts, sorbitan monostearate 4 ~ 7 parts, polyglyceryl fatty acid ester 2 ~ 5 parts, colouring stabilizer IFI-85112 ~ 4 part, polyvinyl alcohol (PVA) 3 ~ 6 parts and microcrystalline cellulose 2 ~ 5 parts add in the water of 40 ~ 50 parts, open muller, when the particle diameter of mensuration particle is between 1 ~ 2.5 μm, stop grinding, dye solution through grinding is dry on atomizing drying equipment, obtain red high temperature resistant dye composite.
First cloth curtain (3) and the second cloth curtain (12) also can scribble the high temperature resistant dye composite of the redness formed by following components by weight percent: 1-phenyl-3-methyl-5-pyrazolone 30 ~ 40 parts, 5,8-dihydroxy-1,4-naphthoquinones 20 ~ 30 parts, 1-(4-sulfonic group phenyl)-3-carboxyl-5-pyrazolone 20 ~ 30 parts, sodium lauroyl sarcosine 5 ~ 8 parts, sorbitan monostearate 4 ~ 7 parts, polyglyceryl fatty acid ester 2 ~ 5 parts, colouring stabilizer IFI-85112 ~ 4 part, polyvinyl alcohol (PVA) 3 ~ 6 parts, component A35 ~ 45 part shown in microcrystalline cellulose 2 ~ 5 parts He formula (I):
(I);
Described component A prepares according to following steps:
1. 4,4'-(phenylimino is taken) biphenol is dissolved in organic solvent, obtains solution; 4,4'-(phenylimino) mol ratio of biphenol and organic solvent is 1:10 ~ 1:100; Described organic solvent is methyl alcohol or ethanol;
2. take highly basic and be dissolved in the solution that 1. step obtain, add 1-ethinyl-4-fluorobenzene wherein, obtain reactant liquor a; Described highly basic is NaOH or potassium hydroxide; Highly basic and step 1. in 4,4'-(phenyliminos) mol ratio of biphenol is 3 ~ 5:1; 1-ethinyl-4-fluorobenzene and step 1. in 4,4'-(phenyliminos) mol ratio of biphenol is 1.5 ~ 2:1;
3. by step 2. gained reactant liquor a start stirring start reaction, at 20 ~ 30 DEG C react 5 ~ 10 hours, obtain reactant liquor b, wash three times with distilled water add methylene chloride in reactant liquor b after, standing separatory obtains organic phase and aqueous phase; The volume ratio of reactant liquor b and methylene chloride is 1:3 ~ 5; The volume ratio of three washing distilled water and methylene chloride is 1:2 ~ 3;
4. by step 3. gained organic phase anhydrous sodium sulfate drying, decompression distillation removing organic solvent, obtain crude product, obtain product a:4-(4-ethinyl phenoxy group)-N-(4-(4-ethinyl phenoxy group) phenyl)-N-phenylaniline by re-crystallizing in ethyl acetate;
5. step 4. products therefrom a, cuprous iodide, N is taken, N-bis-diisopropylethylamine and (Z)-3-(4-azido-2,5-bis-(own oxygen base) phenyl)-2-alpha-cyanoacrylate is dissolved in the mixed liquor of methyl alcohol and tetrahydrofuran, and the volume ratio of methyl alcohol and tetrahydrofuran is 1:1; Under nitrogen protection, react 15 ~ 20 hours, obtain filtrate after filtration at 20 ~ 30 DEG C, decompression distillation, except desolventizing, obtains crude product;
6. by step 5. gained crude product re-crystallizing in ethyl acetate obtain sterling component A.
The reaction principle of more than reacting is as follows:
(1) preparation of product a:
;
(2) preparation of dyestuff (I):
The preparation method of above-mentioned redness is high temperature resistant dye composite comprises the following steps:
(1) preparation of component A:
1. 4,4'-(phenylimino is taken) biphenol is dissolved in organic solvent, obtains solution; 4,4'-(phenylimino) mol ratio of biphenol and organic solvent is 1:10 ~ 1:100; Described organic solvent is methyl alcohol or ethanol;
2. take highly basic and be dissolved in the solution that 1. step obtain, add 1-ethinyl-4-fluorobenzene wherein, obtain reactant liquor a; Described highly basic is NaOH or potassium hydroxide; Highly basic and step 1. in 4,4'-(phenyliminos) mol ratio of biphenol is 3 ~ 5:1; 1-ethinyl-4-fluorobenzene and step 1. in 4,4'-(phenyliminos) mol ratio of biphenol is 1.5 ~ 2:1;
3. by step 2. gained reactant liquor a start stirring start reaction, at 20 ~ 30 DEG C react 5 ~ 10 hours, obtain reactant liquor b, wash three times with distilled water add methylene chloride in reactant liquor b after, standing separatory obtains organic phase and aqueous phase; The volume ratio of reactant liquor b and methylene chloride is 1:3 ~ 5; The volume ratio of three washing distilled water and methylene chloride is 1:2 ~ 3;
4. by step 3. gained organic phase anhydrous sodium sulfate drying, decompression distillation removing organic solvent, obtain crude product, obtain product a:4-(4-ethinyl phenoxy group)-N-(4-(4-ethinyl phenoxy group) phenyl)-N-phenylaniline by re-crystallizing in ethyl acetate;
5. step 4. products therefrom a, cuprous iodide, N is taken, N-bis-diisopropylethylamine and (Z)-3-(4-azido-2,5-bis-(own oxygen base) phenyl)-2-alpha-cyanoacrylate is dissolved in the mixed liquor of methyl alcohol and tetrahydrofuran, and the volume ratio of methyl alcohol and tetrahydrofuran is 1:1; Under nitrogen protection, react 15 ~ 20 hours, obtain filtrate after filtration at 20 ~ 30 DEG C, decompression distillation, except desolventizing, obtains crude product;
6. by step 5. gained crude product re-crystallizing in ethyl acetate obtain sterling component A;
(2) preparation of red high temperature resistant dye composite: with parts by weight, by 1-phenyl-3-methyl-5-pyrazolone 30 ~ 40 parts, 5, 8-dihydroxy-1, 4-naphthoquinones 20 ~ 30 parts, 1-(4-sulfonic group phenyl)-3-carboxyl-5-pyrazolone 20 ~ 30 parts, sodium lauroyl sarcosine 5 ~ 8 parts, sorbitan monostearate 4 ~ 7 parts, polyglyceryl fatty acid ester 2 ~ 5 parts, colouring stabilizer IFI-85112 ~ 4 part, polyvinyl alcohol (PVA) 3 ~ 6 parts, microcrystalline cellulose 2 ~ 5 parts and step (1) obtained component A add in the water of 40 ~ 50 parts, open muller, when the particle diameter of mensuration particle is between 1 ~ 2.5 μm, stop grinding, dye solution through grinding is dry on atomizing drying equipment, obtain red high temperature resistant dye composite.
Embodiment 1
A kind of red high temperature resistant dye composite, with parts by weight, comprise following component: 1-phenyl-3-methyl-5-pyrazolone 30 parts, 5,8-dihydroxy-1,4-naphthoquinones 20 parts, 1-(4-sulfonic group phenyl)-3-carboxyl-5-pyrazolone 20 parts, sodium lauroyl sarcosine 5 parts, sorbitan monostearate 4 parts, polyglyceryl fatty acid ester 2 parts, colouring stabilizer IFI-85112 part, polyvinyl alcohol (PVA) 3 ~ 6 parts and microcrystalline cellulose 2 parts.
The preparation method of said components is as follows: above component added in the water of 50 weight portions, open muller, measure the particle diameter of particle 1 μm time, stop grinding, dye solution through grinding is dry on atomizing drying equipment, obtain red high temperature resistant dye composite.
Embodiment 2
A kind of red high temperature resistant dye composite, with parts by weight, comprise following component: 1-phenyl-3-methyl-5-pyrazolone 40 parts, 5,8-dihydroxy-1,4-naphthoquinones 30 parts, 1-(4-sulfonic group phenyl)-3-carboxyl-5-pyrazolone 30 parts, sodium lauroyl sarcosine 8 parts, sorbitan monostearate 7 parts, polyglyceryl fatty acid ester 5 parts, colouring stabilizer IFI-85114 part, polyvinyl alcohol (PVA) 6 parts and microcrystalline cellulose 5 parts.
The preparation method of said components is as follows: above component added in the water of 40 weight portions, open muller, measure the particle diameter of particle 2.5 μm time, stop grinding, dye solution through grinding is dry on atomizing drying equipment, obtain red high temperature resistant dye composite.
Embodiment 3
A kind of red high temperature resistant dye composite, with parts by weight, comprise following component: 1-phenyl-3-methyl-5-pyrazolone 32 parts, 5,8-dihydroxy-1,4-naphthoquinones 26 parts, 1-(4-sulfonic group phenyl)-3-carboxyl-5-pyrazolone 24 parts, sodium lauroyl sarcosine 6 parts, sorbitan monostearate 6 parts, polyglyceryl fatty acid ester 4 parts, colouring stabilizer IFI-85113 part, polyvinyl alcohol (PVA) 5 parts and microcrystalline cellulose 3 parts.
The preparation method of said components is as follows: above component added in the water of 45 weight portions, open muller, measure the particle diameter of particle 2.0 μm time, stop grinding, dye solution through grinding is dry on atomizing drying equipment, obtain red high temperature resistant dye composite.
Embodiment 4
A kind of red high temperature resistant dye composite, with parts by weight, comprises following component: 1-phenyl-3-methyl-5-pyrazolone 30 parts, 5,8-dihydroxy-1,4-naphthoquinone 20 parts, 1-(4-sulfonic group phenyl)-3-carboxyl-5-pyrazolone 20 parts, sodium lauroyl sarcosine 5 parts, sorbitan monostearate 4 parts, polyglyceryl fatty acid ester 2 parts, colouring stabilizer IFI-85112 part, polyvinyl alcohol (PVA) 3 ~ 6 parts, microcrystalline cellulose 2 parts and component A35 part.
The preparation of component A comprises the following steps:
1. 2.77g(0.01mol is taken) 4,4'-(phenyliminos) biphenol is dissolved in 30ml methyl alcohol, obtains solution;
2. 1.20g(0.03mol is taken) NaOH is dissolved in the solution that 1. step obtains, and adds 1-ethinyl-4-fluorobenzene 1.80g(0.015mol wherein), obtain reactant liquor a;
3. by step 2. gained reactant liquor a start stirring start reaction, at 30 DEG C react 5 hours, obtain reactant liquor b, wash three times with 45ml distilled water add 90ml methylene chloride in reactant liquor b after, standing separatory obtains organic phase and aqueous phase;
4. by step 3. gained organic phase anhydrous sodium sulfate drying, decompression distillation removing organic solvent, obtain crude product, obtain 3.34g product a:4-(4-ethinyl phenoxy group)-N-(4-(4-ethinyl phenoxy group) phenyl)-N-phenylaniline by re-crystallizing in ethyl acetate;
5. 2.38g (0.005mol) step 4. products therefrom a, 2.85g (0.015mol) cuprous iodide, 3.22g (0.025mol) N is taken, N-bis-diisopropylethylamine and 4.14g (0.010mol) (Z)-3-(4-azido-2,5-bis-(own oxygen base) phenyl)-2-alpha-cyanoacrylate is dissolved in the methyl alcohol and tetrahydrofuran mixed liquor that 100ml volume ratio is 1:1, under nitrogen protection, react 20 hours at 30 DEG C, filtrate is obtained after filtration, decompression distillation, except desolventizing, obtains crude product;
6. by step 5. gained crude product re-crystallizing in ethyl acetate obtain 3.90g sterling component A, productive rate is 60%.
The detection data of product a:4-(4-ethinyl phenoxy group)-N-(4-(4-ethinyl phenoxy group) phenyl)-N-phenylaniline are as follows:
Ultimate analysis: C
34h
23nO
2: %C85.51(85.40); %H4.85(4.87); %N2.93(2.97); Be %O6.70(6.65) measured value in bracket;
Mass spectrophotometry: MS(ESP) m/z:478.04(M);
The detection data of the dyestuff of structural formula (I) are as follows:
1HNMR(500MHz,d-DMSO)δ:11.00(s,3H),8.22(s,3H),8.08(s,2H),7.62(d,J=6.5Hz,4H),7.20(m,6H),6.90-6.79(m,9H),6.63-6.59(m,6H),4.06(t,J=8.0Hz,8H),1.43-1.29(m,24H),0.88(t,J=8.5Hz,12H);
Ultimate analysis: C
78h
83n
9o
10: %C71.70(71.55); %H6.40(6.41); %N9.65(9.72); Be %O12.25(12.23) measured value in bracket;
Mass spectrophotometry: MS(ESP) m/z:1306.24(M).
The component of high temperature resistant for redness dye composite is added in the water of 40 ~ 50 weight portions, open muller, when the particle diameter of mensuration particle is between 1 ~ 2.5 μm, stop grinding, dye solution through grinding is dry on atomizing drying equipment, obtain red high temperature resistant dye composite.
Embodiment 5
A kind of red high temperature resistant dye composite, with parts by weight, comprises following component: 1-phenyl-3-methyl-5-pyrazolone 40 parts, 5,8-dihydroxy-1,4-naphthoquinone 30 parts, 1-(4-sulfonic group phenyl)-3-carboxyl-5-pyrazolone 30 parts, sodium lauroyl sarcosine 8 parts, sorbitan monostearate 7 parts, polyglyceryl fatty acid ester 5 parts, colouring stabilizer IFI-85114 part, polyvinyl alcohol (PVA) 6 parts, microcrystalline cellulose 5 parts and component A45 part.
The preparation of component A comprises the following steps:
1. 2.77g(0.01mol is taken) 4,4'-(phenyliminos) biphenol is dissolved in 30ml methyl alcohol, obtains solution;
2. 2.80g(0.05mol is taken) potassium hydroxide is dissolved in the solution that 1. step obtains, and adds 1-ethinyl-4-fluorobenzene 2.40g(0.02mol wherein), obtain reactant liquor a;
3. by step 2. gained reactant liquor a start stirring start reaction, at 20 DEG C react 5 hours, obtain reactant liquor b, wash three times with 50ml distilled water add 150ml methylene chloride in reactant liquor b after, standing separatory obtains organic phase and aqueous phase;
4. by step 3. gained organic phase anhydrous sodium sulfate drying, decompression distillation removing organic solvent, obtain crude product, obtain 3.40g product a:4-(4-ethinyl phenoxy group)-N-(4-(4-ethinyl phenoxy group) phenyl)-N-phenylaniline by re-crystallizing in ethyl acetate;
5. 2.38g (0.005mol) step 4. products therefrom a, 3.80g (0.020mol) cuprous iodide, 2.58g (0.020mol) N is taken, N-bis-diisopropylethylamine and 6.21g (0.015mol) (Z)-3-(4-azido-2,5-bis-(own oxygen base) phenyl)-2-alpha-cyanoacrylate is dissolved in the methyl alcohol and tetrahydrofuran mixed liquor that 150ml volume ratio is 1:1, under nitrogen protection, react 15 hours at 20 DEG C, filtrate is obtained after filtration, decompression distillation, except desolventizing, obtains crude product;
6. by step 5. gained crude product re-crystallizing in ethyl acetate obtain 3.95g sterling component A, productive rate is 65%.
Characterization of compound data are shown in embodiment 4.
The component of high temperature resistant for redness dye composite is added in the water of 40 ~ 50 weight portions, open muller, when the particle diameter of mensuration particle is between 1 ~ 2.5 μm, stop grinding, dye solution through grinding is dry on atomizing drying equipment, obtain red high temperature resistant dye composite.
Embodiment 6
A kind of red high temperature resistant dye composite, with parts by weight, comprises following component: 1-phenyl-3-methyl-5-pyrazolone 32 parts, 5,8-dihydroxy-1,4-naphthoquinone 26 parts, 1-(4-sulfonic group phenyl)-3-carboxyl-5-pyrazolone 24 parts, sodium lauroyl sarcosine 6 parts, sorbitan monostearate 6 parts, polyglyceryl fatty acid ester 4 parts, colouring stabilizer IFI-85113 part, polyvinyl alcohol (PVA) 5 parts, microcrystalline cellulose 3 parts and component A42 part.
The preparation of component A comprises the following steps:
1. 2.77g(0.01mol is taken) 4,4'-(phenyliminos) biphenol is dissolved in 50ml methyl alcohol, obtains solution;
2. 2.24g(0.04mol is taken) potassium hydroxide is dissolved in the solution that 1. step obtains, and adds 1-ethinyl-4-fluorobenzene 2.16g(0.018mol wherein), obtain reactant liquor a;
3. by step 2. gained reactant liquor a start stirring start reaction, at 25 DEG C react 6 hours, obtain reactant liquor b, wash three times with 100ml distilled water add 200ml methylene chloride in reactant liquor b after, standing separatory obtains organic phase and aqueous phase;
4. by step 3. gained organic phase anhydrous sodium sulfate drying, decompression distillation removing organic solvent, obtain crude product, obtain 3.81g product a:4-(4-ethinyl phenoxy group)-N-(4-(4-ethinyl phenoxy group) phenyl)-N-phenylaniline by re-crystallizing in ethyl acetate;
5. 2.38g (0.005mol) step 4. products therefrom a, 4.75g (0.025mol) cuprous iodide, 2.58g (0.020mol) N is taken, N-bis-diisopropylethylamine and 4.14g (0.010mol) (Z)-3-(4-azido-2,5-bis-(own oxygen base) phenyl)-2-alpha-cyanoacrylate is dissolved in the methyl alcohol and tetrahydrofuran mixed liquor that 150ml volume ratio is 1:1, under nitrogen protection, react 18 hours at 25 DEG C, filtrate is obtained after filtration, decompression distillation, except desolventizing, obtains crude product;
6. by step 5. gained crude product re-crystallizing in ethyl acetate obtain 4.28g sterling component A, productive rate is 68%.
Characterization of compound data are shown in embodiment 4.
The component of high temperature resistant for redness dye composite is added in the water of 40 ~ 50 weight portions, open muller, when the particle diameter of mensuration particle is between 1 ~ 2.5 μm, stop grinding, dye solution through grinding is dry on atomizing drying equipment, obtain red high temperature resistant dye composite.
Embodiment 7
With parts by weight, be made up of following component: 1-phenyl-3-methyl-5-pyrazolone 34 parts, 5,8-dihydroxy-1,4-naphthoquinones 26 parts, 1-(4-sulfonic group phenyl)-3-carboxyl-5-pyrazolone 22 parts, sodium lauroyl sarcosine 6 parts, sorbitan monostearate 5 parts, polyglyceryl fatty acid ester 4 parts, colouring stabilizer IFI-85113 part, polyvinyl alcohol (PVA) 5 parts, microcrystalline cellulose 3 parts and component A40 part.
The component of high temperature resistant for redness dye composite is added in the water of 40 ~ 50 weight portions, open muller, when the particle diameter of mensuration particle is between 1 ~ 2.5 μm, stop grinding, dye solution through grinding is dry on atomizing drying equipment, obtain red high temperature resistant dye composite.
The colouring method of the red high temperature resistant dye composite of the present invention is as follows: join in 200ml water respectively by the high temperature resistant dye composite of redness of 0.1g embodiment 1,2,3,5,6 and 7 gained, after dyestuff is dissolved completely, pH is adjusted to be 5 ~ 6 with acetic acid, be warming up to 50 DEG C, add 5g diablement fort and dye, insulation 15min, then 130 DEG C of insulation 45min are slowly warming up to, take out dyed fabric after cooling, soap, wash, dry, obtain red dyeing and weaving thing.
Carry out composite performance test to the red dyeing and weaving thing of above-mentioned gained, adopt GB/T7069-1997, GB/T6152-1997, GB/T3920-1997, GB/T8427-1998, GB/T5718-1997 to measure every fastness, testing result is as shown in table 1.
The composite performance testing result of the red dyeing and weaving thing of table 1
|
Fastness to chlorine-bleaching |
Color fastness to hot pressing |
Rub resistance |
Fast light |
Sublimation reliability (180 DEG C) |
Embodiment 1 |
4 grades |
4 ~ 5 grades |
5 grades |
>=6 grades |
5 grades |
Embodiment 2 |
4 grades |
4 ~ 5 grades |
5 grades |
>=6 grades |
5 grades |
Embodiment 3 |
4 grades |
4 ~ 5 grades |
5 grades |
>=6 grades |
5 grades |
Embodiment 5 |
4 grades |
5 grades |
5 grades |
>=6 grades |
5 grades |
Embodiment 6 |
4 grades |
5 grades |
5 grades |
>=6 grades |
5 grades |
Embodiment 7 |
4 grades |
5 grades |
5 grades |
>=6 grades |
5 grades |
Technical scheme of the present invention is not restricted in the scope of embodiment of the present invention.The technology contents of the not detailed description of the present invention is known technology.