CN107699643B - A kind of fire-retardant and light resistance phosphorylation fatting agent - Google Patents
A kind of fire-retardant and light resistance phosphorylation fatting agent Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C14—SKINS; HIDES; PELTS; LEATHER
- C14C—CHEMICAL TREATMENT OF HIDES, SKINS OR LEATHER, e.g. TANNING, IMPREGNATING, FINISHING; APPARATUS THEREFOR; COMPOSITIONS FOR TANNING
- C14C9/00—Impregnating leather for preserving, waterproofing, making resistant to heat or similar purposes
- C14C9/02—Impregnating leather for preserving, waterproofing, making resistant to heat or similar purposes using fatty or oily materials, e.g. fat liquoring
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Abstract
The invention discloses a kind of fire-retardant and light resistance phosphorylation fatting agents and preparation method thereof, phosphorus pentoxide, castor oil are proportionally added into reaction vessel, after mixing evenly, it is added into container and phosphorus pentoxide dispersion liquid prepared by above-mentioned (1), castor oil is added in 250ml there-necked flask, after mixing evenly, catalyst is added into container, is warming up to 70 DEG C, it is condensed back insulation reaction 1h, obtains product C；Choline chloride 2.5g is added into product C, it is warming up to 80 DEG C after mixing evenly, insulation reaction 1h, add D-sorbite 2.5g, eight amine molybdate 1.5g, cyanuric acid 2.5g, oleamide 1.1g and 1- (3- DimethylAminopropyl) -3- ethyl carbodiimide 1.2g, it is warming up to 60 DEG C, it is stirred to react 2h, obtains product D；Sodium hydroxide solution is added dropwise into product D again to neutrality, obtains brown color liquid, the as described fire-retardant and light resistance phosphorylation fatting agent.Prepared fatting agent had not only kept the organoleptic properties and mechanical strength of traditional fatting agent, but also had good flame resistance and light resistance.
Description
It is fire-retardant with light resistance phosphorylation fatting agent that the application is that application No. is 201610653716.0 entitled one kind
Preparation method patent application divisional application.
Technical field
The present invention relates to a kind of preparation methods of phosphorylation fatting agent, are related specifically to fire-retardant and light resistance phosphorylation stuffing
The preparation method of agent.
Background technique
As the improvement of people's living standards, furniture leather and automobile leather etc. are also in the gesture of growth increasingly.At the same time, by
Fire caused by leather, synthetic leather is also being constantly increasing.The thus fire-retardant problem of leather, becomes an industry research hot spot.
In leather processing procedure, stuffing is an essential procedure, organoleptic properties, mechanics to leather and fur products
Performance influence is very big, but fatting agent used in stuffing at present is easy burning, therefore, it is necessary to be modified to fatting agent, drop
Its low combustibility, improves its flame resistance, to meet the needs of market is to flame-retardant leather product.
In recent ten years, phosphorylation fatting agent becomes the exploitation hot spot of leather fat.Since this kind of fatting agent contains phosphorus
Acid group can be complexed with chromic salts.Therefore, chromic salts can be made to be more evenly distributed in leather in chrome tanning or chrome retanned, and they and energy
In conjunction with fiber, there is permanent stuffing effect.In addition, phosphorylation fatting agent good penetrability, has filling effect to leather, have leather
The surface non-greasy for having a waterproofness, and removing from office, does not turn yellow and free from extraneous odour, is more suitable for the stuffing of white, colored soft leather, high-grade leather, at
Leather has special soft feeling, and leather body is plentiful, and elasticity is good.Thus, phosphorylation fatting agent is modified, its anti-flammability is improved
Can, become the project that industry experts and scholars fall over each other research.
Due to preparing the common phosphorylation agent of phosphorylation fatting agent: the active height of phosphorus pentoxide, reaction rate is fast,
But have the defects that be difficult to be added system, with agglomeration, it is therefore desirable to disperse phosphorus pentoxide.
Acid catalysis is one of most universal, most important reaction in organic synthesis.Traditional liquid acid (such as sulfuric acid, nitric acid)
Though catalytic activity is high, there are serious environmental pollution and safety problems；Though solid acid is environmental-friendly, acid activity center is uneven
Even and effective active centric quantity is few.Acidic functionalized ionic liquid is because of the characteristics of having solid acid and liquid acid concurrently, non-volatility
It is low with corrosivity, very big potentiality are shown in terms of environmental-friendly acid catalysis.
Summary of the invention
The present invention is intended to provide a kind of fire-retardant preparation method with light resistance phosphorylation fatting agent, by by phosphorus pentoxide
It is scattered in liquid, phosphorylation castor oil fatting agent is modified, and with aluminium isopropoxide, 2- hydroxyl -1- naphthoic acid, peroxidating
Double benzoyls, propionic acid aluminium, dihydroxy morphinan-6-ones hydrochloride make the catalyst of fatting agent synthesis, and simultaneous selection selects 2- hydroxyl
Ethyl-trimethyl salmiac, D-sorbite, eight amine molybdates, cyanuric acid, naringin, guanidine hydrochloride, para toluene sulfonamide improve phosphorus
It is acidified the flame retardant type of castor oil fatting agent, 1- (3- DimethylAminopropyl) -3- ethyl carbodiimide, naringin, glutamine, second
Phenoxyl quinoline, beet alkali hydrochlorate, triethylene tetramine, thio-tepa improve the light resistance of phosphorylation castor oil；
The invention adopts the following technical scheme:
1. a kind of fire-retardant preparation method with light resistance phosphorylation fatting agent, it is characterised in that:
(1) preparation of phosphorus pentoxide dispersion liquid: by phosphorus pentoxide 35g, 1- cetyl -3- methylimidazole fluoroform
Sulfonate 50g and diethyl malonate 3g are added in 250ml there-necked flask, are reacted 1h in 70 DEG C of mixings, are obtained five oxygen
Change two phosphorus dispersion liquids；
(2) phosphorus pentoxide dispersion liquid 8g, castor oil 42g prepared by above-mentioned (1) are added in 250ml there-necked flask,
After mixing evenly, aluminium isopropoxide 2g, 2- hydroxyl -1- naphthoic acid 1.2g are added into container, is warming up to 70 DEG C, is condensed back and protects
Temperature reaction 1h, obtains product C；
(3) choline chloride 2.5g is added into product C, is warming up to 80 DEG C after mixing evenly, heat preservation is anti-
1h is answered, D-sorbite 2.5g, eight amine molybdate 1.5g, cyanuric acid 2.5g, oleamide 1.1g and 1- (3- dimethyl are added
Amine propyl) -3- ethyl carbodiimide 1.2g, 60 DEG C are warming up to, 2h is stirred to react, obtains product D；
(4) the sodium hydroxide solution 12ml of mass concentration 10% is added dropwise into product D again to neutrality, obtains brown color liquid,
The as described fire-retardant and light resistance phosphorylation fatting agent.
2. a kind of fire-retardant preparation method with light resistance phosphorylation fatting agent, it is characterised in that:
(1) preparation of phosphorus pentoxide dispersion liquid: by phosphorus pentoxide 25g, 1- butyl -3- methyl imidazolium tetrafluoroborate
54g and butyl sulfochlorides 3g are added in 250ml there-necked flask, are reacted 2h in 40 DEG C of mixings, are obtained phosphorus pentoxide dispersion
Liquid；
(2) phosphorus pentoxide dispersion liquid 42g, castor oil 56g and diethyl malonate 21g prepared by above-mentioned (1) are added
Enter into 250ml there-necked flask, after mixing evenly, Di benzoyl peroxide paste 1.7g and propionic acid aluminium 1.2g, heating is added into container
To 75 DEG C, it is condensed back insulation reaction 2h, obtains product C；
(3) naringin 7g is added into product C, is warming up to 80 DEG C after mixing evenly, insulation reaction 2h adds sorbose
Alcohol 1.2g, eight amine molybdate 0.5g, guanidine hydrochloride 2.5g, para toluene sulfonamide 1.2g and glutamine 1.1g, be warming up to 70 DEG C, stir
Reaction 3h is mixed, product D is obtained；
(4) the sodium hydroxide solution 10ml of mass concentration 15% is added dropwise into product D again to neutrality, obtains brown color liquid,
The as anti-flammability phosphorylation fatting agent.
3. a kind of fire-retardant preparation method with light resistance phosphorylation fatting agent, it is characterised in that:
(1) preparation of phosphorus pentoxide dispersion liquid: by phosphorus pentoxide 32g, dimethylformamide 54g and epoxychloropropane
5g is added in 250ml there-necked flask, is reacted 1h in 50 DEG C of mixings, is obtained the preparation of phosphorus pentoxide dispersion liquid；
(2) the phosphorus pentoxide dispersion liquid 22g, castor oil 70g of above-mentioned (1) preparation and dimethylformamide 20g are added
Into 250ml there-necked flask, after mixing evenly, 2- hydroxyl -1- naphthoic acid 2g is added into container, is warming up to 68 DEG C, be condensed back
Insulation reaction 1h obtains product C；
(3) trimethylolpropane 2g is added into product C, is warming up to 70 DEG C after mixing evenly, insulation reaction 3h is added
Diethyl hypo-aluminum orthophosphate 1.2g, eight amine molybdate 1.5g, ethoxyquinoline 1.8g, beet alkali hydrochlorate 1.2g, are warming up to 70 DEG C,
It is stirred to react 2.5h, obtains product D；
(4) again into product D be added dropwise mass concentration 15% sodium hydroxide solution 10ml to pH value be neutrality, obtain palm fibre
Yellow liquid, the as described fire-retardant and light resistance phosphorylation fatting agent.
4. a kind of preparation method of anti-flammability phosphorylation fatting agent, it is characterised in that:
(1) preparation of phosphorus pentoxide dispersion liquid: by phosphorus pentoxide 20g, nitric acid ethyl ammonium 86g and epoxychloropropane 6g
It is added in 250ml there-necked flask with 4- vinyl epoxy cyclohexane 2.2g, reacts 1h in 50 DEG C of mixings, obtain five oxidations
Two phosphorus dispersion liquids；
(2) by phosphorus pentoxide dispersion liquid 30g prepared by above-mentioned (1), castor oil 50g and 3,4- epoxy tetrahydrofuran
20g is added in 250ml there-necked flask, after mixing evenly, dihydroxy morphinan-6-ones hydrochloride 1.7g is summed it up into container, risen
Temperature is condensed back insulation reaction 3h, obtains product C to 75 DEG C；
(3) trimethylol melamine 8g is added into product C, is warming up to 60 DEG C, insulation reaction 2h after mixing evenly, then
Diethyl hypo-aluminum orthophosphate 1.5g, eight amine molybdate 0.5g, triethylene tetramine 1.3g and thio-tepa 2.3g is added, is warming up to 70 DEG C, stirs
Reaction 3h is mixed, product D is obtained；
(4) again into product D be added dropwise mass concentration 15% sodium hydroxide solution 12ml to pH value be neutrality, obtain palm fibre
Yellow liquid, as the anti-flammability phosphorylation fatting agent.
The beneficial effects of the present invention are:
(1) phosphorylation fatting agent flame retardant property prepared by the method for the present invention is greatly improved, and maintains traditional phosphorylation
Nearly all advantage of castor oil；
(2) raw material used by the method for the present invention preparation anti-flammability phosphorylation fatting agent, it is cheap, it is from a wealth of sources,
While increasing substantially phosphorylation fatting agent anti-flammability, production cost is effectively controlled, is suitble to promote and apply；
(3) using dispersion 1- cetyl -3- methylimidazole fluoroform sulphonate, diethyl malonate, 1- butyl -3- first
Base tetrafluoroborate disperses phosphorus pentoxide, improves in traditional phosphorus pentoxide addition system that heat release is too fast, is not easy point
It dissipates and causes localized heat release too many, make unstable product quality, while greatly improving the too slow defect of solid charging, butyl
Sulfonic acid chloride, 4 vinyl epoxy cyclohexane are to 1- cetyl -3- methylimidazole fluoroform sulphonate, diethyl malonate, 1-
Butyl -3- methyl imidazolium tetrafluoroborate carries out synergy, improves dispersion of the above-mentioned substance to phosphorus pentoxide；
(4) aluminium isopropoxide, 2- hydroxyl -1- naphthoic acid, Di benzoyl peroxide paste, propionic acid aluminium, dihydroxy morphinan-6-ones salt
Hydrochlorate makees catalyst, reduces traditional inorganic acid to the corrosivity of equipment；
(5) select choline chloride, D-sorbite, eight amine molybdates, cyanuric acid, naringin, hydrochloric acid
Guanidine, para toluene sulfonamide improve the anti-flammability of phosphorylation castor oil fatting agent；
(6) 1- (3- DimethylAminopropyl) -3- ethyl carbodiimide, naringin, glutamine, ethoxyquinoline, beet
Alkali salt hydrochlorate, triethylene tetramine, thio-tepa improve the light resistance of phosphorylation castor oil；
(7) oleamide, toluenesulfonamide increase choline chloride, D-sorbite, eight amine molybdates, three
The flame retarding efficiency of paracyanogen acid, guanidine hydrochloride, is equivalent to fire retarding synergist.
Specific embodiment
In order to better understand and implement the present invention, the present invention is further illustrated combined with specific embodiments below.
Example 1
(1) preparation of phosphorus pentoxide dispersion liquid: by phosphorus pentoxide 35g, 1- cetyl -3- methylimidazole fluoroform
Sulfonate 50g and diethyl malonate 3g are added in 250ml there-necked flask, are reacted 1h in 70 DEG C of mixings, are obtained five oxygen
Change two phosphorus dispersion liquids；
(2) phosphorus pentoxide dispersion liquid 8g, castor oil 42g prepared by above-mentioned (1) are added in 250ml there-necked flask,
After mixing evenly, aluminium isopropoxide 2g, 2- hydroxyl -1- naphthoic acid 1.2g are added into container, is warming up to 70 DEG C, is condensed back and protects
Temperature reaction 1h, obtains product C；
(3) choline chloride 2.5g is added into product C, is warming up to 80 DEG C after mixing evenly, heat preservation is anti-
1h is answered, D-sorbite 2.5g, eight amine molybdate 1.5g, cyanuric acid 2.5g, oleamide 1.1g and 1- (3- dimethyl are added
Amine propyl) -3- ethyl carbodiimide 1.2g, 60 DEG C are warming up to, 2h is stirred to react, obtains product D；
(4) the sodium hydroxide solution 12ml of mass concentration 10% is added dropwise into product D again to neutrality, obtains brown color liquid,
The as described fire-retardant and light resistance phosphorylation fatting agent.
Example 2
(1) preparation of phosphorus pentoxide dispersion liquid: by phosphorus pentoxide 25g, 1- butyl -3- methyl imidazolium tetrafluoroborate
54g and butyl sulfochlorides 3g are added in 250ml there-necked flask, are reacted 2h in 40 DEG C of mixings, are obtained phosphorus pentoxide dispersion
Liquid；
(2) phosphorus pentoxide dispersion liquid 42g, castor oil 56g and diethyl malonate 21g prepared by above-mentioned (1) are added
Enter into 250ml there-necked flask, after mixing evenly, Di benzoyl peroxide paste 1.7g and propionic acid aluminium 1.2g, heating is added into container
To 75 DEG C, it is condensed back insulation reaction 2h, obtains product C；
(3) naringin 7g is added into product C, is warming up to 80 DEG C after mixing evenly, insulation reaction 2h adds sorbose
Alcohol 1.2g, eight amine molybdate 0.5g, guanidine hydrochloride 2.5g, para toluene sulfonamide 1.2g and glutamine 1.1g, be warming up to 70 DEG C, stir
Reaction 3h is mixed, product D is obtained；
(4) the sodium hydroxide solution 10ml of mass concentration 15% is added dropwise into product D again to neutrality, obtains brown color liquid,
The as anti-flammability phosphorylation fatting agent.
Example 3
(1) preparation of phosphorus pentoxide dispersion liquid: by phosphorus pentoxide 32g, dimethylformamide 54g and epoxychloropropane
5g is added in 250ml there-necked flask, is reacted 1h in 50 DEG C of mixings, is obtained the preparation of phosphorus pentoxide dispersion liquid；
(2) the phosphorus pentoxide dispersion liquid 22g, castor oil 70g of above-mentioned (1) preparation and dimethylformamide 20g are added
Into 250ml there-necked flask, after mixing evenly, 2- hydroxyl -1- naphthoic acid 2g is added into container, is warming up to 68 DEG C, be condensed back
Insulation reaction 1h obtains product C；
(3) trimethylolpropane 2g is added into product C, is warming up to 70 DEG C after mixing evenly, insulation reaction 3h is added
Diethyl hypo-aluminum orthophosphate 1.2g, eight amine molybdate 1.5g, ethoxyquinoline 1.8g, beet alkali hydrochlorate 1.2g, are warming up to 70 DEG C,
It is stirred to react 2.5h, obtains product D；
(4) again into product D be added dropwise mass concentration 15% sodium hydroxide solution 10ml to pH value be neutrality, obtain palm fibre
Yellow liquid, the as described fire-retardant and light resistance phosphorylation fatting agent.
Example 4
(1) preparation of phosphorus pentoxide dispersion liquid: by phosphorus pentoxide 20g, nitric acid ethyl ammonium 86g and epoxychloropropane 6g
It is added in 250ml there-necked flask with 4- vinyl epoxy cyclohexane 2.2g, reacts 1h in 50 DEG C of mixings, obtain five oxidations
Two phosphorus dispersion liquids；
(2) by phosphorus pentoxide dispersion liquid 30g prepared by above-mentioned (1), castor oil 50g and 3,4- epoxy tetrahydrofuran
20g is added in 250ml there-necked flask, after mixing evenly, 2- hydroxyl -1- naphthoic acid 1.2g and dihydroxy morphine is added into container
Mutter -6- keto hydrochloride 1.7g, is warming up to 75 DEG C, is condensed back insulation reaction 3h, obtains product C；
(3) trimethylol melamine 8g is added into product C, is warming up to 60 DEG C, insulation reaction 2h after mixing evenly, then
Diethyl hypo-aluminum orthophosphate 1.5g, eight amine molybdate 0.5g, triethylene tetramine 1.3g and thio-tepa 2.3g is added, is warming up to 70 DEG C, stirs
Reaction 3h is mixed, product D is obtained；
(4) again into product D be added dropwise mass concentration 15% sodium hydroxide solution 12ml to pH value be neutrality, obtain palm fibre
Yellow liquid, as the anti-flammability phosphorylation fatting agent.
Beneficial effects of the present invention are further illustrated below by experimental data:
Experimental index and bibliography: the anti-flammability of leather is that (maximum smoke density, to reach most opium close by smoke density method
Spend the time) (GB8323-2008, Plastics Combustion method for testing performance-smoke density method [S]), oxygen index (OI) (GB/T5454-1997,
Textile combustion performance test-oxygen index method [S]), vertical combustion index (flaming combustion time, glowing time) (GB/T
5455- 1997, textile combustion can test-normal beam technique [S]) Lai Hengliang, the sense organ of leather is by feel, fullness, flexibility
Measure, wherein feel, fullness, flexibility are divided into three ranks, by it is excellent to bad be successively denoted as, preferably, it is poor (Duan Baorong,
The synthesis of the new fire-retardant retanning agent of property amino resins of Wang Quanjie, Wu Ping Tian and application [J] Chinese leather, 2008, (5): 26-30).
Elongation at break refers to (Jiang Weiqi leather finish physical and chemical inspection [M] China Light Industry Press, 1999,82-96).
Table 1 is fire-retardant to be applied to stuffing gained leather organoleptic indicator in the process with light resistance phosphorylation fatting agent
| Type | Example 1 | Example 2 | Example 3 | Example 4 | Not plus fatting agent |
| Feel | Preferably | Preferably | It is good | Preferably | Preferably |
| Fullness | Preferably | It is good | Preferably | Preferably | Difference |
| Flexibility | Preferably | Preferably | It is good | It is good | Difference |
After having used anti-flammability phosphorylation fatting agent of the present invention it can be seen from the experimental data of table 1, leather organoleptic properties
Improved.
Table 2 is fire-retardant to be applied to elongation at break obtained by leather with light resistance phosphorylation fatting agent
| Type | Example 1 | Example 2 | Example 3 | Example 4 | Not plus fatting agent |
| Elongation at break/% | 88.16 | 139.67 | 126.28 | 163.69 | 76.21 |
Anti-flammability phosphorylation fatting agent of the present invention is used it can be seen from 2 experimental data of table, leather elongation at break obtains
To being obviously improved.
The fire-retardant flame retardant effect index for being applied to leather with light resistance phosphorylation fatting agent of table 3
| Example 1 | Example 2 | Example 3 | Example 4 | Not plus fatting agent | |
| Maximum smoke density | 22 | 13 | 7 | 3 | 38 |
| Reach maximum smoke density time/s | 120 | 150 | 180 | 180 | 91 |
| Oxygen index (OI)/% | 27.4 | 28.1 | 30.8 | 31.4 | 25.2 |
| Flaming combustion time/s | 16.3 | 10.4 | 11.3 | 2.7 | 18.6 |
| Glowing time/s | 0.6 | 2.0 | 0.3 | 2.7 | 6.8 |
Seen from table 3, after having used anti-flammability phosphorylation fatting agent of the present invention, maximum smoke density is significantly reduced, and is reached most
Opium density hours significantly extend, and oxygen index (OI) significantly improves, and burning time is obviously shortened.
For the light fastness of quantitative description fatting agent, the light resistance of fatting agent is used for the light resistance of leather with it to weigh
Amount, is detected using spectrophotometer, to obtain inverse difference △ E, to describe the light resistance of leather.△ E represents color
Variation degree, △ E is bigger, and color change is more obvious.In general, △ E value is 0~1.5 category slight change；△ E value be 1.5~
3.0 categories can feel variation；△ E value is that (referring to Wang Fang, Dang Gaochao, Wang Liqin, several organic historical relics are protected for 3.0~6.0 category significant changes
Protect light degradation [J] the Northwest University journal of polymer coating, 2005,35 (5): 56 ~ 58).
The fire-retardant fast light effectiveness indicator for being applied to leather with light resistance phosphorylation fatting agent of table 4
| Time/s | Example 1 | Example 2 | Example 3 | Example 4 | Not plus fatting agent |
| 90 | 0.3 | 0.2 | 0.5 | 0.1 | 0.5 |
| 150 | 0.3 | 0.2 | 0.5 | 0.2 | 0.5 |
| 270 | 0.4 | 0.3 | 0.5 | 0.3 | 0.6 |
| 330 | 0.7 | 0.6 | 0.5 | 0.5 | 0.6 |
| 390 | 0.9 | 0.7 | 0.7 | 0.5 | 0.7 |
| 450 | 0.9 | 0.8 | 0.8 | 0.6 | 0.8 |
| 510 | 1.2 | 1.2 | 0.9 | 0.7 | 1.5 |
| 540 | 1.2 | 1.2 | 1.0 | 1.0 | 1.7 |
| 600 | 1.2 | 1.3 | 1.1 | 1.1 | 1.9 |
Light resistance phosphorylation fatting agent of the present invention is used it can be seen from 4 experimental data of table, light resistance index obtains bright
It is aobvious.
Claims (3)
1. a kind of fire-retardant and light resistance phosphorylation fatting agent, is prepared using following steps, it is characterised in that:
(1) preparation of phosphorus pentoxide dispersion liquid: by phosphorus pentoxide 25g, 1- butyl -3- methyl imidazolium tetrafluoroborate 54g
It is added in 250ml there-necked flask with butyl sulfochlorides 3g, reacts 2h in 40 DEG C of mixings, obtain phosphorus pentoxide dispersion liquid；
(2) phosphorus pentoxide dispersion liquid 42g, castor oil 56g and diethyl malonate 21g prepared by above-mentioned (1) are added to
In 250ml there-necked flask, after mixing evenly, Di benzoyl peroxide paste 1.7g and propionic acid aluminium 1.2g is added into container, is warming up to 75
DEG C, it is condensed back insulation reaction 2h, obtains product C；
(3) naringin 7g is added into product C, is warming up to 80 DEG C after mixing evenly, insulation reaction 2h adds D-sorbite
1.2g, eight amine molybdate 0.5g, guanidine hydrochloride 2.5g, para toluene sulfonamide 1.2g and glutamine 1.1g are warming up to 70 DEG C, and stirring is anti-
3h is answered, product D is obtained；
(4) the sodium hydroxide solution 10ml of mass concentration 15% is added dropwise into product D again to neutrality, obtains brown color liquid, as
The anti-flammability phosphorylation fatting agent.
2. a kind of fire-retardant and light resistance phosphorylation fatting agent, is prepared using following steps, it is characterised in that:
(1) preparation of phosphorus pentoxide dispersion liquid: phosphorus pentoxide 32g, dimethylformamide 54g and epoxychloropropane 5g are added
Enter into 250ml there-necked flask, reacts 1h in 50 DEG C of mixings, obtain the preparation of phosphorus pentoxide dispersion liquid；
(2) phosphorus pentoxide dispersion liquid 22g, castor oil 70g and dimethylformamide 20g prepared by above-mentioned (1) are added to
In 250ml there-necked flask, after mixing evenly, 2- hydroxyl -1- naphthoic acid 2g is added into container, is warming up to 68 DEG C, be condensed back and protect
Temperature reaction 1h, obtains product C；
(3) trimethylolpropane 2g is added into product C, is warming up to 70 DEG C after mixing evenly, insulation reaction 3h adds diethyl
Base hypo-aluminum orthophosphate 1.2g, eight amine molybdate 1.5g, ethoxyquinoline 1.8g, beet alkali hydrochlorate 1.2g are warming up to 70 DEG C, and stirring is anti-
2.5h is answered, product D is obtained；
(4) again into product D be added dropwise mass concentration 15% sodium hydroxide solution 10ml to pH value be neutrality, obtain brown color
Liquid, the as described fire-retardant and light resistance phosphorylation fatting agent.
3. a kind of anti-flammability phosphorylation fatting agent, is prepared using following steps, it is characterised in that:
(1) preparation of phosphorus pentoxide dispersion liquid: by phosphorus pentoxide 20g, nitric acid ethyl ammonium 86g and epoxychloropropane 6g and 4-
Vinyl epoxy cyclohexane 2.2g is added in 250ml there-necked flask, is reacted 1h in 50 DEG C of mixings, is obtained phosphorus pentoxide point
Dispersion liquid；
(2) phosphorus pentoxide dispersion liquid 30g prepared by above-mentioned (1), castor oil 50g and 3,4- epoxy tetrahydrofuran 20g are added
Enter into 250ml there-necked flask, after mixing evenly, 2- hydroxyl -1- naphthoic acid 1.2g and dihydroxy morphinan-6-ones is added into container
Hydrochloride 1.7g is warming up to 75 DEG C, is condensed back insulation reaction 3h, obtains product C；
(3) trimethylol melamine 8g is added into product C, is warming up to 60 DEG C after mixing evenly, insulation reaction 2h is added
Diethyl hypo-aluminum orthophosphate 1.5g, eight amine molybdate 0.5g, triethylene tetramine 1.3g and thio-tepa 2.3g are warming up to 70 DEG C, and stirring is anti-
3h is answered, product D is obtained；
(4) again into product D be added dropwise mass concentration 15% sodium hydroxide solution 12ml to pH value be neutrality, obtain brown color
Liquid, as the anti-flammability phosphorylation fatting agent.
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| CN1451686A (en) * | 2002-04-12 | 2003-10-29 | 日华化学株式会社 | Flame-retardant processing agent, flame-retardant processing method and flame-retardant processed product |
| CN1455808A (en) * | 2001-03-21 | 2003-11-12 | 日华化学株式会社 | Flame retardant treating agent, flame retardant treating process and flame treatment fibers |
| CN104152602A (en) * | 2014-09-01 | 2014-11-19 | 段宝荣 | Preparation method of flame-retardance and light-resistance phosphorylation fatliquor |
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| JP4897649B2 (en) * | 2007-11-02 | 2012-03-14 | 佳裕 徳永 | Manufacturing method of embossed leather material |
| CN104651546A (en) * | 2013-11-21 | 2015-05-27 | 谈丽娜 | Composite-type phosphate leather fatliquor and preparation method thereof |
| CN105002313A (en) * | 2014-04-22 | 2015-10-28 | 中国科学院成都有机化学有限公司 | Preparation method of composite phosphate leather fatliquor without carbon-carbon unsaturated double bonds |
| CN105256084A (en) * | 2014-07-11 | 2016-01-20 | 中国科学院成都有机化学有限公司 | Preparation method for composite type phosphate ester leather fat-liquoring agent of polyurethane containing nonionic structures |
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| CN1455808A (en) * | 2001-03-21 | 2003-11-12 | 日华化学株式会社 | Flame retardant treating agent, flame retardant treating process and flame treatment fibers |
| CN1451686A (en) * | 2002-04-12 | 2003-10-29 | 日华化学株式会社 | Flame-retardant processing agent, flame-retardant processing method and flame-retardant processed product |
| CN104152602A (en) * | 2014-09-01 | 2014-11-19 | 段宝荣 | Preparation method of flame-retardance and light-resistance phosphorylation fatliquor |
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