A kind of textile long acting antibiotic treatment fluid and preparation method thereof
Technical field
The invention belongs to feature field of new materials, and in particular to it is anti-that one kind make it that hair, cotton and blending textile product have
Common germ, suppress resistance venereal bacteria, high-efficient and lasting, at the free from environmental pollution and textile long acting antibiotic that has no side effect to human body
Manage liquid and preparation method thereof.
Background technology
All kinds of hairs, cotton and blending textile product are with the development of the society, frequency of use more and more higher, and species is also increasingly
It is more.But these products do not have bacteria resistance function, are also easy to produce peculiar smell, easily grow or breed various harmful bacterias, mould, virus etc.
Microorganism, turn into a public propagation source, the health care belt to people carrys out larger puzzlement.
In view of above-mentioned factor, in recent years, the antibiotic property scientific research to hair, cotton and blending textile product both at home and abroad gradually increases
More, it is mainly obtained by adding the method for a small amount of antiseptic.Through searching document, current antiseptic is broadly divided into list by structure
One inorganic, organic and natural three big series.
Inorganic antiseptic be using metal ions such as silver, copper, zinc as antiseptic, it is non-with porous, inorganics such as phosphate, bentonites
Metal material is made for carrier, has that heat resistance is strong, but its is expensive, environmental protection shortcoming, product not wash resistant, it is long-term use of and
Touching the product containing metal ions such as silver, copper, zinc can adversely affect to the liver of human body.
Organic antibacterial agent includes quaternary ammonium salts, imidazoles, pyridines, organic metal class etc., although sterilization speed is fast, antibacterial
Significant effect, but drug resistance is also easy to produce, heat endurance is poor, and Durability of antimicrobial effect is short, and toxicity is larger, new so as to bring
Healthy hidden danger.
By comparison, natural antibacterial agent is extracted from plant, animal or biology, and its wide material sources, cost is low, has peace
Atoxic, nutritive and health protection components enrich, the advantages that being not likely to produce drug resistance and be environmentally friendly, therefore its application and research are increasingly
It is valued by people.But natural antibacterial agent is typically to extract to form from a kind of plant, animal or biology, antimicrobial component list
One, antibacterial range is narrow, the problems such as reunion, scattered uneven be present, and antimicrobial component easily separates out in use, and antibacterial effect is not
Can persistently, also easy product germ is to its resistance to the action of a drug, germ such as methicillin-resistant gold of these antiseptics to drug resistance
Yellow staphylococcus are without effect.
The content of the invention
The present invention is directed to above-mentioned technical problem, and it is anti-general that present invention offer one kind make it that hair, cotton and blending textile product have
Common fault bacterium, suppress resistance venereal bacteria, high-efficient and lasting, textile long acting antibiotic that is free from environmental pollution and having no side effect to human body is handled
Liquid and preparation method thereof, the antimicrobial treatment solution use multiple compounds, with hair, cotton and blending textile product it is compound have it is good
Adhesiveness, be added on hair, cotton and blending textile product surface so that hair, cotton and blending textile product have resist common germ,
Suppress resistance venereal bacteria, high-efficient and lasting, play environment purification, eliminate peculiar smell, self-cleaning health care, it is free from environmental pollution and to human body without pair
Effect, more health benefits are obtained beneficial to people.
To achieve these goals, the present invention uses following technical scheme:
One of technical problems to be solved by the invention are to provide a kind of textile long acting antibiotic treatment fluid.
The invention discloses a kind of textile long acting antibiotic treatment fluid, the raw material of the textile long acting antibiotic treatment fluid is matched somebody with somebody
Side is by weight percentage:Deionized water 84-97.5%, Unined RM antiseptic 0.5-3.5%, adhesive 1.5-
11.5%, dispersant 0.25-0.5% and coupling agent 0.25-0.5%.
Preferably, the Unined RM antiseptics are counted including 10-15 parts phenols, 1-3 part isoquercitrins in parts by weight
Glycosides, 2-4 parts N, N- dihydroxyethylglycin, 3-5 parts mercaptopyridine, 5-8 part dodecylbenzyls dimethyl ammonium, 0.3-10
Part dispersant, 0.56-22 parts acrylic acid and the tetrachloro phthalonitrile of 10-15 parts 2,4,5,6-.
The Antibacterial Mechanism of organic antibacterial agent is mainly combined or and mercapto with the anion of pathogenic microorganism cell membrane surface
Base reaction suppresses the breeding of pathogenic microorganism with this so as to destroy the structure of protein or influence the synthesis of biomembrane.Typically
The mechanism of action of organic antibacterial agent is summarized as in fact:1. act on the protease or other biological activity thing needed for biochemical reaction
Matter;2. act on hereditary material DNA or other hereditary particle structures;3. act on biofilm system or cell membrane.
And the present invention is acted on from each material coordinated, pathogenic microorganism of the absorption with negative electrical charge, microorganism is destroyed
Cell membrane mechanism, makes content leak, and can suppress the effect such as pathogen oxidizing ferment, dehydrogenase;Also it can remove pathogenic microorganism film
In lipid material and make protein denaturation;Also pathogenic microorganism mitosis process is may interfere with, suppresses the formation of spindle, shadow
Ring pathogenic microorganism fission process.
Preferably, the phenols is one kind in isopropyl methyl phenol, triclosan, antiphen, clorofene, chloreresol
Or several composition.
Preferably, the preparation method of the Unined RM antiseptics is:
(1) by load weighted phenols, isoquercitrin, N, N- dihydroxyethylglycins, mercaptopyridine, dodecylbenzyl
Dimethyl ammonium and 2,4,5,6- tetrachloro phthalonitriles form uniform suspension in mixed at room temperature;
(2) dispersant is added in the suspension obtained to step (1), 10-12 hours is mixed, then adds acrylic acid, is mixed
2-5 minutes are closed, obtain the Unined RM antiseptics.
Preferably, the dispersant is Sodium Polyacrylate.
In some embodiments of the invention, the dispersant Sodium Polyacrylate uses commercially available Sodium Polyacrylate, i.e. A11
Non-ionic dispersing agent.
In some embodiments of the invention, the preparation process of the dispersant Sodium Polyacrylate is:
By acrylic acid and isopropanol with mass ratio 1:(0.9-1.2) is mixed, and obtains mixed liquor A;By ammonium persulfate and go from
Sub- water is with solid-to-liquid ratio 1:(20-25) (g/mL) is well mixed, obtains mixed liquid B;By n- dodecyl mereaptan, isopropanol and deionized water
With mass ratio 1:(22-25):7 is well mixed, obtains mixed liquor C, wherein n- dodecyl mereaptan, acrylic acid, ammonium persulfate quality
Than for 1:(20-25):1;Mixed liquor C is heated to 80-85 DEG C, while mixed liquor A is added dropwise with 5-8 μ L/s rate of addition and mixed
Close liquid B;After charging, 2.5-3 hours are reacted in 80-85 DEG C;After reaction terminates, reaction solution is cooled to 40-45 DEG C, uses matter
Measure the sodium hydrate aqueous solution that fraction is 25-30% and adjust the pH value of reaction solution to 7-8;Reaction solution is evaporated under reduced pressure, removed
Isopropyl alcohol and water, obtain the dispersant Sodium Polyacrylate.
In some embodiments of the invention, the preparation process of the dispersant Sodium Polyacrylate is:
(1) n- dodecyl mereaptan, the chlorination of methyl trioctylphosphine are added sequentially in reaction vessel by with acetone, described positive 12
Mercaptan, methyl trioctylphosphine chlorination are pressed and the mass ratio of acetone is 1:0.07:(3.2-3.5), nitrogen is passed through, while makes reaction system
Temperature remains 2-5 DEG C, and 2-3 minutes are stirred with 150-200 revs/min of rotating speed;Add the hydrogen-oxygen that mass fraction is 40-50%
The mass ratio of change sodium water solution, sodium hydrate aqueous solution and n- dodecyl mereaptan is (0.4-0.5):1, with 150-200 revs/min
Rotating speed stirs 15-20 minutes;Then the acetone soln for the carbon disulfide that addition mass fraction is 25-30%, the third of carbon disulfide
The mass ratio of ketone solution and n- dodecyl mereaptan is (1.3-1.4):1,5-10 minutes are stirred with 150-200 revs/min of rotating speed;With
Chloroform and mass fraction are added for 40-50% sodium hydrate aqueous solution successively afterwards, chloroform, sodium hydrate aqueous solution and positive ten
The mass ratio that the mass ratio of two mercaptan is is (0.8-0.9):2:1, it is small with 150-200 revs/min of rotating speed stirring reaction 12-18
When;React after terminating, addition deionized water, the mass ratio of deionized water and n- dodecyl mereaptan is (30-40):1, after mixing, add
Enter the hydrochloric acid that mass fraction is 35-37%, the volume ratio of hydrochloric acid and deionized water is 1:(20-25), with 150-200 revs/min
Rotating speed stirring 20-25 minutes;Nitrogen is passed through, removes acetone;Using 80-100 mesh filter-cloth filterings, filter cake is collected;By filter cake in
50-60 DEG C, 8-10 hours are dried under conditions of vacuum 0.06-0.08MPa, obtain the chain-transferring agent;
(2) acrylic acid, initiator A IBN, the tert-butyl alcohol and chain-transferring agent are added in reaction vessel, wherein acrylic acid, initiation
Agent AIBN, the tert-butyl alcohol and chain-transferring agent mass ratio are 1:0.002:(1.8-1.9):0.4, it is passed through nitrogen, 10-15 points of mixing
Clock;Reaction solution is then warming up to 75-80 DEG C, reacts 7-8 hours;Reaction solution is evaporated under reduced pressure, removes the tert-butyl alcohol, is obtained described
Dispersant Sodium Polyacrylate.
The dispersant Sodium Polyacrylate molecular weight that the present invention obtains is low, and range of molecular weight distributions is narrow, can effectively subtract
Few material is reunited, and improves dispersion effect.
Preferably, described adhesive is polyacrylic binder, aqueous polyurethane adhesive, lactyl polyester binder
In one or more mixtures.
The preparation process of the lactyl polyester binder is:DL-LACTIC ACID, 6-caprolactone and pungent are added in reaction vessel
The mass ratio of sour stannous, wherein DL-LACTIC ACID, 6-caprolactone and stannous octoate is (90-94):(6-10):0.1, in 400-600
Rev/min mixing speed under stirring be warming up to 120-140 DEG C, react 2-8 hours;Reaction solution is warming up to 160-180 DEG C, gathered
Close 4-8 hours;After polymerization terminates, reaction solution is cooled to room temperature, adds the volume ratio of chloroform, reaction solution and chloroform
For 1:(0.6-0.8), 5-10 minutes are stirred with 200-300 revs/min of rotating speed;Then methanol is added, methanol and reaction solution
Volume ratio is (5-6):1,10-15 minutes are stirred with 200-300 revs/min of rotating speed, have precipitation to produce;With 1000-2000 turn/
The rotating speed centrifugation 10-15 minutes of minute, supernatant is abandoned, obtains bottom solid;By bottom solid in 50-60 DEG C, vacuum 0.08-
6-10 hours are dried under conditions of 0.09MPa, obtain the lactyl polyester binder.
PLA obtains because of its good biocompatibility and Bioabsorbable in terms of medical treatment with degradation material
It is widely applied.The present invention is improved using 6-caprolactone as the stiffness with poly lactic acid polymerized monomer, segment, submissive
Property be improved, their copolymer is used for adhesive used for textiles, not only with excellent bond properties, and can biology drop
Solution, it is environmentally friendly.
Inventor has found by experiment, when the mixture that adhesive is polyacrylic binder and lactyl polyester binder
When, bonding effect is more excellent.Preferably, described adhesive is the mixing of polyacrylic binder and lactyl polyester binder
Thing, the wherein mass ratio of polyacrylic binder and lactyl polyester binder are 1:(3-5).
The two of the technical problems to be solved by the invention are to provide a kind of preparation method of textile long acting antibiotic treatment fluid.
The preparation method of the textile long acting antibiotic treatment fluid comprises the following steps:Each raw material is weighed by formula;By original
In material input high-speed mixer, 10-12 hours are stirred with 100-200 revs/min of rotating speed in 25-35 DEG C, obtain the weaving
Product long acting antibiotic treatment fluid.
Beneficial effects of the present invention:The antimicrobial treatment solution of the present invention uses multiple compounds, weaves and produces with hair, cotton and blending
Product are compound to have good adhesiveness, is added on hair, cotton and blending textile product surface so that hair, cotton and blending weaving production
Product, which have, to be resisted common germ, suppresses resistance venereal bacteria, high-efficient and lasting, is played environment purification, is eliminated peculiar smell, self-cleaning health care, not dirty
Contaminate environment and have no side effect to human body, obtain more health benefits beneficial to people, the present invention uses multiple compounds, Mei Zhonghua
Coordinated effect between the different functional groups of compound, plays a part of anti-common germ, suppresses resistance venereal bacteria, get rid of simultaneously
The not water-fastness of natural antibacterial agent is abandoned, it is toxic to wait side effect.
Embodiment
Each raw material introduction in embodiment:
Polyacrylic binder, purchased from Jiangyin Fine Chemical Works.
A11 non-ionic dispersing agents, purchased from Foshan City Shuande head of district's sky trade Co., Ltd, specific composition is polyacrylic acid
Sodium.
Coupling agent, purchased from Zhengzhou City Jinshui District Jia Xuan chemical industry firm, model KH570.
Antiphen, No. CAS:97-23-4, purchased from Hubei giant dragon hall medication chemistry Co., Ltd.
Isoquercitrin, No. CAS:21637-25-2, purchased from Nanjing Duo Long bio tech ltd.
N, N- dihydroxyethylglycin, CAS:150-25-4, purchased from Shanghai Nuo Yuan Industrial Co., Ltd.s.
3- mercaptopyridines, CAS:16133-26-9, purchased from Shanghai Nuo He Chemical Industry Science Co., Ltd.
Dodecyl benzyl dimethyl ammonium chloride, CAS:139-07-1, purchased from Shanghai Losec Chemical Co., Ltd..
Acrylic acid, purchased from subfamily power Chemical Industry Science Co., Ltd of BOE.
2,4,5,6- tetrachloro phthalonitriles, No. CAS:1897-45-6, purchased from Wuhan Yi Tai Science and Technology Ltd.s Shanghai point
Company.
Isopropanol, No. CAS:67-63-0, purchased from this hundred full chemistries (Shanghai) Co., Ltd..
Ammonium persulfate, No. CAS:7727-54-0, purchased from this hundred full chemistries (Shanghai) Co., Ltd..
N- dodecyl mereaptan, No. CAS:112-55-0, purchased from Rui Pu new materials Co., Ltd of Liyang City.
Methyl tricapryl ammonium chloride, No. CAS:5137-55-3, purchased from Chengdu Hua Xia chemical reagent Co., Ltd.
Acetone, No. CAS:67-64-1.
Carbon disulfide, No. CAS:75-15-0, purchased from lark prestige Science and Technology Ltd..
Initiator A IBN, No. CAS:78-67-1, purchased from azodiisobutyronitrile lark prestige Science and Technology Ltd..
The tert-butyl alcohol, No. CAS:75-65-0, hundred million bio tech ltd are praised purchased from Zhuhai.
DL-LACTIC ACID, No. CAS:598-82-3, purchased from Nanjing Kang Manlin chemical industry Industrial Co., Ltd..
6-caprolactone, No. CAS:502-44-3, hundred million bio tech ltd are praised purchased from Zhuhai.
Stannous octoate, No. CAS:301-10-0, purchased from Nantong chemical products Co., Ltd of Hao Thailands.
Chloroform, No. CAS:67-66-3, purchased from Shanghai Nuo Yuan Industrial Co., Ltd.s.
Below by embodiment, the present invention will be further described.
In the present invention, if not refering in particular to, all devices and raw material are commercially available or the industry is conventional, following
Method in embodiment, it is this area conventional method unless otherwise instructed.
The specific preparation process of the Unined RM antiseptics used in embodiment 1-3 for:
The Unined RM antiseptics are counted including 15 parts of antiphens, 3 parts of isoquercitrin, 4 parts of N, N- dihydroxies in parts by weight
Base ethyl glycine, 5 parts of mercaptopyridines, 8 parts of dodecylbenzyl dimethyl ammoniums, 10 parts of A11 non-ionic dispersing agents, 22 parts
Acrylic acid and 15 part 2,4,5,6- tetrachloro phthalonitriles.
The preparation method of the Unined RM antiseptics is:
(1) by load weighted antiphen, isoquercitrin, N, N- dihydroxyethylglycins, mercaptopyridine, dodecyl benzyl
Base dimethyl ammonium and 2,4,5,6- tetrachloro phthalonitriles mix at room temperature, form unit for uniform suspension;
(2) A11 non-ionic dispersing agents are added in the suspension obtained to step (1), with 500 in homogenizer
Rev/min rotating speed be stirred 12 hours after, add acrylic acid, continue to be stirred 5 minutes with 500 revs/min of rotating speed,
Obtain the Unined RM antiseptics.
Treatment fluid is tested:
Embodiment 1
Raw material:Water:97.5wt%, Unined RM antiseptics:0.5wt%, polyacrylic binder:1.5wt%, A11 are non-
Ionic dispersant:0.25wt%, coupling agent:0.25wt%.
The preparation method of the textile long acting antibiotic treatment fluid is:Each raw material is weighed by formula;Raw material is put at a high speed
In mixer, stirred 10 hours with 200 revs/min of rotating speed in 30 DEG C, obtain the textile long acting antibiotic treatment fluid.
Embodiment 2
Raw material:Water:84wt%, Unined RM antiseptics:3.5wt%, polyacrylic binder:11.5wt%, A11 are non-
Ionic dispersant:0.5wt%, coupling agent:0.5wt%.
The preparation method of the textile long acting antibiotic treatment fluid is:Each raw material is weighed by formula;Raw material is put at a high speed
In mixer, stirred 10 hours with 200 revs/min of rotating speed in 30 DEG C, obtain the textile long acting antibiotic treatment fluid.
Embodiment 3
Raw material:Water:90wt%, Unined RM antiseptics:2wt%, polyacrylic binder:7.3wt%, A11 nonionic
Type dispersant 0.4wt%, coupling agent:0.3wt%.
The preparation method of the textile long acting antibiotic treatment fluid is:Each raw material is weighed by formula;Raw material is put at a high speed
In mixer, stirred 10 hours with 200 revs/min of rotating speed in 30 DEG C, obtain the textile long acting antibiotic treatment fluid.
The long acting antibiotic performance of embodiment 1-2 textile long acting antibiotic treatment fluid is tested:
Material:
Textile long acting antibiotic treatment fluid
Textile 1:Wool Overcoat of baby (100% wool), it is commercially available.
Textile 2:Pure cotton Overcoat of baby (100% combed cotton), it is commercially available.
Textile 3:Blending upper garment of children clothes (80% combed cotton, 17% terylene, 3% spandex), it is commercially available.
Machine:Antibacterial textile process for producing line, including wash, soak, spin-drying device, drying plant device.
Step:
The textile of outsourcing is put into antimicrobial treatment production line, adds the treatment fluid produced according to embodiment, the place
The weight ratio for managing liquid and textile is 10:1;Then stirred 30 minutes with 60 revs/min of mixing speed at room temperature;Again will place
Reason liquid bleeds off standby;After the textile of moistening dries at a high speed in spin dryer tube, it is put into dryer and is heated to 120 DEG C of drying 1
Hour, it is stand-by.
Textile 1, textile 2, the textile 3 handled by the antimicrobial treatment solution of embodiment 1 is denoted as sample 1, sample
2, sample 3.
Textile 1, textile 2, the textile 3 handled by the antimicrobial treatment solution of embodiment 2 is denoted as sample 4, sample
5, sample 6.
Antibacterial test
Antibacterial test is carried out according to FZ/T73023-2006 standards.The strain of experiment is Escherichia coli (ATCC25922), resistance to
Methicillin golden yellow staphylococcus (ATCC43300), golden yellow staphylococcus (ATCC6538), Candida albicans (ATCC10231).
Washing by soaking is tested
By the textile samples that antimicrobial treatment solution obtained above is handled according to FZ/T73023 standard wash, but wash
Number is 50 times required in 100 times rather than standard.Obtained textile carries out antibacterial test.
The embodiment 1 of table 1. processing textile print wash 100 times after bacteriostasis rate (%)
Experimental strain |
Sample 1 |
Sample 2 |
Sample 3 |
Escherichia coli |
96.1 |
98.9 |
97.2 |
Golden yellow staphylococcus |
99.3 |
99.2 |
98.3 |
Candida albicans |
96.7 |
98.6 |
90.2 |
Methicillin-resistant staphylococcus staphylococcus |
99.8 |
99.2 |
99.1 |
As it can be seen from table 1 the bacteriostasis rate after washing 100 times of the textile after the processing of embodiment 1 is above 70%, explanation
The present invention has the bacteriostasis of practicality.
The embodiment 2 of table 2. processing textile print wash 100 times after bacteriostasis rate (%)
Experimental strain |
Sample 4 |
Sample 5 |
Sample 6 |
Escherichia coli |
99.9 |
99.9 |
98.5 |
Golden yellow staphylococcus |
99.8 |
99.3 |
99.2 |
Candida albicans |
98.9 |
99.1 |
95.1 |
Methicillin-resistant staphylococcus staphylococcus |
98.4 |
99.7 |
93.4 |
From table 2 it can be seen that the bacteriostasis rate after washing 100 times of the textile after the processing of embodiment 2 is above 70%, explanation
The present invention has the bacteriostasis of practicality.
Embodiment 4
Raw material:Water:97.5wt%, Unined RM antiseptics:0.5wt%, polyacrylic binder:1.5wt%, disperse
Agent Sodium Polyacrylate:0.25wt%, coupling agent:0.25wt%.
The preparation method of the textile long acting antibiotic treatment fluid is:Each raw material is weighed by formula;Raw material is put at a high speed
In mixer, stirred 10 hours with 200 revs/min of rotating speed in 30 DEG C, obtain the textile long acting antibiotic treatment fluid.
Wherein the specific preparation process for the Unined RM antiseptics that embodiment 4 uses for:
The Unined RM antiseptics are counted including 15 parts of antiphens, 3 parts of isoquercitrin, 4 parts of N, N- dihydroxies in parts by weight
Base ethyl glycine, 5 parts of mercaptopyridines, 8 parts of dodecylbenzyl dimethyl ammoniums, 10 parts of dispersant Sodium Polyacrylates, 22 parts
Acrylic acid and 15 part 2,4,5,6- tetrachloro phthalonitriles.
The preparation method of the Unined RM antiseptics is:
(1) by load weighted antiphen, isoquercitrin, N, N- dihydroxyethylglycins, mercaptopyridine, dodecyl benzyl
Base dimethyl ammonium and 2,4,5,6- tetrachloro phthalonitriles mix at room temperature, form unit for uniform suspension;
(2) in the suspension obtained to step (1) add dispersant Sodium Polyacrylate, in homogenizer with 500 turns/
After the rotating speed of minute is stirred 12 hours, acrylic acid is added, continues to be stirred 5 minutes with 500 revs/min of rotating speed, obtains
To the Unined RM antiseptics.
The preparation process of the dispersant Sodium Polyacrylate is:By acrylic acid and isopropanol with mass ratio 1:1 mixing, is obtained
Mixed liquor A;By ammonium persulfate and deionized water with solid-to-liquid ratio 1:25 (g/mL) are well mixed, obtain mixed liquid B;By positive 12 sulphur
Alcohol, isopropanol and deionized water are with mass ratio 1:25:7 is well mixed, obtains mixed liquor C, wherein n- dodecyl mereaptan, acrylic acid,
The mass ratio of ammonium persulfate is 1:22:1;Mixed liquor C is heated to 85 DEG C, while mixed liquor A is added dropwise with 8 μ L/s rate of addition
And mixed liquid B;After charging, reacted 3 hours in 85 DEG C;After reaction terminates, reaction solution is cooled to 40 DEG C, uses mass fraction
The pH value of reaction solution is adjusted to 7 for 30% sodium hydrate aqueous solution;Reaction solution is evaporated under reduced pressure, removes isopropyl alcohol and water,
Obtain the dispersant Sodium Polyacrylate.
Embodiment 5
Raw material:Water:97.5wt%, Unined RM antiseptics:0.5wt%, polyacrylic binder:1.5wt%, disperse
Agent Sodium Polyacrylate:0.25wt%, coupling agent:0.25wt%.
The preparation method of the textile long acting antibiotic treatment fluid is:Each raw material is weighed by formula;Raw material is put at a high speed
In mixer, stirred 10 hours with 200 revs/min of rotating speed in 30 DEG C, obtain the textile long acting antibiotic treatment fluid.
Wherein the specific preparation process for the Unined RM antiseptics that embodiment 5 uses for:
The Unined RM antiseptics are counted including 15 parts of antiphens, 3 parts of isoquercitrin, 4 parts of N, N- dihydroxies in parts by weight
Base ethyl glycine, 5 parts of mercaptopyridines, 8 parts of dodecylbenzyl dimethyl ammoniums, 10 parts of dispersant Sodium Polyacrylates, 22 parts
Acrylic acid and 15 part 2,4,5,6- tetrachloro phthalonitriles.
The preparation method of the Unined RM antiseptics is:
(1) by load weighted antiphen, isoquercitrin, N, N- dihydroxyethylglycins, mercaptopyridine, dodecyl benzyl
Base dimethyl ammonium and 2,4,5,6- tetrachloro phthalonitriles mix at room temperature, form unit for uniform suspension;
(2) in the suspension obtained to step (1) add dispersant Sodium Polyacrylate, in homogenizer with 500 turns/
After the rotating speed of minute is stirred 12 hours, acrylic acid is added, continues to be stirred 5 minutes with 500 revs/min of rotating speed, obtains
To the Unined RM antiseptics.
The preparation process of the dispersant Sodium Polyacrylate is:(1) by n- dodecyl mereaptan, methyl tricapryl ammonium chloride and third
Ketone is added sequentially in reaction vessel, and the n- dodecyl mereaptan, methyl trioctylphosphine chlorination are pressed and the mass ratio of acetone is 1:0.07:
3.5, nitrogen is passed through, while temperature of reaction system is remained 5 DEG C, stirred 3 minutes with 180 revs/min of rotating speed;Add quality
Fraction is 40% sodium hydrate aqueous solution, and the mass ratio of sodium hydrate aqueous solution and n- dodecyl mereaptan is 0.4:1, with 180 turns/
The rotating speed of minute stirs 20 minutes;Then the acetone soln for the carbon disulfide that addition mass fraction is 25%, the third of carbon disulfide
The mass ratio of ketone solution and n- dodecyl mereaptan is 1.4:1, stirred 10 minutes with 180 revs/min of rotating speed;Then successively by chloroform
With the sodium hydrate aqueous solution addition that mass fraction is 40%, the mass ratio of chloroform, sodium hydrate aqueous solution and n- dodecyl mereaptan
For 0.9:2:1, with 180 revs/min of rotating speed stirring reaction 16 hours;Reaction terminate after, add deionized water, deionized water and
The mass ratio of n- dodecyl mereaptan is 30:1, after mixing, add the volume of the hydrochloric acid that mass fraction is 36%, hydrochloric acid and deionized water
Than for 1:20, stirred 25 minutes with 180 revs/min of rotating speed;Nitrogen is passed through, makes acetone volatilization totally;Using 80 mesh filter cloth mistakes
Filter, collect filter cake;Filter cake is dried 8 hours under conditions of 55 DEG C, vacuum 0.07MPa, obtains chain-transferring agent;(2) by third
Olefin(e) acid, initiator A IBN, the tert-butyl alcohol and chain-transferring agent are added in reaction vessel, wherein acrylic acid, initiator A IBN, the tert-butyl alcohol and
The mass ratio of chain-transferring agent is 1:0.002:1.8:0.4, nitrogen is passed through, is mixed 15 minutes;Reaction solution is then warming up to 80 DEG C,
Reaction 7 hours;Reaction solution is evaporated under reduced pressure, the tert-butyl alcohol is removed, obtains the dispersant Sodium Polyacrylate.
The dispersive property of the dispersant of embodiment 1,4 and 5 is measured:A diameter of 6 μm of glass fibres (are purchased from and appointed
The emerging glass fibre factory in Qiu Shi Yongxings), the section that length is 5cm is cut into, be put into beater (has purchased from Xianyang Tai Site testing equipments
Limit company, model PL4-00) in 10-20 minutes are beaten with 500 revs/min of rotating speed, glass fibre is cut off rapidly in wadding
Solid fraction, it is dried 8 hours in 60 DEG C, it is stand-by;200mL water, 4g glass fibres and 0.4g dispersants (are purchased from good fortune with agitator
Hai Te Machinery Co., Ltd.s of Jian Sheng Nan'ans) it is scattered 10 minutes with 200 revs/min of rotating speed, the sedimentation time is then determined, simultaneously
Observe the state of dispersion liquid.
Specific test result is shown in Table 3.
The dispersive property test result table of table 3.
Embodiment 6
Raw material:Water:97.5wt%, Unined RM antiseptics:0.5wt%, lactyl polyester binder:1.5wt%, point
Powder Sodium Polyacrylate:0.25wt%, coupling agent:0.25wt%.
The preparation method of the textile long acting antibiotic treatment fluid is:Each raw material is weighed by formula;Raw material is put at a high speed
In mixer, stirred 10 hours with 200 revs/min of rotating speed in 30 DEG C, obtain the textile long acting antibiotic treatment fluid.
Wherein the specific preparation process for the Unined RM antiseptics that embodiment 6 uses for:
The Unined RM antiseptics are counted including 15 parts of antiphens, 3 parts of isoquercitrin, 4 parts of N, N- dihydroxies in parts by weight
Base ethyl glycine, 5 parts of mercaptopyridines, 8 parts of dodecylbenzyl dimethyl ammoniums, 10 parts of dispersant Sodium Polyacrylates, 22 parts
Acrylic acid and 15 part 2,4,5,6- tetrachloro phthalonitriles.
The preparation method of the Unined RM antiseptics is:
(1) by load weighted antiphen, isoquercitrin, N, N- dihydroxyethylglycins, mercaptopyridine, dodecyl benzyl
Base dimethyl ammonium and 2,4,5,6- tetrachloro phthalonitriles mix at room temperature, form unit for uniform suspension;
(2) in the suspension obtained to step (1) add dispersant Sodium Polyacrylate, in homogenizer with 500 turns/
After the rotating speed of minute is stirred 12 hours, acrylic acid is added, continues to be stirred 5 minutes with 500 revs/min of rotating speed, obtains
To the Unined RM antiseptics.
The preparation process of the dispersant Sodium Polyacrylate is:(1) by n- dodecyl mereaptan, methyl tricapryl ammonium chloride and third
Ketone is added sequentially in reaction vessel, and the n- dodecyl mereaptan, methyl trioctylphosphine chlorination are pressed and the mass ratio of acetone is 1:0.07:
3.5, nitrogen is passed through, while temperature of reaction system is remained 5 DEG C, stirred 3 minutes with 180 revs/min of rotating speed;Add quality
Fraction is 40% sodium hydrate aqueous solution, and the mass ratio of sodium hydrate aqueous solution and n- dodecyl mereaptan is 0.4:1, with 180 turns/
The rotating speed of minute stirs 20 minutes;Then the acetone soln for the carbon disulfide that addition mass fraction is 25%, the third of carbon disulfide
The mass ratio of ketone solution and n- dodecyl mereaptan is 1.4:1, stirred 10 minutes with 180 revs/min of rotating speed;Then successively by chloroform
With the sodium hydrate aqueous solution addition that mass fraction is 40%, the mass ratio of chloroform, sodium hydrate aqueous solution and n- dodecyl mereaptan
For 0.9:2:1, with 180 revs/min of rotating speed stirring reaction 16 hours;Reaction terminate after, add deionized water, deionized water and
The mass ratio of n- dodecyl mereaptan is 30:1, after mixing, add the volume of the hydrochloric acid that mass fraction is 36%, hydrochloric acid and deionized water
Than for 1:20, stirred 25 minutes with 180 revs/min of rotating speed;Nitrogen is passed through, makes acetone volatilization totally;Using 80 mesh filter cloth mistakes
Filter, collect filter cake;Filter cake is dried 8 hours under conditions of 55 DEG C, vacuum 0.07MPa, obtains the chain-transferring agent;(2)
Acrylic acid, initiator A IBN, the tert-butyl alcohol and chain-transferring agent are added in reaction vessel, wherein acrylic acid, initiator A IBN, tertiary fourth
The mass ratio of alcohol and chain-transferring agent is 1:0.002:1.8:0.4, nitrogen is passed through, is mixed 15 minutes;Then reaction solution is warming up to
80 DEG C, react 7 hours;Reaction solution is evaporated under reduced pressure, the tert-butyl alcohol is removed, obtains the dispersant Sodium Polyacrylate.
The preparation process of the lactyl polyester binder is:DL-LACTIC ACID, 6-caprolactone and pungent are added in reaction vessel
The mass ratio of sour stannous, wherein DL-LACTIC ACID, 6-caprolactone and stannous octoate is 90:10:0.1, in 500 revs/min of stirring speed
The lower stirring of degree is warming up to 120 DEG C, reacts 3 hours, with the moisture in elimination reaction system;Reaction solution is warming up to 160 DEG C, polymerization
8 hours;After reaction terminates, reaction solution is cooled to room temperature, adds chloroform, the volume ratio of reaction solution and chloroform is 1:
0.8, stirred 5 minutes with 300 revs/min of rotating speed;Then methanol is added, the volume ratio of methanol and reaction solution is 6:1, with 200-
300 revs/min of rotating speed stirring 10-15 minutes, there is precipitation to produce;Centrifuged 15 minutes with 1000 revs/min of rotating speed, abandon supernatant
Liquid, obtain bottom solid;Bottom solid is dried 10 hours under conditions of 55 DEG C, vacuum 0.08MPa, obtains the lactic acid
Base polyester binder.
Embodiment 7
Raw material:Water:97.5wt%, Unined RM antiseptics:0.5wt%, adhesive:1.5wt%, dispersant polypropylene
Sour sodium:0.25wt%, coupling agent:0.25wt%.
Described adhesive is the mixture of polyacrylic binder and lactyl polyester binder, wherein polyacrylic adhesive
The mass ratio of agent and lactyl polyester binder is 1:3.
The preparation method of the textile long acting antibiotic treatment fluid is:Each raw material is weighed by formula;Raw material is put at a high speed
In mixer, stirred 10 hours with 200 revs/min of rotating speed in 30 DEG C, obtain the textile long acting antibiotic treatment fluid.
Wherein the specific preparation process for the Unined RM antiseptics that embodiment 7 uses for:
The Unined RM antiseptics are counted including 15 parts of antiphens, 3 parts of isoquercitrin, 4 parts of N, N- dihydroxies in parts by weight
Base ethyl glycine, 5 parts of mercaptopyridines, 8 parts of dodecylbenzyl dimethyl ammoniums, 10 parts of dispersant Sodium Polyacrylates, 22 parts
Acrylic acid and 15 part 2,4,5,6- tetrachloro phthalonitriles.
The preparation method of the Unined RM antiseptics is:
(1) by load weighted antiphen, isoquercitrin, N, N- dihydroxyethylglycins, mercaptopyridine, dodecyl benzyl
Base dimethyl ammonium and 2,4,5,6- tetrachloro phthalonitriles mix at room temperature, form unit for uniform suspension;
(2) in the suspension obtained to step (1) add dispersant Sodium Polyacrylate, in homogenizer with 500 turns/
After the rotating speed of minute is stirred 12 hours, acrylic acid is added, continues to be stirred 5 minutes with 500 revs/min of rotating speed, obtains
To the Unined RM antiseptics.
The preparation process of the dispersant Sodium Polyacrylate is:(1) by n- dodecyl mereaptan, methyl tricapryl ammonium chloride and third
Ketone is added sequentially in reaction vessel, and the n- dodecyl mereaptan, methyl trioctylphosphine chlorination are pressed and the mass ratio of acetone is 1:0.07:
3.5, nitrogen is passed through, while temperature of reaction system is remained 5 DEG C, stirred 3 minutes with 180 revs/min of rotating speed;Add quality
Fraction is 40% sodium hydrate aqueous solution, and the mass ratio of sodium hydrate aqueous solution and n- dodecyl mereaptan is 0.4:1, with 180 turns/
The rotating speed of minute stirs 20 minutes;Then the acetone soln for the carbon disulfide that addition mass fraction is 25%, the third of carbon disulfide
The mass ratio of ketone solution and n- dodecyl mereaptan is 1.4:1, stirred 10 minutes with 180 revs/min of rotating speed;Then successively by chloroform
With the sodium hydrate aqueous solution addition that mass fraction is 40%, the mass ratio of chloroform, sodium hydrate aqueous solution and n- dodecyl mereaptan
For 0.9:2:1, with 180 revs/min of rotating speed stirring reaction 16 hours;Reaction terminate after, add deionized water, deionized water and
The mass ratio of n- dodecyl mereaptan is 30:1, after mixing, add the volume of the hydrochloric acid that mass fraction is 36%, hydrochloric acid and deionized water
Than for 1:20, stirred 25 minutes with 180 revs/min of rotating speed;Nitrogen is passed through, makes acetone volatilization totally;Using 80 mesh filter cloth mistakes
Filter, collect filter cake;Filter cake is dried 8 hours under conditions of 55 DEG C, vacuum 0.07MPa, obtains the chain-transferring agent;(2)
Acrylic acid, initiator A IBN, the tert-butyl alcohol and chain-transferring agent are added in reaction vessel, wherein acrylic acid, initiator A IBN, tertiary fourth
The mass ratio of alcohol and chain-transferring agent is 1:0.002:1.8:0.4, nitrogen is passed through, is mixed 15 minutes;Then reaction solution is warming up to
80 DEG C, react 7 hours;Reaction solution is evaporated under reduced pressure, the tert-butyl alcohol is removed, obtains the dispersant Sodium Polyacrylate.
The preparation process of the lactyl polyester binder is:DL-LACTIC ACID, 6-caprolactone and pungent are added in reaction vessel
The mass ratio of sour stannous, wherein DL-LACTIC ACID, 6-caprolactone and stannous octoate is 90:10:0.1, in 500 revs/min of stirring speed
The lower stirring of degree is warming up to 120 DEG C, reacts 3 hours, with the moisture in elimination reaction system;Reaction solution is warming up to 160 DEG C, polymerization
8 hours;After reaction terminates, reaction solution is cooled to room temperature, adds chloroform, the volume ratio of reaction solution and chloroform is 1:
0.8, stirred 5 minutes with 300 revs/min of rotating speed;Then methanol is added, the volume ratio of methanol and reaction solution is 6:1, with 200-
300 revs/min of rotating speed stirring 10-15 minutes, there is precipitation to produce;Centrifuged 15 minutes with 1000 revs/min of rotating speed, abandon supernatant
Liquid, obtain bottom solid;Bottom solid is dried 10 hours under conditions of 55 DEG C, vacuum 0.08MPa, obtains the lactic acid
Base polyester binder.
The bond properties of embodiment 5-7 adhesive is measured, specific testing procedure is as follows:
(1) slurry is configured:25g adhesives are weighed, add 100mL distilled water, are mixed 10 minutes, are warming up to 95 DEG C, insulation 1
Hour, obtain slurry;
(2) the pure cotton rove being wound on metal frame is impregnated 5 (purchased from Weifang profit Photar Textile Co., Ltd.) in slurries
Minute, by rove framework take out hang airing, then by light sizing rove bar cut collect it is standby;
(3) 24 hours are balanced after light sizing rove bar is dried, in the environment of 20 DEG C of temperature, relative humidity 65%, then
Using universal testing machine (being purchased from Shanghai Zhu Jin Analytical Instrument Co., Ltd, model zwick) test light sizing rove bar
Maximum strength and work to break.
Test condition:Draw speed is 50mm/min, and sample chuck distance is 100mm, 20 DEG C of test temperature, relative humidity
65%, each embodiment tests 20 samples.After rejecting abnormalities value, its average value is taken as test result.
Specific test result is shown in Table 4.
Table 4:Bond properties test result table
|
Maximum strength (N) |
Work to break (J) |
Embodiment 5 |
58.3 |
0.215 |
Embodiment 6 |
66.2 |
0.279 |
Embodiment 7 |
72.8 |
0.302 |
It is described above, simply one embodiment of the invention, not the invention is made any formal
Limitation, on the basis of the technical scheme of the invention is not departed from, made simple modification, equivalent variations or modification, falls
Enter the protection domain of the invention.