CN104727143A - Preparation method of composite antistatic agent for fiber fabric - Google Patents
Preparation method of composite antistatic agent for fiber fabric Download PDFInfo
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- CN104727143A CN104727143A CN201510120620.3A CN201510120620A CN104727143A CN 104727143 A CN104727143 A CN 104727143A CN 201510120620 A CN201510120620 A CN 201510120620A CN 104727143 A CN104727143 A CN 104727143A
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Abstract
The invention discloses a preparation method of a composite antistatic agent for a fiber fabric. The composite antistatic agent for the fiber fabric in the preparation method comprises the following components: a butanol phosphate ester antistatic agent, a terminal hydroxyl hyperbranched antistatic agent, a terminal carboxyl hyperbranched antistatic agent and a terminal quaternary ammonium salt hyperbranched antistatic agent; and the preparation method comprises the following steps: firstly, respectively preparing the butanol phosphate ester antistatic agent, the terminal hydroxyl hyperbranched antistatic agent, the terminal carboxyl hyperbranched antistatic agent and the terminal quaternary ammonium salt hyperbranched antistatic agent; and mixing the four antistatic agents to prepare the composite antistatic agent for the fiber fabric. The preparation method is simple and feasible; and the prepared antistatic agent has a good antistatic effect, good heat resistance and good acid and alkali resistance.
Description
Technical field
The invention belongs to textile technology field, be specifically related to the preparation method of a kind of fabric lining Combined Electrostatic agent.
Background technology
Chemical fibre, especially synthetic fiber, because it compares the characteristic with many excellences with natural fabric, as they can obtain special performance and aesthetic properties in procedure of fibre production processing, and cheap, meeting with property is high, strength and toughness is good, developed rapidly and applied widely.Synthetic fiber have plurality of advantages, but also there are many very important shortcomings, poor, the easy Accumulating charge of as low in hygroscopicity, dyeability, produce electrostatic and snugness of fit difference etc., must carry out many-side to its performance to improve, the development of synthesising fibre dimension just may have more brilliant breakthrough.
Along with the output of synthetic fiber increases severely rapidly, weaving electrostatic problem is just becoming increasingly acute, and current anlistatig method can be divided into physical method and chemical method.Physical method has: (1) improves relative air humidity to improve the leakage electrostatic capacity of fiber; (2) the opposite polarity different fibrage of electrification is selected to become fabric; (3) send out spraying plating layer of metal film in fiber surface vacuum, make metalized fibers; (4) composite conducting fiber is become with stainless short metal fibre or fibre bundle with chemical fibre blending; (5) carbon granules is embedded to make carbon fibre at fiber surface.Chemical method has (1) adds chemical agent or antistatic fibre made by antistatic additive in the spinning solution of chemical fibre polymer; (2) chemically metalized fibers is produced; (3) fiber and something chemically reactive is made; (4) with surfactant, fiber is processed.Physical has certain use restriction in these methods, is one of common method of antistatic fibre with antistatic additive to fibre finish.
In the anti-static agent of current use, although CATION anti-static agent antistatic effect is good, its Main N-containing Compounds, is easy to variable color in hot environment, affects the dyeing of fiber and fabric thereof; The anti-electric effect of anionic antistatic agent is also very desirable, but wherein sulfuric acid to oxygen and hot less stable; Non-ionic antistatic agent toxicity compared with ionic anti-static agent is little, stimulates skin thing, and with emulsification and wetting action, but it is poor and itself can not ionize to fibers adsorption, and therefore antistatic property is poor; Organic silicon type antistatic additive is given prominence to antistatic effect, but its residue under High Temperature And Velocity rubbing action after decomposes is more, is easy to form white powder; Organic fluorine-type antistatic additive, due to expensive, seldom uses; The Aqueous Solution Viscosity of Polymer Antistatic Agent is large, is easy to coefficient of friction is raised in high speed spinning process, not favourable to preventing the generation of electrostatic.Develop a kind of good water solubility, foaming type is little, have good heat resistance and acid-proof alkaline, anti-electricity is respond well, and preparation is relatively simple, and the antistatic additive that cost is low is the problem that the art personnel need solution badly.
Summary of the invention
Technical problem to be solved by this invention is, for the shortcoming that above prior art exists, propose a kind of preparation method of fabric lining composite antistatic agent, this preparation method is simple, the antistatic additive prepared has good anti-electric effect, has good heat resistance, acid-proof alkaline.
The technical scheme that the present invention solves above technical problem is:
A preparation method for fabric lining composite antistatic agent, in this preparation method, fabric lining composite antistatic agent comprises following component according to the mass fraction:
Butanol phosphate antistatic additive 35-40 part
Superbrnaching end-hydroxy antistatic additive 5-10 part
End carboxyl super branched anti-antistatic additive 10-15 part
End quaternary ammonium salt hyperbranched antistatic additive 20-25 part
The concrete preparation method of this fabric lining composite antistatic agent is as follows:
(1) preparation of butanol phosphate antistatic additive
(1) joined in clean there-necked flask by n-butanol, then add phosphorus pentoxide, slowly put in the there-necked flask of n-butanol with spoon, there-necked flask is placed on and is equipped with in the large beaker of cold water, is no more than 50 DEG C to control its temperature in adition process;
(2) finished, respectively with plug, with thermometer plug, there-necked flask is sealed, there-necked flask is fixed on electric mixer, and puts into the modulated thermostat water bath to 70 DEG C, when thermometer registration is 70 DEG C, start timing, accurately pipette deionized water with pipette after reaction 4h to add there-necked flask and be hydrolyzed, hydrolysis time is 2-3h, after reaction terminates, and cooling, take out product, namely obtain butanol phosphate antistatic additive;
(2) preparation of superbrnaching end-hydroxy antistatic additive
(1) chlorinated dodecane is dissolved in absolute ethyl alcohol, add in there-necked flask, stirring is warming up to 70-80 DEG C, be dissolved in ethanol and drip in there-necked flask getting diethanol amine, stirring, add sodium hydroxid powder, be warming up to backflow to produce, insulation reaction 4-5h, decompression distillation after thick product of purifying to obtain, obtains core molecule;
The mass ratio wherein adding chlorinated dodecane, diethanol amine and NaOH is 10:1:0.4;
(2) by diethanol amine and succinic anhydride, be dissolved in respectively in DMA, diethanolamine solution added in there-necked flask, be warming up to 30 DEG C, slowly add succinic anhydride, dropwise in control 1h, react 3h at 26-30 DEG C, obtain monomer.
Wherein, the mass ratio adding diethanol amine and succinic anhydride is 1.03:1;
(3) obtained core molecule is joined prepare in the reactor of monomer, mixing and stirring, adds toluene and makes water entrainer, is adding catalyst, connect water knockout drum, agitating heating is until there is backflow to produce, and insulation reaction 3-4h, until anhydrous generation in water entrainer toluene, decompression distillation is carried out to product, except desolventizing, obtain a kind of faint yellow thick substances, i.e. superbrnaching end-hydroxy antistatic additive;
(3) preparation of carboxyl super branched anti-antistatic additive
Superbrnaching end-hydroxy antistatic additive obtained in step (two) is dissolved in N, in N-dimethylacetylamide, dissolve succinic anhydride with DMA, add DMAP, temperature is controlled at 80-85 DEG C, continuous stirring, mixing speed controls at 200-250r/min, drips succinic anhydride solution, reaction 5-6h, namely obtains end carboxyl super branched antistatic additive;
Wherein, superbrnaching end-hydroxy antistatic additive and succinic anhydride mass ratio be 7:1.3;
(4) preparation of the hyperbranched antistatic additive of quaternary ammonium salt is held
(1) the superbrnaching end-hydroxy antistatic additive of preparation in (two) is dissolved in DMA, adds in four-hole boiling flask, stir under nitrogen protection, add sodium hydroxid and epoxychloropropane, be warmed up to 45 DEG C, mixing speed is 300-350r/min, reaction 5-6h;
(2) product of reaction in above-mentioned steps (1) is filtered, getting worry liquid adds in four-hole boiling flask, stirred under nitrogen atmosphere is warming up to 65 DEG C, slow dropping triethylamine, reaction 5-6h, decompression distillation removes desolventizing and unreacted raw material, by further for product of distillation purification processes, dry 24h in 30 DEG C of vacuum drying chambers, namely obtain the hyperbranched antistatic additive of end quaternary ammonium salt;
Wherein, the mass ratio adding sodium hydroxid and epoxychloropropane is 13:18;
(5) the mixed system of fabric lining composite antistatic agent
(1) superbrnaching end-hydroxy antistatic additive, end carboxyl super branched anti-antistatic additive, end quaternary ammonium salt hyperbranched antistatic additive added in dispersion cylinder and stir, mixing speed is 400-500r/min, and temperature is 40-45 DEG C, and mixing time is 30-50min;
(2) in above-mentioned steps (1), add butanol phosphate antistatic additive to stir at 25-30 DEG C, mixing speed is 800-900r/min, and mixing time is 50-60min, namely obtains fabric lining composite antistatic agent.
The further technical scheme of the present invention is:
In the preparation method of aforementioned fibers fabric composite antistatic agent, when preparing butanol phosphate antistatic additive, the mol ratio of n-butanol and phosphorus pentoxide is 3.5:1; The amount adding deionized water is the 4-6% of n-butanol and five oxidation two mound gross masses.
In the preparation method of aforementioned fibers fabric composite antistatic agent, when prepared by superbrnaching end-hydroxy antistatic additive, catalyst used is toluenesulfonic acid.
The invention has the beneficial effects as follows:
(1) with the addition of supermolecule antistatic additive in the fabric lining composite antistatic agent prepared in the present invention, have three-D space structure, in fabric, antistatic additive can have good dispersiveness, and good compatibility can be had with matrix in fabric, thus there is good water-wash resistance.
(2) the superbrnaching end-hydroxy antistatic additive added in the present invention, is obtained by esterification, has good water-wash resistance, water imbibition, stability.
(3) the butanol phosphate antistatic additive added in the present invention, has higher hydrophily, good heat-resisting quantity, and the antistatic property of excellence.
(4) the butanol phosphate antistatic additive added in the present invention can at polymer surface oriented attachment, and lipophilic group is towards macromolecule, and hydrophilic radical is towards air, the latter can be associated with water, thus can surface conductivity be improved, rapid leak charge, reach anlistatig effect.
(5) in the present invention, phosphate antistatic additive has excellent heat-resisting quantity, and along with the growth of esterifying reagent carbochain, its heat-resisting quantity is become better and better, and can meet and use under the high temperature conditions, butanol phosphate antistatic additive, has higher resisting electrically relative to traditional phosphate anti-static agent.
(6) epoxychloropropane is adopted to carry out modification as the superbrnaching end-hydroxy antistatic additive of modifier to synthesis in the present invention, carry out quaternized with triethylamine again, the quaternary ammonium salt-modified property of first synthesis that the hyperbranched antistatic additive of end quaternary ammonium salt be obtained by reacting adopts with tradition, the method ratio of grafting again, productive rate adornment rate is high.
(7) the hyperbranched antistatic additive structure comparison synthesized in the present invention is complete, and end has more active group, and application has antistatic property excellent, good with matrix phase capacitive, viscosity is low, the feature that stability is high.
(8) the hyperbranched anti-static agent added in the present invention possesses special structure and good antistatic property, and simple on synthesis technique, cost of material is cheap.
Detailed description of the invention
embodiment 1
The present embodiment provides a kind of preparation method of fabric lining composite antistatic agent, and in this preparation method, fabric lining composite antistatic agent comprises following component according to the mass fraction:
Butanol phosphate antistatic additive: 40 parts, superbrnaching end-hydroxy antistatic additive: 8 parts, end carboxyl super branched anti-antistatic additive: 15 parts, the hyperbranched antistatic additive of end quaternary ammonium salt: 23 parts;
The concrete preparation method of this fabric lining composite antistatic agent is as follows:
(1) preparation of butanol phosphate antistatic additive
(1) joined in clean there-necked flask by n-butanol, then add phosphorus pentoxide, slowly put in the there-necked flask of n-butanol with spoon, there-necked flask is placed on and is equipped with in the large beaker of cold water, is no more than 50 DEG C to control its temperature in adition process;
The mol ratio of n-butanol and phosphorus pentoxide is 3.5:1;
(2) finished, respectively with plug, with thermometer plug, there-necked flask is sealed, there-necked flask is fixed on electric mixer, and puts into the modulated thermostat water bath to 70 DEG C, when thermometer registration is 70 DEG C, start timing, accurately pipette deionized water with pipette after reaction 4h to add there-necked flask and be hydrolyzed, hydrolysis time is 2h, after reaction terminates, and cooling, take out product, namely obtain butanol phosphate antistatic additive;
The amount adding deionized water is 5% of n-butanol and five oxidation two mound gross masses;
(2) preparation of superbrnaching end-hydroxy antistatic additive
(1) chlorinated dodecane is dissolved in absolute ethyl alcohol, add in there-necked flask, stirring is warming up to 75 DEG C, be dissolved in ethanol and drip in there-necked flask getting diethanol amine, stirring, add sodium hydroxid powder, be warming up to backflow to produce, insulation reaction 4h, decompression distillation after thick product of purifying to obtain, obtains core molecule;
The mass ratio wherein adding chlorinated dodecane, diethanol amine and NaOH is 10:1:0.4;
(2) by diethanol amine and succinic anhydride, be dissolved in respectively in DMA, diethanolamine solution added in there-necked flask, be warming up to 30 DEG C, slowly add succinic anhydride, dropwise in control 1h, react 3h at 28 DEG C, obtain monomer.
Wherein, the mass ratio adding diethanol amine and succinic anhydride is 1.03:1;
(3) obtained core molecule is joined prepare in the reactor of monomer, mixing and stirring, adds toluene and makes water entrainer, is adding catalyst toluenesulfonic acid, connect water knockout drum, agitating heating is until there is backflow to produce, and insulation reaction 4h, until anhydrous generation in water entrainer toluene, decompression distillation is carried out to product, except desolventizing, obtain a kind of faint yellow thick substances, i.e. superbrnaching end-hydroxy antistatic additive;
(3) preparation of carboxyl super branched anti-antistatic additive
Superbrnaching end-hydroxy antistatic additive obtained in step (two) is dissolved in N, in N-dimethylacetylamide, dissolve succinic anhydride with DMA, add DMAP, temperature is controlled at 80 DEG C, continuous stirring, mixing speed controls at 200r/min, drips succinic anhydride solution, reaction 5h, namely obtains end carboxyl super branched antistatic additive;
Wherein, superbrnaching end-hydroxy antistatic additive and succinic anhydride mass ratio be 7:1.3;
(4) preparation of the hyperbranched antistatic additive of quaternary ammonium salt is held
(1) the superbrnaching end-hydroxy antistatic additive of preparation in (two) is dissolved in DMA, adds in four-hole boiling flask, stir under nitrogen protection, add sodium hydroxid and epoxychloropropane, be warmed up to 45 DEG C, mixing speed is 350r/min, reaction 5h;
(2) product of reaction in above-mentioned steps (1) is filtered, getting worry liquid adds in four-hole boiling flask, stirred under nitrogen atmosphere is warming up to 65 DEG C, slow dropping triethylamine, reaction 6h, decompression distillation removes desolventizing and unreacted raw material, by further for product of distillation purification processes, dry 24h in 30 DEG C of vacuum drying chambers, namely obtain the hyperbranched antistatic additive of end quaternary ammonium salt;
Wherein, the mass ratio adding sodium hydroxid and epoxychloropropane is 13:18;
(5) the mixed system of fabric lining composite antistatic agent
(1) superbrnaching end-hydroxy antistatic additive, end carboxyl super branched anti-antistatic additive, end quaternary ammonium salt hyperbranched antistatic additive added in dispersion cylinder and stir, mixing speed is 450r/min, and temperature is 40 DEG C, and mixing time is 40min;
(2) in above-mentioned steps (1), add butanol phosphate antistatic additive to stir at 25 DEG C, mixing speed is 860r/min, and mixing time is 55min, namely obtains fabric lining composite antistatic agent.
embodiment 2
The present embodiment provides a kind of preparation method of fabric lining composite antistatic agent, and in this preparation method, fabric lining composite antistatic agent comprises following component according to the mass fraction:
Butanol phosphate antistatic additive: 35 parts, superbrnaching end-hydroxy antistatic additive: 5 parts, end carboxyl super branched anti-antistatic additive: 10 parts, the hyperbranched antistatic additive of end quaternary ammonium salt: 25 parts;
The concrete preparation method of this fabric lining composite antistatic agent is as follows:
(1) preparation of butanol phosphate antistatic additive
(1) joined in clean there-necked flask by n-butanol, then add phosphorus pentoxide, slowly put in the there-necked flask of n-butanol with spoon, there-necked flask is placed on and is equipped with in the large beaker of cold water, is no more than 50 DEG C to control its temperature in adition process;
The mol ratio of n-butanol and phosphorus pentoxide is 3.5:1;
(2) finished, respectively with plug, with thermometer plug, there-necked flask is sealed, there-necked flask is fixed on electric mixer, and puts into the modulated thermostat water bath to 70 DEG C, when thermometer registration is 70 DEG C, start timing, accurately pipette deionized water with pipette after reaction 4h to add there-necked flask and be hydrolyzed, hydrolysis time is 3h, after reaction terminates, and cooling, take out product, namely obtain butanol phosphate antistatic additive;
The amount adding deionized water is 5% of n-butanol and five oxidation two mound gross masses;
(2) preparation of superbrnaching end-hydroxy antistatic additive
(1) chlorinated dodecane is dissolved in absolute ethyl alcohol, add in there-necked flask, stirring is warming up to 70 DEG C, be dissolved in ethanol and drip in there-necked flask getting diethanol amine, stirring, add sodium hydroxid powder, be warming up to backflow to produce, insulation reaction 5h, decompression distillation after thick product of purifying to obtain, obtains core molecule;
The mass ratio wherein adding chlorinated dodecane, diethanol amine and NaOH is 10:1:0.4;
(2) by diethanol amine and succinic anhydride, be dissolved in respectively in DMA, diethanolamine solution added in there-necked flask, be warming up to 30 DEG C, slowly add succinic anhydride, dropwise in control 1h, react 3h at 26 DEG C, obtain monomer.
Wherein, the mass ratio adding diethanol amine and succinic anhydride is 1.03:1;
(3) obtained core molecule is joined prepare in the reactor of monomer, mixing and stirring, adds toluene and makes water entrainer, is adding catalyst toluenesulfonic acid, connect water knockout drum, agitating heating is until there is backflow to produce, and insulation reaction 3h, until anhydrous generation in water entrainer toluene, decompression distillation is carried out to product, except desolventizing, obtain a kind of faint yellow thick substances, i.e. superbrnaching end-hydroxy antistatic additive;
(3) preparation of carboxyl super branched anti-antistatic additive
Superbrnaching end-hydroxy antistatic additive obtained in step (two) is dissolved in N, in N-dimethylacetylamide, dissolve succinic anhydride with DMA, add DMAP, temperature is controlled at 85 DEG C, continuous stirring, mixing speed controls at 250r/min, drips succinic anhydride solution, reaction 6h, namely obtains end carboxyl super branched antistatic additive;
Wherein, superbrnaching end-hydroxy antistatic additive and succinic anhydride mass ratio be 7:1.3;
(4) preparation of the hyperbranched antistatic additive of quaternary ammonium salt is held
(1) the superbrnaching end-hydroxy antistatic additive of preparation in (two) is dissolved in DMA, adds in four-hole boiling flask, stir under nitrogen protection, add sodium hydroxid and epoxychloropropane, be warmed up to 45 DEG C, mixing speed is 300r/min, reaction 6h;
(2) product of reaction in above-mentioned steps (1) is filtered, getting worry liquid adds in four-hole boiling flask, stirred under nitrogen atmosphere is warming up to 65 DEG C, slow dropping triethylamine, reaction 5h, decompression distillation removes desolventizing and unreacted raw material, by further for product of distillation purification processes, dry 24h in 30 DEG C of vacuum drying chambers, namely obtain the hyperbranched antistatic additive of end quaternary ammonium salt;
Wherein, the mass ratio adding sodium hydroxid and epoxychloropropane is 13:18;
(5) the mixed system of fabric lining composite antistatic agent
(1) superbrnaching end-hydroxy antistatic additive, end carboxyl super branched anti-antistatic additive, end quaternary ammonium salt hyperbranched antistatic additive added in dispersion cylinder and stir, mixing speed is 400r/min, and temperature is 45 DEG C, and mixing time is 30min;
(2) in above-mentioned steps (1), add butanol phosphate antistatic additive to stir at 30 DEG C, mixing speed is 800r/min, and mixing time is 50min, namely obtains fabric lining composite antistatic agent.
embodiment 3
The present embodiment provides a kind of preparation method of fabric lining composite antistatic agent, and in this preparation method, fabric lining composite antistatic agent comprises following component according to the mass fraction:
Butanol phosphate antistatic additive: 38 parts, superbrnaching end-hydroxy antistatic additive: 10 parts, end carboxyl super branched anti-antistatic additive: 13 parts, the hyperbranched antistatic additive of end quaternary ammonium salt: 20 parts;
The concrete preparation method of this fabric lining composite antistatic agent is as follows:
(1) preparation of butanol phosphate antistatic additive
(1) joined in clean there-necked flask by n-butanol, then add phosphorus pentoxide, slowly put in the there-necked flask of n-butanol with spoon, there-necked flask is placed on and is equipped with in the large beaker of cold water, is no more than 50 DEG C to control its temperature in adition process;
The mol ratio of n-butanol and phosphorus pentoxide is 3.5:1;
(2) finished, respectively with plug, with thermometer plug, there-necked flask is sealed, there-necked flask is fixed on electric mixer, and puts into the modulated thermostat water bath to 70 DEG C, when thermometer registration is 70 DEG C, start timing, accurately pipette deionized water with pipette after reaction 4h to add there-necked flask and be hydrolyzed, hydrolysis time is 2h, after reaction terminates, and cooling, take out product, namely obtain butanol phosphate antistatic additive;
The amount adding deionized water is 4% of n-butanol and five oxidation two mound gross masses;
(2) preparation of superbrnaching end-hydroxy antistatic additive
(1) chlorinated dodecane is dissolved in absolute ethyl alcohol, add in there-necked flask, stirring is warming up to 80 DEG C, be dissolved in ethanol and drip in there-necked flask getting diethanol amine, stirring, add sodium hydroxid powder, be warming up to backflow to produce, insulation reaction 4h, decompression distillation after thick product of purifying to obtain, obtains core molecule;
The mass ratio wherein adding chlorinated dodecane, diethanol amine and NaOH is 10:1:0.4;
(2) by diethanol amine and succinic anhydride, be dissolved in respectively in DMA, diethanolamine solution added in there-necked flask, be warming up to 30 DEG C, slowly add succinic anhydride, dropwise in control 1h, react 3h at 30 DEG C, obtain monomer.
Wherein, the mass ratio adding diethanol amine and succinic anhydride is 1.03:1;
(3) obtained core molecule is joined prepare in the reactor of monomer, mixing and stirring, adds toluene and makes water entrainer, is adding catalyst toluenesulfonic acid, connect water knockout drum, agitating heating is until there is backflow to produce, and insulation reaction 4h, until anhydrous generation in water entrainer toluene, decompression distillation is carried out to product, except desolventizing, obtain a kind of faint yellow thick substances, i.e. superbrnaching end-hydroxy antistatic additive;
(3) preparation of carboxyl super branched anti-antistatic additive
Superbrnaching end-hydroxy antistatic additive obtained in step (two) is dissolved in N, in N-dimethylacetylamide, dissolve succinic anhydride with DMA, add DMAP, temperature is controlled at 83 DEG C, continuous stirring, mixing speed controls at 220r/min, drips succinic anhydride solution, reaction 6h, namely obtains end carboxyl super branched antistatic additive;
Wherein, superbrnaching end-hydroxy antistatic additive and succinic anhydride mass ratio be 7:1.3;
(4) preparation of the hyperbranched antistatic additive of quaternary ammonium salt is held
(1) the superbrnaching end-hydroxy antistatic additive of preparation in (two) is dissolved in DMA, adds in four-hole boiling flask, stir under nitrogen protection, add sodium hydroxid and epoxychloropropane, be warmed up to 45 DEG C, mixing speed is 320r/min, reaction 6h;
(2) product of reaction in above-mentioned steps (1) is filtered, getting worry liquid adds in four-hole boiling flask, stirred under nitrogen atmosphere is warming up to 65 DEG C, slow dropping triethylamine, reaction 5h, decompression distillation removes desolventizing and unreacted raw material, by further for product of distillation purification processes, dry 24h in 30 DEG C of vacuum drying chambers, namely obtain the hyperbranched antistatic additive of end quaternary ammonium salt;
Wherein, the mass ratio adding sodium hydroxid and epoxychloropropane is 13:18;
(5) the mixed system of fabric lining composite antistatic agent
(1) by superbrnaching end-hydroxy antistatic additive, end carboxyl super branched 500r/min, temperature is 42 DEG C, and mixing time is 50min;
(2) in above-mentioned steps (1), add butanol phosphate antistatic additive to stir at 28 DEG C, mixing speed is 900r/min, and mixing time is 60min, namely obtains fabric lining composite antistatic agent.
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of application claims.
Claims (3)
1. a preparation method for fabric lining composite antistatic agent, is characterized in that, in this preparation method, fabric lining composite antistatic agent comprises following component according to the mass fraction:
Butanol phosphate antistatic additive 35-40 part
Superbrnaching end-hydroxy antistatic additive 5-10 part
End carboxyl super branched anti-antistatic additive 10-15 part
End quaternary ammonium salt hyperbranched antistatic additive 20-25 part
The concrete preparation method of this fabric lining composite antistatic agent is as follows:
(1) preparation of butanol phosphate antistatic additive
(1) joined in clean there-necked flask by n-butanol, then add phosphorus pentoxide, slowly put in the there-necked flask of n-butanol with spoon, there-necked flask is placed on and is equipped with in the large beaker of cold water, is no more than 50 DEG C to control its temperature in adition process;
(2) finished, respectively with plug, with thermometer plug, there-necked flask is sealed, there-necked flask is fixed on electric mixer, and puts into the modulated thermostat water bath to 70 DEG C, when thermometer registration is 70 DEG C, start timing, accurately pipette deionized water with pipette after reaction 4h to add there-necked flask and be hydrolyzed, hydrolysis time is 2-3h, after reaction terminates, and cooling, take out product, namely obtain butanol phosphate antistatic additive;
(2) preparation of superbrnaching end-hydroxy antistatic additive
(1) chlorinated dodecane is dissolved in absolute ethyl alcohol, add in there-necked flask, stirring is warming up to 70-80 DEG C, be dissolved in ethanol and drip in there-necked flask getting diethanol amine, stirring, add sodium hydroxid powder, be warming up to backflow to produce, insulation reaction 4-5h, decompression distillation after thick product of purifying to obtain, obtains core molecule;
The wherein said mass ratio adding chlorinated dodecane, diethanol amine and NaOH is 10:1:0.4;
(2) by diethanol amine and succinic anhydride, be dissolved in respectively in DMA, diethanolamine solution added in there-necked flask, be warming up to 30 DEG C, slowly add succinic anhydride, dropwise in control 1h, react 3h at 26-30 DEG C, obtain monomer;
Wherein, the mass ratio adding diethanol amine and succinic anhydride is 1.03:1;
(3) obtained core molecule is joined prepare in the reactor of monomer, mixing and stirring, adds toluene and makes water entrainer, is adding catalyst, connect water knockout drum, agitating heating is until there is backflow to produce, and insulation reaction 3-4h, until anhydrous generation in water entrainer toluene, decompression distillation is carried out to product, except desolventizing, obtain a kind of faint yellow thick substances, i.e. superbrnaching end-hydroxy antistatic additive;
(3) preparation of carboxyl super branched anti-antistatic additive
Superbrnaching end-hydroxy antistatic additive obtained in step (two) is dissolved in N, in N-dimethylacetylamide, dissolve succinic anhydride with DMA, add DMAP, temperature is controlled at 80-85 DEG C, continuous stirring, mixing speed controls at 200-250r/min, drips succinic anhydride solution, reaction 5-6h, namely obtains end carboxyl super branched antistatic additive;
Wherein, described superbrnaching end-hydroxy antistatic additive and succinic anhydride mass ratio be 7:1.3;
(4) preparation of the hyperbranched antistatic additive of quaternary ammonium salt is held
(1) the superbrnaching end-hydroxy antistatic additive of preparation in (two) is dissolved in DMA, adds in four-hole boiling flask, stir under nitrogen protection, add sodium hydroxid and epoxychloropropane, be warmed up to 45 DEG C, mixing speed is 300-350r/min, reaction 5-6h;
(2) product of reaction in above-mentioned steps (1) is filtered, getting worry liquid adds in four-hole boiling flask, stirred under nitrogen atmosphere is warming up to 65 DEG C, slow dropping triethylamine, reaction 5-6h, decompression distillation removes desolventizing and unreacted raw material, by further for product of distillation purification processes, dry 24h in 30 DEG C of vacuum drying chambers, namely obtain the hyperbranched antistatic additive of end quaternary ammonium salt;
Wherein, the described mass ratio adding sodium hydroxid and epoxychloropropane is 13:18;
(5) the mixed system of fabric lining composite antistatic agent
(1) superbrnaching end-hydroxy antistatic additive, end carboxyl super branched anti-antistatic additive, end quaternary ammonium salt hyperbranched antistatic additive added in dispersion cylinder and stir, mixing speed is 400-500r/min, and temperature is 40-45 DEG C, and mixing time is 30-50min;
(2) in above-mentioned steps (1), add butanol phosphate antistatic additive to stir at 25-30 DEG C, mixing speed is 800-900r/min, and mixing time is 50-60min, namely obtains fabric lining composite antistatic agent.
2. the preparation method of fabric lining composite antistatic agent according to claim 1, is characterized in that: when preparing butanol phosphate antistatic additive, the mol ratio of described n-butanol and phosphorus pentoxide is 3.5:1; The described amount adding deionized water is the 4-6% of n-butanol and five oxidation two mound gross masses.
3. the preparation method of fabric lining composite antistatic agent according to claim 1, is characterized in that: when prepared by superbrnaching end-hydroxy antistatic additive, and catalyst used is toluenesulfonic acid.
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