CN105133331B - A kind of anti-soda acid finishing agent and its preparation method and application - Google Patents
A kind of anti-soda acid finishing agent and its preparation method and application Download PDFInfo
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- CN105133331B CN105133331B CN201510710857.7A CN201510710857A CN105133331B CN 105133331 B CN105133331 B CN 105133331B CN 201510710857 A CN201510710857 A CN 201510710857A CN 105133331 B CN105133331 B CN 105133331B
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Abstract
The invention discloses a kind of anti-soda acid finishing agent and its preparation method and application, it comprises the component of following weight concentration meter: waterproof oil-proof finishing agent 80 ~ 120g/L, reinforcing agent 30 ~ 60g/L and film forming catalyst 10 ~ 20g/L; Described waterproof oil-proof finishing agent is prepared from by following raw material: acrylic acid ten trifluoro monooctyl ester, octadecyl acrylate, n-methylolacrylamide, vinylidene chloride, emulsifying agent, cosolvent, initator and water; Described reinforcing agent is oxidized polyethylene wax emulsion; Described film forming catalyst is prepared from by following raw material: isocyanate trimer, terminal methyl polyethylene glycol, sealer, organic solvent and water.The present invention's anti-soda acid finishing agent good film-forming property, pressure resistance, can prevent from, by the wetting of acid & alkali liquid and various chemical substance and infiltration, can resisting the erosion of strong acid, highly basic, strong oxidizer, and have the advantages such as ventilative comfortable, soft light, easy washing concurrently.
Description
Technical field
The invention belongs to printing and dyeing assistant technical field, be specifically related to a kind of anti-soda acid finishing agent and its preparation method and application.
Background technology
Labourer is being engaged in production, is carrying, is toppling over, is modulating soda acid; repair or clean in the vocational activities such as chemical devices; all likely cause the burn caused by the chemical substances such as strong acid, highly basic, phosphorus and hydrofluoric acid; wear suitable chemical protecting suit; can effectively intercept the harmful chemical such as inorganic acid, alkali; make it can not with skin contact, the personal safety of operating personnel can be protected to greatest extent.
Traditional anti-soda acid Work Clothes is in base fabrics, be coated with the fluid-tight rubber of one deck or plastic coating agent, plays the effect preventing acid & alkali liquid from permeating.There is heavy, airtight, not moisture-inhibiting in this acid-proof fabric, and the heavy inconvenience of whole clothes, comfortableness extreme difference.The labourer wearing anti-soda acid Work Clothes natively operates when working environment is more severe, and the protective clothing of this comfortableness extreme difference is obviously very disadvantageous to the health of operator and operating efficiency.Market also has the anti-soda acid clothes of vapor-permeable type, but due to barrier propterty poor, can only acid strength be applicable to low, the occasion of discontinuous work, not be suitable for the situation of continuous operation under strong acid and strong base.
Chinese patent application CN103694484A discloses a kind of water-based fluorocarbon fabric three-proof finishing agent, it comprises monomer (perfluorinated acrylate, lauryl acid esters, n-methylolacrylamide etc.), initator, softening agent and crosslinking and curing agent, described crosslinking and curing agent for disclosed in Chinese patent application CN103668957A by two hydroxyl fluorine ether (HO-R
f-OH) under sealer, react obtained, this finishing agent water resistant oil resistant with diisocyanate monomer, water-fastness, but its anti-Acidity of Aikalinity can be poor.
In sum, be necessary to research and develop a kind of anti-soda acid finishing agent, it can form diaphragm at fabric face, can prevent the erosion of the number of chemical materials such as strong acid, highly basic, strong oxidizer, and has the advantages such as ventilative comfortable, soft light, easy washing concurrently.
Summary of the invention
In order to overcome the deficiencies in the prior art; the object of the present invention is to provide a kind of anti-soda acid finishing agent and preparation method thereof; this anti-soda acid finishing agent good film-forming property; can be formed evenly at fabric face, fine and close, chemically inert diaphragm; wetting and the infiltration by acid & alkali liquid and various chemical substance can be prevented; the erosion of strong acid, highly basic, strong oxidizer can be resisted, and have the advantages such as ventilative comfortable, soft light, easy washing concurrently.
To achieve these goals, technical scheme of the present invention is as follows:
A kind of anti-soda acid finishing agent, comprises the component of following weight concentration meter: waterproof oil-proof finishing agent 80 ~ 120g/L, reinforcing agent 30 ~ 60g/L and film forming catalyst 10 ~ 20g/L;
Described waterproof oil-proof finishing agent is prepared from by the raw material of following weight portion: acrylic acid ten trifluoro monooctyl ester 110 ~ 130 parts, octadecyl acrylate 110 ~ 130 parts, n-methylolacrylamide 3 ~ 6 parts, vinylidene chloride 50 ~ 70 parts, emulsifying agent 40 ~ 50 parts, cosolvent 90 ~ 110 parts, initator 0.5 ~ 0.7 part and 450 ~ 550 parts, water;
Described reinforcing agent is oxidized polyethylene wax emulsion;
Described film forming catalyst is prepared from by the raw material of following weight portion: isocyanate trimer 90 ~ 110 parts, terminal methyl polyethylene glycol 20 ~ 30 parts, sealer 40 ~ 60 parts, organic solvent 10 ~ 20 parts and 350 ~ 400 parts, water.
Further, described emulsifying agent is the composition of fatty alcohol-polyoxyethylene ether AEO9 and octadecyl trimethyl ammonium chloride, and the weight ratio of described fatty alcohol-polyoxyethylene ether AEO9 and octadecyl trimethyl ammonium chloride is 2:1.
Further, described cosolvent is butyl or dipropylene.
Further, described initator is ammonium persulfate or azo two NSC 18620.
Further, described terminal methyl polyethylene glycol is at least one in terminal methyl polyethylene glycol MPEG500, terminal methyl polyethylene glycol MPEG1000 and terminal methyl polyethylene glycol MPEG2000.
Further, described sealer is silane resin acceptor kh-550, sodium hydrogensulfite or diacetylmonoxime.
Further, described organic solvent is acetone or butanone.
The preparation method of the anti-soda acid finishing agent of the present invention comprises the following steps:
(1) preparation of waterproof oil-proof finishing agent:
S1, initator is mixed with the initiator solution that mass concentration is 10%, for subsequent use; Add water toward emulsifying agent, be warming up to 75 ~ 85 DEG C, stirring and dissolving 30min, obtain emulsifier solution;
S2, get emulsifier solution described in 3/5, add acrylic acid ten trifluoro monooctyl ester, octadecyl acrylate, n-methylolacrylamide and vinylidene chloride, at 25 ~ 35 DEG C of emulsification 50 ~ 60min, emulsification is complete, obtains pre-emulsion, for subsequent use;
S3, get emulsifier solution described in 2/5 put into band reflux condenser reactor, add pre-emulsion described in 1/10, be warming up to 70 ~ 80 DEG C, add described initiator solution 2 parts, insulation reaction 25 ~ 35min;
S4, be warming up to 80 ~ 85 DEG C, drip pre-emulsion described in 9/10 and dropwise in 110 ~ 130min, described initiator solution 0.5 part is dripped every 15min while dripping described pre-emulsion, described pre-emulsion dropwises rear insulation 25 ~ 35min, be down to room temperature, filter discharging and namely obtain waterproof oil-proof finishing agent;
(2) preparation of film forming catalyst:
Terminal methyl polyethylene glycol is added at the upper still of synthesis device, maintain the temperature at more than 30 DEG C, lower still adds isocyanate trimer, organic solvent and dibutyl tin laurate, open and stir, lower still is heated to 55 ~ 65 DEG C, still material in dropping, use cooling water control temperature at 55 ~ 65 DEG C in dropping process, time for adding controls in 0.5 ~ 3h, insulation reaction 1.5 ~ 2.5h, heat up 75 ~ 85 DEG C, add sealer, insulation reaction 30 ~ 120min, be cooled to room temperature, water is added under stirring, add water complete, continue stirring 30 ~ 40min, filter discharging and namely obtain film forming catalyst,
(3) preparation of anti-soda acid finishing agent:
According to weight concentration meter, waterproof oil-proof finishing agent 80 ~ 120g/L, reinforcing agent 30 ~ 60g/L, film forming catalyst 10 ~ 20g/L, get reinforcing agent and mix with described waterproof oil-proof finishing agent, film forming catalyst, add water, stir and get final product.
Further, the addition of described dibutyl tin laurate is 0.010 ~ 0.014% of isocyanate trimer weight.
The anti-soda acid mechanism of the present invention's anti-soda acid finishing agent with refuse water, to refuse oily preventing principle substantially identical, namely the surface tension of fabric is reduced, increase contact angle, prevent wetted and infiltration, but the water and oil repellent agent of routine is because it is reactive and film forming is poor, easily cause fabric face film forming uneven, easily permeated, so be difficult to reach good anti-soda acid effect.Therefore, the present invention have developed a kind of new waterproof oil-proof finishing agent, it is with acrylic acid ten trifluoro monooctyl ester, octadecyl acrylate, n-methylolacrylamide and vinylidene chloride copolymerization, obtain that there is the good Organic fluoride emulsion being reacted into film properties, after crosslinked film forming, form low surface tension state, effectively prevent the wetting and infiltration of soda acid and various chemicals.
In order to strengthen the performance of described waterproof oil-proof finishing agent further, the present invention uses oxidized polyethylene wax emulsion as reinforcing agent, develops a kind of film forming catalyst simultaneously.Oxidized polyethylene wax emulsion is a kind of nano-high molecule polymer emulsion of nucleocapsid structure, there is the shell of antiacid alkali functional group formation and the internal layer multipolymer structure of film forming densification, itself and described waterproof oil-proof finishing agent are cross-linked, and form the cooperative effect of acid-fast alkali-proof and resistance to various chemicals; Can in fabric face uniform spreading when high temperature bakes, in subsequent cooling process, its special kernel nanostructured forms state of aggregation Microphase Separation, shows as film formation surface uneven, considerably increases fabric specific area.Film forming catalyst of the present invention terminal methyl polyethylene glycol under the catalysis of dibutyl tin laurate is polymerized with isocyanate trimer; stable under forming a kind of normal temperature; there is the special polyurethanes compound of height reactivity under specific temperature conditions; it can promote that described waterproof oil-proof finishing agent and oxidized polyethylene wax emulsion are cross-linked further, works in coordination with the reticular protection film forming strong mechanical performance and high chemical stability on fabric simultaneously.
Simultaneously, present invention also offers the application of above-mentioned anti-soda acid finishing agent in protective clothing, it can be used for arranging the multiple fabrics such as cotton textiles, polyester-cotton blend, Polyester Taffeta and nylon tower husband, significantly improve the function such as resistance to acid fracturing, strong acid-base resistance of fabric, the fabric through the process of the present invention's anti-soda acid finishing agent can be made into protective clothing and is widely used in the various special chemical fields such as military project, medical treatment, oil field.
Therefore, compared with prior art, advantage of the present invention is:
(1) waterproof oil-proof finishing agent of the present invention and reinforcing agent and film forming catalyst three kinds of components organically combine, the anti-soda acid finishing agent formed can form special nano-micro structure rough surface at fabric face, produce huge specific surface energy, obtain the hydrophobic state tension force having larger contact angle, increase contact angle, effectively prevent the wetting and infiltration by acid & alkali liquid and various chemical substance; Simultaneously even, fine and close owing to forming chemically inert diaphragm; the erosion of strong acid, highly basic, strong oxidizer etc. can be resisted; fabric after this product treatment can effectively avoid acid & alkali liquid to the splash of human body and infiltration; there is the acidproof time long; the premium properties that resistance to acid fracturing is high; have air-moisture-permeable concurrently; snugness of fit is good, softness is light, easy washing and wash resistant etc. are functional and the advantage of comfortableness; can be applicable in protective clothing, be widely used in the various special chemical fields such as military project, medical treatment, oil field.
(2) the anti-soda acid finishing agent of the present invention is not containing APEO, can be applicable to the multiple fabrics such as cotton textiles, polyester-cotton blend, Polyester Taffeta and nylon tower husband, still can meet Oeko-TexStandard100 standard after fabric treating; And the present invention's anti-soda acid finishing agent good film-forming property, excellent performance, stable preparation process, condition are easily controlled, and have good application prospect.
Detailed description of the invention
Below by embodiment, the present invention will be described, but the present invention is not limited to these embodiments.
Oxidized polyethylene wax emulsion described in the embodiment of the present invention is the product P oligenWE6 of German BASF group.Described isocyanate trimer is the product B asonat HI100 of German BASF group.
Embodiment 1, the anti-soda acid finishing agent of the present invention and preparation thereof
The present embodiment anti-soda acid finishing agent is made up of the component of following weight concentration meter: waterproof oil-proof finishing agent 80g/L, reinforcing agent 30g/L and film forming catalyst 10g/L;
Described waterproof oil-proof finishing agent is prepared from by the raw material of following weight portion: acrylic acid ten trifluoro monooctyl ester 110kg, octadecyl acrylate 130kg, n-methylolacrylamide 6kg, vinylidene chloride 70kg, emulsifying agent 40kg(fatty alcohol-polyoxyethylene ether AEO9 and octadecyl trimethyl ammonium chloride mix by weight 2:1), butyl 110kg, ammonium persulfate 0.6kg and water 450kg;
Described reinforcing agent is oxidized polyethylene wax emulsion.
Described film forming catalyst is prepared from by the raw material of following weight portion: isocyanate trimer 90kg, terminal methyl polyethylene glycol MPEG50030kg, silane resin acceptor kh-550 40kg, acetone 20kg and water 350kg.
The preparation method of the present embodiment anti-soda acid finishing agent is as follows:
(1) preparation of waterproof oil-proof finishing agent:
S1, ammonium persulfate is mixed with the ammonium persulfate aqueous solution that mass concentration is 10%, for subsequent use; Add water toward emulsifying agent, be warming up to 75 DEG C, stirring and dissolving 30min, obtain emulsifier solution;
S2, get emulsifier solution described in 3/5, add acrylic acid ten trifluoro monooctyl ester, octadecyl acrylate, n-methylolacrylamide and vinylidene chloride, at 25 DEG C of emulsification 60min, emulsification is complete, obtains pre-emulsion, for subsequent use;
S3, get emulsifier solution described in 2/5 put into band reflux condenser reactor, add pre-emulsion described in 1/10, be warming up to 70 DEG C, add described ammonium persulfate aqueous solution 2kg, insulation reaction 35min;
S4, be warming up to 80 DEG C, drip pre-emulsion described in 9/10 and dropwise in 110min, drip described initiator solution 0.5kg every 15min while dripping described pre-emulsion, described pre-emulsion dropwises rear insulation 35min, be down to room temperature, filter discharging and namely obtain waterproof oil-proof finishing agent;
(2) preparation of film forming catalyst:
Terminal methyl polyethylene glycol MPEG500 is added at the upper still of synthesis device, maintain the temperature at more than 30 DEG C, lower still adds isocyanate trimer, the dibutyl tin laurate of acetone and isocyanate trimer weight 0.010%, open and stir, lower still is heated to 55 DEG C, still material in dropping, use cooling water control temperature at 55 DEG C in dropping process, time for adding controls in 3h, insulation reaction 1.5h, heat up 75 DEG C, add silane resin acceptor kh-550, insulation reaction 50min, test free NCO content simultaneously, and calculate free NCO content, free NCO content < 1%, be cooled to room temperature, add water under vigorous stirring, add water complete, continue to stir 30min, filter discharging and namely obtain film forming catalyst,
(3) preparation of anti-soda acid finishing agent:
According to weight concentration meter, waterproof oil-proof finishing agent 80g/L, reinforcing agent 30g/L, film forming catalyst 10g/L, get reinforcing agent and mix with described waterproof oil-proof finishing agent, film forming catalyst, add water, stir and get final product.
Embodiment 2, the anti-soda acid finishing agent of the present invention and preparation thereof
The present embodiment anti-soda acid finishing agent is made up of the component of following weight concentration meter: waterproof oil-proof finishing agent 120g/L, reinforcing agent 60g/L and film forming catalyst 20g/L;
Described waterproof oil-proof finishing agent is prepared from by the raw material of following weight portion: acrylic acid ten trifluoro monooctyl ester 130kg, octadecyl acrylate 110kg, n-methylolacrylamide 3kg, vinylidene chloride 50kg, emulsifying agent 50kg(fatty alcohol-polyoxyethylene ether AEO9 and octadecyl trimethyl ammonium chloride mix by weight 2:1), dipropylene 90kg, azo two NSC 18620 0.65kg and water 550kg;
Described reinforcing agent is oxidized polyethylene wax emulsion.
Described film forming catalyst is prepared from by the raw material of following weight portion: isocyanate trimer 110kg, terminal methyl polyethylene glycol MPEG200020kg, sodium hydrogensulfite 60kg, butanone 10kg and water 400kg.
The preparation method of the present embodiment anti-soda acid finishing agent is as follows:
(1) preparation of waterproof oil-proof finishing agent:
S1, azo two NSC 18620 is mixed with the azo two NSC 18620 aqueous solution that mass concentration is 10%, for subsequent use; Add water toward emulsifying agent, be warming up to 85 DEG C, stirring and dissolving 30min, obtain emulsifier solution;
S2, get emulsifier solution described in 3/5, add acrylic acid ten trifluoro monooctyl ester, octadecyl acrylate, n-methylolacrylamide and vinylidene chloride, at 35 DEG C of emulsification 50min, emulsification is complete, obtains pre-emulsion, is down to room temperature, for subsequent use;
S3, get emulsifier solution described in 2/5 put into band reflux condenser reactor, add pre-emulsion described in 1/10, be warming up to 80 DEG C, add described initiator solution 2kg, insulation reaction 25min;
S4, be warming up to 85 DEG C, drip pre-emulsion described in 9/10 and dropwise in 130min, drip described initiator solution 0.5kg every 15min while dripping described pre-emulsion, described pre-emulsion dropwises rear insulation 25min, be down to room temperature, filter discharging and namely obtain waterproof oil-proof finishing;
(2) preparation of film forming catalyst:
Sodium hydrogensulfite uses 200kg water fully to dissolve, and obtains solution of sodium bisulfite.Terminal methyl polyethylene glycol MPEG2000 is added at the upper still of synthesis device, maintain the temperature at more than 30 DEG C, lower still adds isocyanate trimer, the dibutyl tin laurate of butanone and isocyanate trimer weight 0.014%, open and stir, lower still is heated to 65 DEG C, still material in dropping, use cooling water control temperature at 65 DEG C in dropping process, time for adding controls in 0.5h, insulation reaction 2.5h, heat up 85 DEG C, add described solution of sodium bisulfite, insulation reaction 120min, test free NCO content simultaneously, and calculate free NCO content, free NCO content < 1%, be cooled to room temperature, add 200kg water under vigorous stirring, add water complete, continue to stir 40min, filter discharging and namely obtain film forming catalyst,
(3) preparation of anti-soda acid finishing agent:
According to weight concentration meter, waterproof oil-proof finishing agent 120g/L, reinforcing agent 60g/L, film forming catalyst 20g/L, get reinforcing agent and mix with described waterproof oil-proof finishing agent, film forming catalyst, add water, stir and get final product.
Embodiment 3, the anti-soda acid finishing agent of the present invention and preparation thereof
The present embodiment anti-soda acid finishing agent is made up of the component of following weight concentration meter: waterproof oil-proof finishing agent 100g/L, reinforcing agent 50g/L and film forming catalyst 15g/L;
Described waterproof oil-proof finishing agent is prepared from by the raw material of following weight portion: acrylic acid ten trifluoro monooctyl ester 120kg, octadecyl acrylate 120kg, n-methylolacrylamide 5kg, vinylidene chloride 60kg, emulsifying agent 45kg(fatty alcohol-polyoxyethylene ether AEO9 and octadecyl trimethyl ammonium chloride mix by weight 2:1), butyl 100kg, ammonium persulfate 0.65kg and water 500kg;
Described reinforcing agent is oxidized polyethylene wax emulsion.
Described film forming catalyst is prepared from by the raw material of following weight portion: isocyanate trimer 100kg, terminal methyl polyethylene glycol MPEG100025kg, diacetylmonoxime 50kg, butanone 15kg and water 380kg.
The preparation method of the present embodiment anti-soda acid finishing agent is as follows:
(1) preparation of waterproof oil-proof finishing agent:
S1, ammonium persulfate is mixed with the ammonium persulfate aqueous solution that mass concentration is 10%, for subsequent use; Add water toward emulsifying agent, be warming up to 80 DEG C, stirring and dissolving 30min, obtain emulsifier solution;
S2, get emulsifier solution described in 3/5, add acrylic acid ten trifluoro monooctyl ester, octadecyl acrylate, n-methylolacrylamide and vinylidene chloride, at 30 DEG C of emulsification 60min, emulsification is complete, obtains pre-emulsion, is down to room temperature, for subsequent use;
S3, get emulsifier solution described in 2/5 put into band reflux condenser reactor, add pre-emulsion described in 1/10, be warming up to 75 DEG C, add described initiator solution 2kg, insulation reaction 30min;
S4, be warming up to 80 DEG C, drip pre-emulsion described in 9/10 and dropwise in 120min, drip described initiator solution 0.5kg every 15min while dripping described pre-emulsion, described pre-emulsion dropwises rear insulation 30min, be down to room temperature, filter discharging and namely obtain waterproof oil-proof finishing agent;
(2) preparation of film forming catalyst:
Terminal methyl polyethylene glycol MPEG1000 is added at the upper still of synthesis device, maintain the temperature at more than 30 DEG C, lower still adds isocyanate trimer, the dibutyl tin laurate of butanone and isocyanate trimer weight 0.014%, open and stir, lower still is heated to 60 DEG C, still material in dropping, use cooling water control temperature at 60 DEG C in dropping process, time for adding controls in 2h, insulation reaction 2h, heat up 80 DEG C, add diacetylmonoxime, insulation reaction 30min, test free NCO content simultaneously, and calculate free NCO content, free NCO content < 1%, be cooled to room temperature, add water under vigorous stirring, add water complete, continue to stir 30min, filter discharging and namely obtain film forming catalyst,
(3) preparation of anti-soda acid finishing agent:
According to weight concentration meter, waterproof oil-proof finishing agent 100g/L, reinforcing agent 50g/L, film forming catalyst 15g/L, get reinforcing agent and mix with described waterproof oil-proof finishing agent, film forming catalyst, add water, stir and get final product.
Comparative example 1
This comparative example finishing agent is made up of the component of following weight concentration meter: the crosslinking and curing agent 15g/L of embodiment 2 in waterproof oil-proof finishing agent 100g/L, reinforcing agent 50g/L and Chinese patent application CN103668957A description.Other are with embodiment 3.
Comparative example 2
This comparative example finishing agent is made up of the component of following weight concentration meter: waterproof oil-proof finishing agent 100g/L, reinforcing agent 50g/L and film forming catalyst 15g/L;
Described waterproof oil-proof finishing agent is prepared from by the raw material of following weight portion: acrylic acid ten trifluoro monooctyl ester 120kg, octadecyl acrylate 120kg, n-methylolacrylamide 5kg, fatty alcohol-polyoxyethylene ether AEO945kg, butyl 100kg, ammonium persulfate 0.65kg and water 500kg;
Described reinforcing agent is oxidized polyethylene wax emulsion.
Described film forming catalyst is prepared from by the raw material of following weight portion: toluene di-isocyanate(TDI) 100kg, terminal methyl polyethylene glycol MPEG100025kg, diacetylmonoxime 50kg, butanone 15kg and water 380kg.
Preparation method's reference example 3.
Comparative example 3
The formula of this comparative example finishing agent is with embodiment 3.
The preparation of the preparation method of this comparative example finishing agent (1) waterproof oil-proof finishing agent as different from Example 3:
S1, ammonium persulfate is mixed with the ammonium persulfate aqueous solution that mass concentration is 10%, for subsequent use; Add water toward emulsifying agent, be warming up to 80 DEG C, stirring and dissolving 30min, obtain emulsifier solution;
S2, get described emulsifier solution, add acrylic acid ten trifluoro monooctyl ester, octadecyl acrylate, n-methylolacrylamide and vinylidene chloride, at 30 DEG C of emulsification 60min, emulsification is complete, obtains pre-emulsion, is down to room temperature, for subsequent use;
S3, get pre-emulsion described in 1/10 put into band reflux condenser reactor, be warming up to 75 DEG C, add described initiator solution 2kg, insulation reaction 30min;
S4, be warming up to 80 DEG C, drip pre-emulsion described in 9/10 and dropwise in 120min, drip described initiator solution 0.5kg every 15min while dripping described pre-emulsion, described pre-emulsion dropwises rear insulation 30min, be down to room temperature, filter discharging and namely obtain waterproof oil-proof finishing agent; Other are with embodiment 3.
The performance test of test example, the anti-soda acid finishing agent of the present invention
Part I:
1, tested fabrics: T/C65/35
2, finishing agent is tested: the anti-soda acid finishing agent of the embodiment of the present invention 1 ~ 3, comparative example 1 ~ 3
3, treatment process a: leaching one is rolled, and 100 DEG C of oven dry, bake for 180 DEG C × 60 seconds
4, experimental technique: GB24540-2009 protective clothes acid-base class chemical protection takes
5, experimental result:
Part II:
1, tested fabrics: 100% cotton, 100% Polyester Taffeta and 100% nylon tower husband
2, finishing agent is tested: the anti-soda acid finishing agent of the embodiment of the present invention 3
3, treatment process a: leaching one is rolled, and 100 DEG C of oven dry, bake for 180 DEG C × 60 seconds
4, experimental technique: GB24540-2009 protective clothes acid-base class chemical protection takes
5, experimental result:
From the above-mentioned experimental result of this test example:
(1) the present invention's anti-soda acid finishing agent can significantly improve the function such as resistance to acid fracturing, strong acid-base resistance of fabric, long through the fabric strong acid-base resistance of the present invention's anti-soda acid finishing agent process, acid and alkali-resistance time of break-through, resistance to acid fracturing is high, wash resistant, its index of correlation all reaches and is even better than GB24540-2009 standard, wherein with the best performance of the anti-soda acid finishing agent of embodiment 3.
(2) the anti-soda acid finishing agent of the present invention can be applicable to the multiple fabrics such as cotton textiles, polyester-cotton blend, Polyester Taffeta and nylon tower husband, it is formed evenly at fabric face, fine and close, chemically inert reticular protection film, effectively avoid acid & alkali liquid to the splash of human body and infiltration, fabric face is bright and clean, smooth, flexible simultaneously, soft, air-moisture-permeable, comfortable and easy to wear; Fabric through the process of the present invention's anti-soda acid finishing agent can be widely used in the various special chemical fields such as military project, medical treatment, oil field.
(3) after testing, the anti-soda acid finishing agent of the present invention containing APEO, still can not meet Oeko-TexStandard100 standard after fabric treating.
(4) comparative example 1 uses existing crosslinking and curing agent to replace described film forming catalyst; Comparative example 2 is raw materials difference to some extent compared with embodiment 3; Comparative example 3 is compared with embodiment 3, and preparation method is different, and the performance of its obtained finishing agent, all than the difference of embodiment 1 ~ 3, also has part index number not reach relevant criterion.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (10)
1. an anti-soda acid finishing agent, is characterized in that, comprises the component of following weight concentration meter: waterproof oil-proof finishing agent 80 ~ 120g/L, reinforcing agent 30 ~ 60g/L and film forming catalyst 10 ~ 20g/L;
Described waterproof oil-proof finishing agent is prepared from by the raw material of following weight portion: acrylic acid ten trifluoro monooctyl ester 110 ~ 130 parts, octadecyl acrylate 110 ~ 130 parts, n-methylolacrylamide 3 ~ 6 parts, vinylidene chloride 50 ~ 70 parts, emulsifying agent 40 ~ 50 parts, cosolvent 90 ~ 110 parts, initator 0.5 ~ 0.7 part and 450 ~ 550 parts, water;
Described reinforcing agent is oxidized polyethylene wax emulsion;
Described film forming catalyst is prepared from by the raw material of following weight portion: isocyanate trimer 90 ~ 110 parts, terminal methyl polyethylene glycol 20 ~ 30 parts, sealer 40 ~ 60 parts, organic solvent 10 ~ 20 parts and 350 ~ 400 parts, water.
2. anti-soda acid finishing agent as claimed in claim 1, it is characterized in that, described emulsifying agent is the composition of fatty alcohol-polyoxyethylene ether AEO9 and octadecyl trimethyl ammonium chloride, and the weight ratio of described fatty alcohol-polyoxyethylene ether AEO9 and octadecyl trimethyl ammonium chloride is 2:1.
3. anti-soda acid finishing agent as claimed in claim 1, it is characterized in that, described cosolvent is butyl or dipropylene.
4. anti-soda acid finishing agent as claimed in claim 1, it is characterized in that, described initator is ammonium persulfate or azo two NSC 18620.
5. anti-soda acid finishing agent as claimed in claim 1, is characterized in that, described terminal methyl polyethylene glycol is at least one in terminal methyl polyethylene glycol MPEG500, terminal methyl polyethylene glycol MPEG1000 and terminal methyl polyethylene glycol MPEG2000.
6. anti-soda acid finishing agent as claimed in claim 1, it is characterized in that, described sealer is silane resin acceptor kh-550, sodium hydrogensulfite or diacetylmonoxime.
7. anti-soda acid finishing agent as claimed in claim 1, it is characterized in that, described organic solvent is acetone or butanone.
8. prepare as arbitrary in claim 1 ~ 7 as described in the method for anti-soda acid finishing agent, it is characterized in that, comprise the following steps:
(1) preparation of waterproof oil-proof finishing agent:
S1, initator is mixed with the initiator solution that mass concentration is 10%, for subsequent use; Add water toward emulsifying agent, be warming up to 75 ~ 85 DEG C, stirring and dissolving 30min, obtain emulsifier solution;
S2, get emulsifier solution described in 3/5, add acrylic acid ten trifluoro monooctyl ester, octadecyl acrylate, n-methylolacrylamide and vinylidene chloride, at 25 ~ 35 DEG C of emulsification 50 ~ 60min, emulsification is complete, obtains pre-emulsion, for subsequent use;
S3, get emulsifier solution described in 2/5 put into band reflux condenser reactor, add pre-emulsion described in 1/10, be warming up to 70 ~ 80 DEG C, add described initiator solution 2 parts, insulation reaction 25 ~ 35min;
S4, be warming up to 80 ~ 85 DEG C, drip pre-emulsion described in 9/10 and dropwise in 110 ~ 130min, described initiator solution 0.5 part is dripped every 15min while dripping described pre-emulsion, described pre-emulsion dropwises rear insulation 25 ~ 35min, be down to room temperature, filter discharging and namely obtain waterproof oil-proof finishing agent;
(2) preparation of film forming catalyst:
Terminal methyl polyethylene glycol is added at the upper still of synthesis device, maintain the temperature at more than 30 DEG C, lower still adds isocyanate trimer, organic solvent and dibutyl tin laurate, open and stir, lower still is heated to 55 ~ 65 DEG C, still material in dropping, use cooling water control temperature at 55 ~ 65 DEG C in dropping process, time for adding controls in 0.5 ~ 3h, insulation reaction 1.5 ~ 2.5h, heat up 75 ~ 85 DEG C, add sealer, insulation reaction 30 ~ 120min, be cooled to room temperature, water is added under stirring, add water complete, continue stirring 30 ~ 40min, filter discharging and namely obtain film forming catalyst,
(3) preparation of anti-soda acid finishing agent:
According to weight concentration meter, waterproof oil-proof finishing agent 80 ~ 120g/L, reinforcing agent 30 ~ 60g/L, film forming catalyst 10 ~ 20g/L, get reinforcing agent and mix with described waterproof oil-proof finishing agent, film forming catalyst, add water, stir and get final product.
9. the preparation method of anti-soda acid finishing agent as claimed in claim 8, it is characterized in that, the addition of described dibutyl tin laurate is 0.010 ~ 0.014% of isocyanate trimer weight.
10. the application of anti-soda acid finishing agent in protective clothing as claimed in claim 1.
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Effective date of registration: 20221228 Address after: No. 233, Langwan Road, Zhuhai City, Guangdong Province, 519000 Patentee after: Zhuhai Huada Haohong New Material Co.,Ltd. Address before: No. 10, Mingfeng 4th Road, Xiangzhou District, Zhuhai, Guangdong 519075 Patentee before: ZHUHAI HUADA-WHOLEWIN CHEMICAL LTD. |