CN106478745A - A kind of formaldehyde-free aqueous crosslinking agent and preparation method thereof and the finishing technique to fabric - Google Patents

A kind of formaldehyde-free aqueous crosslinking agent and preparation method thereof and the finishing technique to fabric Download PDF

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CN106478745A
CN106478745A CN201610899567.6A CN201610899567A CN106478745A CN 106478745 A CN106478745 A CN 106478745A CN 201610899567 A CN201610899567 A CN 201610899567A CN 106478745 A CN106478745 A CN 106478745A
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fabric
crosslinking agent
formaldehyde
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agent
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CN106478745B (en
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高介平
高辛格
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H9/00—Compounds containing a hetero ring sharing at least two hetero atoms with a saccharide radical
    • C07H9/02—Compounds containing a hetero ring sharing at least two hetero atoms with a saccharide radical the hetero ring containing only oxygen as ring hetero atoms
    • C07H9/04—Cyclic acetals
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D401/00—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom
    • C07D401/14—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing three or more hetero rings
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H1/00—Processes for the preparation of sugar derivatives
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/11—Compounds containing epoxy groups or precursors thereof
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/03—Polysaccharides or derivatives thereof
    • D06M15/13—Alginic acid or derivatives thereof
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/227—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of hydrocarbons, or reaction products thereof, e.g. afterhalogenated or sulfochlorinated
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • D06M15/647—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing polyether sequences
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/20—Treatment influencing the crease behaviour, the wrinkle resistance, the crease recovery or the ironing ease

Abstract

The invention belongs to shrinkproof, crease-resistant, the non-ironing technical field of the formaldehydeless crosslinking of cellulosic fabric, more particularly to a kind of formaldehyde-free aqueous crosslinking agent and preparation method thereof and the finishing technique to fabric.By two kinds of new water cross-linking agents, and the water-soluble multi-carboxylate of selection is crosslinking catalyst, two steps are divided to process cellulosic fabric, cellulosic fabric formaldehyde-free durable-press finishing technology is made to reach a new height, i.e. while the strength of fabric is injury-free, shrinkproof, crease-resistant, the noniron finish performance of high-grade formaldehydeless crosslinking is obtained, particularly the wet recovery angle of cellulosic fabric is significantly improved after treatment.

Description

A kind of formaldehyde-free aqueous crosslinking agent and preparation method thereof and the finishing technique to fabric
Technical field
The invention belongs to shrinkproof, crease-resistant, the non-ironing technical field of the formaldehydeless crosslinking of cellulosic fabric, more particularly to a kind of nothing first Aldehyde water cross-linking agent and preparation method thereof and the finishing technique to fabric.
Background technology
Cellulose (cotton, fiber crops, viscose glue, Modal, tencel) material make textile (clothes, home textile etc.) with pro-skin, The excellent comfort property such as moisture absorption is ventilative, is favored by consumers in general, but can produce the chis such as shrink, corrugation, deformation after washing How very little unstable phenomenon, make such textile dimensionally stable for a long time, constantly meets what consumers in general were constantly lifted Require, be textile industry key subjects of interest.
Glyoxal at present in textile industry and its each analog derivative process cellulose as formaldehyde-free durable-press finishing crosslinking agent Following Railway Project is mainly faced during fabric：Fabric xanthochromia is serious, finishing effect is undesirable, strength declines seriously.
After the hydroxyl crosslinking for being primarily due to its each analog derivative of glyoxal and cellulose of xanthochromia, can be remaining a large amount of Hemiacetal hydroxyl, can occur dehydration to generate unsaturated carbon-carbon double bond or hydroxyl occurs during high-temperature heat treatment before washing Oxidation, so as to become flaxen compound.
And undesirable the decline with strength of finishing effect is seriously the contradiction for being difficult to for a pair take into account all the time：Because crosslinking is anti-at present The catalyst that should be adopted is hydrochloric acid (HCl), the MgCl of higher concentration2·6H2O (magnesium chloride hexahydrate), (NH4)2HPO4(phosphoric acid hydrogen two Ammonium), NH4NO3The acid such as (ammonium nitrate) Lewis (lewis acid), the pH value of finish solution is generally less than 4, in the highly acid bar Under part, cellulose macromolecule chain easily inhales acid and fracture of degrading, and causes cellulosic fabric drop strong serious；And in order to control strength not Excessive descent, reducing addition can make that cross-linking reaction is insufficient again, and non-ironing effect is poor, hemiacetal remaining hydroxyl groups are many, finishing effect Undesirable.
Content of the invention
The present invention provide firstly a kind of formaldehyde-free aqueous crosslinking agent for solving above-mentioned technical problem, is denoted as cross-linking agents Ⅰ, becomes Dividing includes
Present invention also offers a kind of preparation technology of above-mentioned cross-linking agents Ⅰ：
After polyhydroxy aldehydes monose is dissolved in glyoxal solution, it is initially charged acid catalyst distillation dehydration and hemiacetal occurs Change reaction, adding polyalcohol continuation distillation dehydration makes the aldehyde radical acetalation of polyalcohol and polyhydroxy aldehydes monose, finally neutralizes Acid catalyst simultaneously cools down (villaumite for generating neutralization reaction) crystallization, filters, obtains the mixing with acetal and hemiacetal structure Thing is formaldehyde-less crosslinker I,
Wherein, polyhydroxy aldehydes monose is fisher's formula glucose,
Acid catalyst is hydrochloric acid, and after reaction, neutralization acid catalyst adopts NaOH,
Polyalcohol is ethylene glycol, glycerine, diethylene glycol etc.,
The concrete reaction equation of I preparation method of above-mentioned formaldehyde-less crosslinker is following (polyalcohol selection ethylene glycol)：
In above-mentioned reaction, the IPN between ring and ring in glucose structure, during aldehyde radical acetalation cyclization, can be formed (as two Molecule interpenetration structures of above-mentioned product), are conducive to increasing elasticity；And as glucose hydroxyl is that have fixing point Mode for cloth, between other ring structures of above-mentioned product due to sterically hindered larger due to, occur IPN possibility very little, Therefore products therefrom is main still based on above two composition, and in product, the composition of IPN does not occur and IPN occurs Between composition, mass ratio is 80～85：15～20.
The invention provides another kind of water cross-linking agent, is denoted as crosslinking agent II, the molecular structural formula of the crosslinking agent II is：
Present invention also offers a kind of preparation method of above-mentioned crosslinking agent II：
(1) 2,4- diamino benzene sulfonic acid sodium and NaOH are dissolved in water, and add three polychlorostyrene piperazines to react to system in thoroughly Bright shape,
Wherein, the consumption mol ratio preferably 1 of 2,4- diamino benzene sulfonic acid sodium, NaOH, three polychlorostyrene piperazines：2：2,
The reaction temperature after three polychlorostyrene piperazines is added to be controlled to 20 DEG C -40 DEG C,
After reaction terminates, generated in system, the molecular structural formula of intermediate product is：
(2) in the system of step (1) gained, NaOH, acidum nicotinicum is added to react transparent again to system Shape, adjustment system are neutrality, obtain crosslinking agent II,
Wherein, the mol ratio of intermediate product in the system of the NaOH, acidum nicotinicum and step (1) gained that are added For 4：2：1,
It is 7 to 8 using the pH value of cushioning liquid regulation system, the crosslinking agent II of gained can keep steady below 50 DEG C for a long time Fixed.
The invention provides a kind of finishing technique to fabric：
Organic polycarboxylic acid soluble ester is added in the aqueous solution of crosslinking agent as crosslinking catalyst, to cellulosic fabric Process is padded, then bakees the moisture content that 5%-8% is kept to fabric under the conditions of low temperature (75 DEG C -85 DEG C), then in normal temperature Coat, with plastic foil, 1-5 hour of banking up under (25 DEG C -35 DEG C), finally washing, 160 DEG C -170 DEG C drying, cellulosic fabric can be made Good shrinkproof, crease-resistant, ironing-free performance is obtained,
Wherein, crosslinking agent is above-mentioned cross-linking agents Ⅰ, and cross-linking agents Ⅰ and organic polycarboxylic acid soluble ester crosslinking catalyst Consumption mass ratio be 4～8：1,
Above-mentioned organic polycarboxylic acid soluble ester is synthesized by water-soluble polyol and polybasic carboxylic acid, wherein water-soluble polynary Alcohol is ethylene glycol, glycerine, the combination of one or more in diethylene glycol, polybasic carboxylic acid is citric acid, ethanedioic acid, the third two Acid, succinic acid, malic acid, tartaric acid, the combination of one or more in BTCA,
The organic polycarboxylic acid soluble ester can be miscible rear in homogeneous transparent solution with arbitrary proportion with water, and the matter of gained Amount concentration can be stablized in 5-7 for the pH value of the aqueous solution of 1%-2%, so that it is guaranteed that cellulosic fabric is padding cross-linking agents Ⅰ and is being somebody's turn to do During crosslinking catalyst, and fabric, when being heat-treated for follow-up 75 DEG C -85 DEG C, the pH value in fabric is consistently greater than 5, knits cellulose The strength damage of thing is less；And as the hydroxyl activity on crosslinking catalyst is far below the hemiacetal hydroxyl on cross-linking agents Ⅰ, therefore Itself is not involved in etherification reaction substantially,
In addition, above-mentioned cross-linking agents Ⅰ concentration in aqueous is 50g/L-300g/L.
Present invention also offers a kind of finishing technique of above-mentioned crosslinking agent II to fabric：
Add oxidized polyethylene wax emulsion, polyaminoester emulsion in the aqueous solution of crosslinking agent II, containing amino and polyether-based Organosiloxane emulsion, antishifting agent are simultaneously mixed, by blank or after above-mentioned cross-linking agents Ⅰ is processed cellulosic fabric Be padded in the mixed liquor, then preliminary drying, baking in 170 DEG C × 90 seconds in 95 DEG C × 30 seconds is carried out to fabric, 160 after fully washing DEG C of -170 DEG C drying, can make cellulosic fabric obtain more excellent shrinkproof, crease-resistant, ironing-free performance, and cellulosic fabric Strength effectively can be lifted,
Wherein, the concentration in aqueous of crosslinking agent II is 50g/L-250g/L,
In addition, oxidized polyethylene wax emulsion, polyaminoester emulsion, organosiloxane emulsion, anti-swimming containing amino and polyether-based The solid content for moving agent (also known as " migration inhibitor ") is followed successively by 20%, 30%, 30%, 3%,
Wherein, antishifting agent is selected from sodium alginate.
The beneficial effects of the present invention is：
By two kinds of new water cross-linking agents in the present invention, and it is crosslinking catalyst from water-soluble multi-carboxylate, point Two steps are processed to cellulosic fabric, make cellulosic fabric formaldehyde-free durable-press finishing technology reach a new height, i.e., in fabric Strength injury-free while, obtain high-grade formaldehydeless crosslinking shrinkproof, crease-resistant, noniron finish performance, particularly pass through After process, (in industry although creasy recovery angle has two kinds to the wet recovery angle of cellulosic fabric：Dry recovery angle, wet recovery angle, but It is that so-called " non-ironing " refers to fabric washing by after wet, it is not necessary to press, washing fold just can recover smooth when drying again, so Judge whether to need to refer to the data of wet recovery angle with non-ironing effect in industry, typically wet recovery angle reaches more than 240 °, i.e., With non-ironing function) it is significantly improved；
Cross-linking agents Ⅰ eliminates aldehyde radical, it is to avoid follow-up arrange during the generation of hemiacetal hydroxyl and the fabric that causes becomes Yellow phenomenon, and itself designed based on special molecular structure, with outstanding cross-linking properties, which has been activated with cellulose hydroxyl group (compared to the hydroxyl on this patent cross-linking agents Ⅰ, between common hydroxyl, etherification reaction is much more difficult, such as two points for etherification reaction At sub- ethanol dehydration becomes ether to need 145 DEG C, sulphuric acid catalysis can just be carried out) so that after cross-linking reaction, residual hydroxyl greatly reduces, On the one hand cross-linking efficiency and non-ironing effect is improve, on the other hand takes in (75 DEG C -85 DEG C) heat treatments of lower temperature, in fabric Aqueous 5%-8% containing cross-linking reaction of banking up under the conditions of wet, it is ensured that there is no xanthochromia in fabric；
As catalyst, catalytic crosslinking is sufficient with the soluble ester (as ethylene glycol citric acid three ester) of polybasic carboxylic acid for the present invention While making the pH value condition of cross-linking reaction control more than 5, it is ensured that the strength damage of fabric is less；
Present invention design has synthesized water-soluble cross-linker II, by its remote crosslinking features, allows the hydroxyl of cellulose to lead to Cross chemical bonds oxidized polyethylene wax emulsion, polyaminoester emulsion, organosiloxane emulsion, anti-migration containing amino and polyether-based High-molecular organic material in agent, makes cellulosic fabric obtain strong compensation, and improves the elasticity of fabric further so that fabric While anti-wrinkle shrink-proof, ironing-free performance are improved further, the tearing brute force of fabric also gets a promotion.
Specific embodiment
Embodiment 1
The preparation of cross-linking agents Ⅰ：
After 180g glucose being dissolved in the technical grade glyoxal solution of 250g Solute mass fraction 40%, it is initially charged The concentrated hydrochloric acid catalyst of 0.8ml Solute mass fraction 36.5%, is heated to reflux hemiacetalization reaction 1.5 hours, then controls Temperature processed distillates part in 102 DEG C～108 DEG C distillation dehydrations to nothing；110 DEG C are to slowly warm up to after adding 62g ethylene glycol and are incubated To the aldehyde radical acetalation for making ethylene glycol and glucose nothing distillate, it is eventually adding in NaOH and hydrochloric acid crystallisation by cooling, mistake Filter, obtains the mixture of multiple acetals and hemiacetal, i.e. cross-linking agents Ⅰ.
Embodiment 2
The preparation of crosslinking agent II：
(1) 2,4- diamino benzene sulfonic acid sodium and NaOH are dissolved completely in water, and add three polychlorostyrene piperazines to react in 35 DEG C To the transparent shape of system,
2,4- diamino benzene sulfonic acid sodium, NaOH, the consumption mol ratio of three polychlorostyrene piperazines are 1：2：2；
(2) in the system of step (1) gained add NaOH, acidum nicotinicum and react at 47 DEG C -50 DEG C to System transparent shape again, is 7 using the pH value of neutral buffer regulation system, obtains the aqueous solution of crosslinking agent II, and in Less than 50 DEG C preserve,
Wherein, in the system of the NaOH, acidum nicotinicum and step (1) gained that are added, pure intermediate product rubs You are than being 4：2：1.
The pretreatment of fabric：
Bafta through desizing, kiering, bleaching, mercerising pre-treatment is carried out Liquid Ammonia Treatment, obtains high-count and high-density cotton mansion Silk (warp × latitude weave specification：Yarn count 80s × 80s, 685 × 512/10cm of density).Room is carried out to pretreated fabric Moisture regain test (the results are shown in Table one) under the conditions of temperature.
Embodiment 3
(its in the aqueous solution of the cross-linking agents Ⅰ prepared by embodiment 1 will be dipped through the cotton poplin cloth of above-mentioned pretreatment In, cross-linking agents Ⅰ 80g/L, catalyst glycol citric acid three ester 15g/L, pH value are 6), pick-up 78%, dries at 85 DEG C It is 7% to do and make within 60 seconds fabric moisture percentage now, is then banked up 3 hours with plastic foil cladding at 30 DEG C, last fully washing And dry in 160 DEG C,
Solution, cloth cover when in experimentation repeatedly to dipping, the cloth cover in 85 DEG C of drying courses, cloth cover when banking up, And cloth cover during final 160 DEG C of drying is detected, pH value is measured all in the range of 6-7, sample room temperature condition after cooling Lower moisture regain test (the results are shown in Table).
Embodiment 4
Cotton poplin cloth through 3 crosslinking Treatment of embodiment is dipped in the aqueous solution of the crosslinking agent II prepared by embodiment 2 In (wherein, II 100g/L of crosslinking agent, the oxidized polyethylene wax emulsion 20g/L of solid content 20%, solid content 30% polyurethane breast Liquid 15g/L, organosiloxane emulsion 20g/L containing amino and polyether-based of solid content 30%, the sodium alginate of solid content 3% resist Migration agent
2g/L), pick-up 75%, entering back into multistage continuous baking oven carries out the preliminary drying of 95 DEG C × 30 seconds and 170 DEG C × 90 seconds Bake, then fully washing dry at 160 DEG C, sampling after cooling under room temperature condition moisture regain test (the results are shown in Table One).
Comparative example 1
Catalyst " ethylene glycol citric acid three ester " in embodiment 3 is replaced with the acetic acid of 3 times of molal quantitys, remaining operation is constant.
After treatment to moisture regain test (the results are shown in Table) under fabric room temperature condition.
Table 1
(note：Due to using absorption photometry detection content of formaldehyde lower limit be 20ppm, so the world respectively detect tissue with The correlation standard of formulation, textile of the content of formaldehyde less than 20ppm belong to formaldehydeless class textile)

Claims (10)

1. a kind of formaldehyde-free aqueous crosslinking agent, is denoted as cross-linking agents Ⅰ, it is characterised in that：Described cross-linking agents Ⅰ composition includes
2. a kind of preparation method of formaldehyde-free aqueous as claimed in claim 1 crosslinking agent, it is characterised in that：Described preparation side Method is,
After polyhydroxy aldehydes monose is dissolved in glyoxal solution, it is initially charged acid catalyst distillation dehydration and occurs hemiacetalization anti- Should, adding polyalcohol continuation distillation dehydration makes the aldehyde radical acetalation of polyalcohol and polyhydroxy aldehydes monose, and finally neutralization acid is urged Agent crystallisation by cooling, filter, obtain the mixture i.e. formaldehyde-less crosslinker I with acetal and hemiacetal structure.
3. the preparation method of formaldehyde-free aqueous crosslinking agent as claimed in claim 2, it is characterised in that：Described polyhydroxy aldehydes Monose is glucose, and described acid catalyst is hydrochloric acid, and after reaction, neutralization acid catalyst adopts NaOH.
4. the preparation method of formaldehyde-free aqueous crosslinking agent as claimed in claim 2, it is characterised in that：Described polyalcohol is second Glycol, glycerine or diethylene glycol.
5. a kind of water cross-linking agent, is denoted as crosslinking agent II, it is characterised in that：The molecular structural formula of the crosslinking agent II is
6. a kind of preparation method of water cross-linking agent as claimed in claim 5, it is characterised in that：Described preparation method is, (1) 2,4- diamino benzene sulfonic acid sodium and NaOH are dissolved in water, and add three polychlorostyrene piperazines to react shape transparent to system；
(2) in the system of step (1) gained, add NaOH, acidum nicotinicum to react to system transparent shape again, adjust Overall system is neutrality, obtains crosslinking agent II.
7. a kind of finishing technique to fabric, it is characterised in that：Described finishing technique includes,
Organic polycarboxylic acid soluble ester is added in the aqueous solution of crosslinking agent as crosslinking catalyst, to cellulosic fabric in upper Stating in the aqueous solution carries out padding process, then bakees under cryogenic, then banks up at normal temperatures, finally washing, drying.
8. finishing technique as claimed in claim 7, it is characterised in that：Described crosslinking agent is the friendship described in claim 1 Connection agent I.
9. finishing technique as claimed in claim 8, it is characterised in that：Described cross-linking agents Ⅰ is water-soluble with organic polycarboxylic acid The consumption mass ratio of ester crosslinking catalyst is 4～8：1.
10. finishing technique of a kind of water cross-linking agent based on described in claim 5 to fabric, it is characterised in that：Described is whole Science and engineering skill includes,
Add oxidized polyethylene wax emulsion, polyaminoester emulsion in the aqueous solution of crosslinking agent II, containing the organic of amino and polyether-based Silicone emulsion, antishifting agent are simultaneously mixed, and the blank or cellulosic fabric after claim 7 is arranged is padded in In the mixed liquor, then preliminary drying, fully baking, washing, drying is carried out to fabric.
CN201610899567.6A 2016-10-14 2016-10-14 A kind of formaldehyde-free aqueous crosslinking agent and preparation method thereof and finishing technique to fabric Expired - Fee Related CN106478745B (en)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN113789658A (en) * 2021-09-28 2021-12-14 鲁泰纺织股份有限公司 Non-ironing production method of pure cotton knitted shirt ready-made clothes

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