CN106436278A - Ammoniation modification method of ramine fibers and application method thereof in liquid ammonia solvent dyeing - Google Patents
Ammoniation modification method of ramine fibers and application method thereof in liquid ammonia solvent dyeing Download PDFInfo
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- CN106436278A CN106436278A CN201610885187.7A CN201610885187A CN106436278A CN 106436278 A CN106436278 A CN 106436278A CN 201610885187 A CN201610885187 A CN 201610885187A CN 106436278 A CN106436278 A CN 106436278A
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- yarn
- thread
- dyeing
- ramine
- ammoniation
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 238000000034 method Methods 0.000 title claims abstract description 44
- 238000004043 dyeing Methods 0.000 title claims abstract description 36
- 239000002904 solvent Substances 0.000 title claims abstract description 22
- 239000000835 fiber Substances 0.000 title claims abstract description 20
- 238000002715 modification method Methods 0.000 title abstract 4
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 59
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000008367 deionised water Substances 0.000 claims abstract description 15
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 14
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims abstract description 10
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 240000008564 Boehmeria nivea Species 0.000 claims description 73
- 238000009970 yarn dyeing Methods 0.000 claims description 22
- 239000000047 product Substances 0.000 claims description 21
- 239000000975 dye Substances 0.000 claims description 19
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 19
- 230000008569 process Effects 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000004458 analytical method Methods 0.000 claims description 14
- 230000008859 change Effects 0.000 claims description 13
- 230000000694 effects Effects 0.000 claims description 13
- 239000001257 hydrogen Substances 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 239000004327 boric acid Substances 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 239000012467 final product Substances 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 239000000985 reactive dye Substances 0.000 claims description 7
- 239000008399 tap water Substances 0.000 claims description 7
- 235000020679 tap water Nutrition 0.000 claims description 7
- -1 Imines ion Chemical class 0.000 claims description 4
- 230000003321 amplification Effects 0.000 claims description 4
- 238000003199 nucleic acid amplification method Methods 0.000 claims description 4
- GCFAQSYBSUQUPL-UHFFFAOYSA-I pentasodium 5-[[4-chloro-6-[3-(2-sulfonatooxyethylsulfonyl)anilino]-1,3,5-triazin-2-yl]amino]-3-[(1,5-disulfonatonaphthalen-2-yl)diazenyl]-4-hydroxynaphthalene-2,7-disulfonate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].Oc1c(N=Nc2ccc3c(cccc3c2S([O-])(=O)=O)S([O-])(=O)=O)c(cc2cc(cc(Nc3nc(Cl)nc(Nc4cccc(c4)S(=O)(=O)CCOS([O-])(=O)=O)n3)c12)S([O-])(=O)=O)S([O-])(=O)=O GCFAQSYBSUQUPL-UHFFFAOYSA-I 0.000 claims description 2
- 238000004176 ammonification Methods 0.000 claims 1
- 239000000463 material Substances 0.000 claims 1
- 239000004753 textile Substances 0.000 abstract description 7
- 238000001035 drying Methods 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract 2
- 229960002645 boric acid Drugs 0.000 abstract 1
- 235000010338 boric acid Nutrition 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000012986 modification Methods 0.000 abstract 1
- 230000004048 modification Effects 0.000 abstract 1
- 238000010992 reflux Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 9
- 241001649247 Boehmeria Species 0.000 description 6
- 230000008901 benefit Effects 0.000 description 4
- 239000004744 fabric Substances 0.000 description 4
- 238000005411 Van der Waals force Methods 0.000 description 3
- 229920002678 cellulose Polymers 0.000 description 3
- 239000001913 cellulose Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000009941 weaving Methods 0.000 description 2
- 240000004246 Agave americana Species 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 description 1
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 238000005576 amination reaction Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000009120 camo Nutrition 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 235000005607 chanvre indien Nutrition 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000011487 hemp Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- 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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
-
- 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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/58—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides
- D06M11/59—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with ammonia; with complexes of organic amines with inorganic substances
- D06M11/60—Ammonia as a gas or in solution
-
- 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
- D06M13/12—Aldehydes; Ketones
- D06M13/127—Mono-aldehydes, e.g. formaldehyde; Monoketones
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/38—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using reactive dyes
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
- D06P3/66—Natural or regenerated cellulose using reactive dyes
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Coloring (AREA)
Abstract
The invention relates to an ammoniation modification method of ramine fibers and an application method thereof in liquid ammonia solvent dyeing, and belongs to the technical field of textile chemistry. The ammoniation modification method comprises the following steps: pretreatment of the ramine fibers: selecting ramine yarns from the ramine fibers, placing the ramine yarns in a 200 mL of NaOH solution of which the concentration is 15%, heating to the temperature of 50 DEG C, insulating for 4 hours, and cleaning with running water until pH of eluate is 7-8 to obtain pretreated yarns; modification to the pretreated yarns: adding 10-15 mL of formaldehyde, 1-2 mL of boracic acid and 150 mL of deionized water in a three-necked flask with the volume of 250 ml, stirring uniformly, adding the pretreated ramine yarns, heating the reaction temperature to be 40 DEG C, feeding ammonia, refluxing, stirring and reacting for 3 hours, taking out the yarns after reaction is finished, washing with the deionized water, and drying the yarns after pH of the eluate is 6-7 to obtain the ammoniation modified ramine yarns. The ammoniation modification method of the ramine fibers is used in ramine fiber liquid ammonia solvent dyeing, and dyeing uniformity of the ramine fibers can be improved obviously.
Description
Technical field
The invention belongs to technical field of textile chemistry, and in particular to a kind of ammoniation modified method of ramee and its in liquid
Application process in ammonia solvent dyeing.
Background technology
Textile industry is the conventional column industry of Chinese national economy and important people's livelihood industry, and international competitive advantage
Obvious industry, ramee is one of primary raw material of weaving face fabric, occupies critical role in weaving face fabric.China is generation
, mainly there are Boehmeria, Folium Agaves Sisalanae, Caulis et Folium Lini and yellow mestha etc. in one of most abundant country of hemp resource in boundary, and wherein, Boehmeria is grown with which
Speed is fast, yield is high, easy survival the advantages of extensively plant in China.The fabric that ramee is made into has ventilative, moisture absorbing and sweat releasing
The advantages of, it is preferable summer high-grade clothing fabric.
In recent years, China's textile industry ecological circulation economic development contradiction, the height of water resource is relied on and
The environmental problem that maximum discharge is caused seriously governs the sustainable development of the sector.According to statistics, China's textile printing and dyeing industry year consumption
1,700,000,000 tons of the water yield, up to 1,600,000,000 tons of disposal of pollutants.Compared with foreign countries, the water consumption of China's textile printing and dyeing industry is external 2-3
Times, energy consumption is external 3-5 times.In order to solve a difficult problem for high energy consumption, applicants studied the non-aqueous dyeing of ramee, will
Ramee is put in liquefied ammonia dicyandiamide solution and dyes, and using the volatility of liquefied ammonia, liquefied ammonia solvent is carried out recycling use.?
During this, applicants have discovered that a problem, i.e. ramee molecule are poor with the wellability of liquefied ammonia molecule.
Ramee has the preferable compatibility with aqueous solution, this is because which contains a lot of hydrophilic radicals, such as hydrogen-oxygen
Root etc..Applicant have studied the dyeing of ramee in liquefied ammonia system, as a result find, profit of the ramee in liquefied ammonia solvent
Moist poor.When ramie yarn and thread is more, be wrapped in the inside yarn dyeing effect poor, it is found by the applicant that be due to ramie yarn
Line fails complete wetting in liquefied ammonia solvent, and the dyeing so as to cause yarn is uneven.Under the same conditions, dye in aqueous solvent
When, the yarn for being wrapped in the inside can then obtain preferable Color.For this problem, applicant is proposed to ramie yarn and thread
Carry out ammoniation modified, make Boehmeria surface increase more amino.When the amino of ramee is more, former according to " similar mix "
The feature of hydrogen bond or Van der Waals force can be produced between reason and ramee and amino molecule, and ramee preferably will infiltrate
In liquefied ammonia solvent, so as to realize the dyeing in liquefied ammonia solvent.
At present, the ammoniation modified report of ramee is less, wherein, has one with regard to the amination modifying of ramee
Patent report, the patent application of Application No. 88100237.2 discloses a kind of process for ammoniation modifying of ramie fibre, and the invention is used
Sodium hydroxide solution carries out, to ramee, the crystalline substance that disappears, and is then entered for aminating agent using 1- chlorine-2-hydroxyl propyl group tri alkyl ammomium chloride
Row aminating reaction, the reaction have effectively achieved the amido for introducing charged cation on ramee surface, its chemistry knot
Structure formula isBut, the present invention is to introduce uncharged amino in fiber surface, and its chemical structural formula is-NH2, with
The former has the difference of essence.
Requirement more and more higher of the domestic and international market to ecological textile and environmental conservation, the need of few water or waterless staining technique
Ask increasing, in order to this kind of novel technical method is realized, have some technical barriers to need to break through further in the process.This
Bright application is dyeed and invents to realize ramee in liquefied ammonia dicyandiamide solution.
Content of the invention
The deficiency that the present invention is present for pointed problem in background technology and prior art, it is an object of the invention to
Ammoniation modified method and its application process in liquefied ammonia solvent dyeing of a kind of ramee are provided, so that Boehmeria surface is increased more
Many amino.When the amino of ramee is more, permissible between principle and ramee and amino molecule according to " similar mix "
The feature of hydrogen bond or Van der Waals force is produced, ramee preferably will be infiltrated in liquefied ammonia solvent, so as to realize liquefied ammonia solvent
In dyeing.
In order to realize the above-mentioned purpose of the present invention, inventor have developed a kind of Boehmeria fibre through substantial amounts of experimental study
The ammoniation modified method of dimension, it is characterised in that methods described comprises the steps：
(1) pretreatment of ramee：Ramee chooses ramie yarn and thread, and 2-5g ramie yarn and thread is put into 200mL concentration
For 15% NaOH solution, 50 DEG C are heated to, 4h are incubated, are cleaned with tap water, until eluate pH is 7-8, that is, to obtain
Pretreatment yarn；This step is to carry out alkali process to ramee, so that ramee occurs the expanded phenomenon of profit, makes cellulose
Become high resilience and gloss, while it is partly dissolved the low polymerization degree in cellulose, so as to improve the equal of molecular weight cellulose
One property, makes the physicochemical change of fiber and structure variation to improve fiber chemical reaction ability itself；
(2) method of modifying：10-15mL formaldehyde, 1-2mL boric acid and 150mL deionization are added toward in 250ml three-neck flask
Water, uniform stirring, the pretreated 1-2g ramie yarn and thread of step (1) is added, reaction temperature is increased to 40 DEG C, then is passed through ammonia
Gas, is refluxed reaction 3 hours, after the completion of reaction, yarn is taken out, and deionized water is rinsed, will when eluate pH is for 6-7
Drying yarn, obtains final product ammoniation modified ramie yarn and thread；
(3) elementary analysiss are done modified yarn with unmodified yarn, obtains following result：
From elementary analysiss result：Ramie yarn and thread is through modified, and essential element carbon (C), hydrogen (H) are all without significantly
Change, and nitrogen content substantially increases, up to 9-16 times of amplification, and amino (- NH is described2) be successfully grafted on fiber.
Further, the reaction in technique scheme in step (2) method of modifying can be represented with following equation：
Above-mentioned reaction is reacted for Mannich, and its reaction principle is as follows：First, amino molecule is reacted with formaldehyde, sloughs hydrone
Obtain imines ion intermediate；Then, the reactive hydrogen atom on imines ion intermediate attack ramee, removing proton is obtained
Ammoniation modified ramie yarn and thread.
The present invention also provides a kind of ammoniation modified application process in liquefied ammonia solvent dyeing of above-mentioned ramee, and which is special
Levy and be, methods described comprises the steps：
The first step, chooses the ammoniation modified ramie yarn and thread of certain mass and unmodified yarn, by ammoniation modified ramie yarn
Line and unmodified yarn are wound in closely knit a branch of respectively, and the reactive dye REACTIVE Red 195 that can be dissolved in liquefied ammonia is dissolved in
In liquefied ammonia, ammoniation modified ramie yarn and thread and unmodified yarn are immersed in liquefied ammonia dye liquor are dyeed respectively, dyeing condition
For：Dye dosage 10-15% (o.m.f), bath raio 1：20, the dyeing time 20-50 second, obtain product dyed thereby；
Second step, observes this product dyed thereby, as a result finds, ammoniation modified ramie yarn and thread product dyed thereby color even, no pattern are existing
As the yarn for being wrapped in the inside is all consistent with the yarn dyeing effect of outside；Unmodified yarn dyeing thing surface color is more equal
Even, surface no obvious pattern phenomenon, the yarn dyeing for being wrapped in the inside is uneven.
Compared with prior art, the present invention has following beneficial effect：
(1) present invention carries out ammoniation modified to ramee, makes ramee surface increase more amino.When Boehmeria fibre
When the amino of dimension is more, hydrogen bond or Van der Waals force can be produced according to " similar mix " between principle and ramee and amino molecule
Feature, ramee preferably will be infiltrated in liquefied ammonia solvent, so as to realize the dyeing in liquefied ammonia solvent；
(2) ammoniation modified ramie yarn and thread in the present invention, with good wellability in liquefied ammonia, is ramie yarn and thread in liquid
Dyeing in ammonia provides condition, the problems such as solve aberration heterogeneity in ramie yarn and thread dyeing course；Its application process has dye
Color processing step is few, and dyeing time is short, dyestuff reusable edible after dye, reduce environmental pollution the advantages of, achievable ramie yarn and thread
In dyeing course, non-aqueous dyeing is required.
Specific embodiment
Form is described in further detail again to the above of the present invention by the following examples, but should not be managed this
Solve the scope for the above-mentioned theme of the present invention and be only limitted to below example, all technology that is realized based on the above of the present invention are equal
Belong to the scope of the present invention.
Embodiment 1
(1) pretreatment of ramee：Ramee chooses ramie yarn and thread, and 2g ramie yarn and thread is put into 200mL concentration is
15% NaOH solution, is heated to 50 DEG C, is incubated 4h, is cleaned with tap water, until eluate pH is 7.6, that is, to obtain pre-
Process yarn.
(2) method of modifying：10mL formaldehyde, 1mL boric acid and 150mL deionized water are added toward in 250ml three-neck flask, uniformly
Stirring, adds the pretreated 1g ramie yarn and thread of step (1), reaction temperature is increased to 40 DEG C, then is passed through ammonia, and backflow is stirred
Reaction 3 hours is mixed, after the completion of reaction, yarn is taken out, deionized water is rinsed, by drying yarn when eluate pH is 6-7,
Obtain final product ammoniation modified ramie yarn and thread.
(3) elementary analysiss are done modified yarn with unmodified yarn, obtains following result：
From elementary analysiss result：Ramie yarn and thread is through modified, and essential element carbon (C), hydrogen (H) are all without significantly
Change, and nitrogen content substantially increases, and increases about 13 times of multiple, and amino (- NH is described2) be successfully grafted on fiber.
The ammoniation modified application process in liquefied ammonia solvent dyeing of ramee：
The first step, (2) ammoniation modified ramie yarn and thread for obtaining and unmodified yarn the step of choose certain mass, by ammonia
Change modified ramie yarn and unmodified yarn be wound in respectively closely knit a branch of, by the reactive dye that can be dissolved in liquefied ammonia activity
Red 195 are dissolved in liquefied ammonia, ammoniation modified ramie yarn and thread and unmodified yarn are immersed in liquefied ammonia dye liquor are contaminated respectively
Color, dye dosage 15% (o.m.f), bath raio 1：20, dyeing time obtained product dyed thereby under conditions of 20 seconds.
Second step, observes this product dyed thereby, as a result finds：Ammoniation modified ramie yarn and thread product dyed thereby color even, no pattern are existing
As the yarn for being wrapped in the inside is all consistent with the yarn dyeing effect of outside；Unmodified yarn dyeing thing surface color is more equal
Even, surface no obvious pattern phenomenon, the yarn dyeing for being wrapped in the inside is uneven.
Embodiment 2
(1) pretreatment of ramee：Ramee chooses ramie yarn and thread, and 2g ramie yarn and thread is put into 200mL concentration is
15% NaOH solution, is heated to 50 DEG C, is incubated 4h, is cleaned with tap water, until eluate pH is 7.3, that is, to obtain pre-
Process yarn.
(2) method of modifying：12mL formaldehyde, 1.5mL boric acid and 150mL deionized water are added toward in 250ml three-neck flask, all
Even stirring, adds the pretreated 1g ramie yarn and thread of step (1), reaction temperature is increased to 40 DEG C, then is passed through ammonia, backflow
Stirring reaction 3 hours, after the completion of reaction, yarn is taken out, and deionized water is rinsed, and is dried yarn when eluate pH is 6-7
Dry, obtain final product ammoniation modified ramie yarn and thread.
(3) elementary analysiss are done modified yarn with unmodified yarn, obtains following result：
From elementary analysiss result：Ramie yarn and thread is through modified, and essential element carbon (C), hydrogen (H) are all without significantly
Change, and nitrogen content substantially increases, and increases about 11 times of multiple, and amino (- NH is described2) be successfully grafted on fiber.
The ammoniation modified application process in liquefied ammonia solvent dyeing of ramee：
The first step, (2) ammoniation modified ramie yarn and thread for obtaining and unmodified yarn the step of choose certain mass, by ammonia
Change modified ramie yarn and unmodified yarn be wound in respectively closely knit a branch of, by the reactive dye that can be dissolved in liquefied ammonia activity
Red 195 are dissolved in liquefied ammonia, ammoniation modified ramie yarn and thread and unmodified yarn are immersed in liquefied ammonia dye liquor are contaminated respectively
Color, dye dosage 10% (o.m.f), bath raio 1：20, dyeing time obtained product dyed thereby under conditions of 30 seconds.
Second step, observes this product dyed thereby, as a result finds：Ammoniation modified ramie yarn and thread product dyed thereby color even, no pattern are existing
As the yarn for being wrapped in the inside is all consistent with the yarn dyeing effect of outside；Unmodified yarn dyeing thing surface color is more equal
Even, surface no obvious pattern phenomenon, the yarn dyeing for being wrapped in the inside is uneven.
Embodiment 3
(1) pretreatment of ramee：Ramee chooses ramie yarn and thread, and 2g ramie yarn and thread is put into 200mL concentration is
15% NaOH solution, is heated to 50 DEG C, is incubated 4h, is cleaned with tap water, until eluate pH is 7.1, that is, to obtain pre-
Process yarn.
(2) method of modifying：12mL formaldehyde, 1.5mL boric acid and 150mL deionized water are added toward in 250ml three-neck flask, all
Even stirring, adds the pretreated 1g ramie yarn and thread of step (1), reaction temperature is increased to 40 DEG C, then is passed through ammonia, backflow
Stirring reaction 3 hours, after the completion of reaction, yarn is taken out, and deionized water is rinsed, and is dried yarn when eluate pH is 6-7
Dry, obtain final product ammoniation modified ramie yarn and thread.
(3) elementary analysiss are done modified yarn with unmodified yarn, obtains following result：
From elementary analysiss result：Ramie yarn and thread is through modified, and essential element carbon (C), hydrogen (H) are all without significantly
Change, and nitrogen content substantially increases, and increases about 9 times of multiple, and amino (- NH is described2) be successfully grafted on fiber.
The ammoniation modified application process in liquefied ammonia solvent dyeing of ramee：
The first step, (2) ammoniation modified ramie yarn and thread for obtaining and unmodified yarn the step of choose certain mass, by ammonia
Change modified ramie yarn and unmodified yarn be wound in respectively closely knit a branch of, by the reactive dye that can be dissolved in liquefied ammonia activity
Red 195 are dissolved in liquefied ammonia, ammoniation modified ramie yarn and thread and unmodified yarn are immersed in liquefied ammonia dye liquor are contaminated respectively
Color, dye dosage 15% (o.m.f), bath raio 1：20, dyeing time obtained product dyed thereby under conditions of 40 seconds.
Second step, observes this product dyed thereby, as a result finds：Ammoniation modified ramie yarn and thread product dyed thereby color even, no pattern are existing
As the yarn for being wrapped in the inside is all consistent with the yarn dyeing effect of outside；Unmodified yarn dyeing thing surface color is more equal
Even, surface no obvious pattern phenomenon, the yarn dyeing for being wrapped in the inside is uneven.
Embodiment 4
(1) pretreatment of ramee：Ramee chooses ramie yarn and thread, and 2g ramie yarn and thread is put into 200mL concentration is
15% NaOH solution, is heated to 50 DEG C, is incubated 4h, is cleaned with tap water, until eluate pH is 7.5, that is, to obtain pre-
Process yarn.
(2) method of modifying：15mL formaldehyde, 2mL boric acid and 150mL deionized water are added toward in 250ml three-neck flask, uniformly
Stirring, adds the pretreated 1.5g ramie yarn and thread of step (1), reaction temperature is increased to 40 DEG C, then is passed through ammonia, backflow
Stirring reaction 3 hours, after the completion of reaction, yarn is taken out, and deionized water is rinsed, and is dried yarn when eluate pH is 6-7
Dry, obtain final product ammoniation modified ramie yarn and thread.
(3) elementary analysiss are done modified yarn with unmodified yarn, obtains following result：
From elementary analysiss result：Ramie yarn and thread is through modified, and essential element carbon (C), hydrogen (H) are all without significantly
Change, and nitrogen content substantially increases, up to 16 times of amplification, and amino (- NH is described2) be successfully grafted on fiber.
The ammoniation modified application process in liquefied ammonia solvent dyeing of ramee：
The first step, (2) ammoniation modified ramie yarn and thread for obtaining and unmodified yarn the step of choose certain mass, by ammonia
Change modified ramie yarn and unmodified yarn be wound in respectively closely knit a branch of, by the reactive dye that can be dissolved in liquefied ammonia activity
Red 195 are dissolved in liquefied ammonia, ammoniation modified ramie yarn and thread and unmodified yarn are immersed in liquefied ammonia dye liquor are contaminated respectively
Color, dye dosage 15% (o.m.f), bath raio 1：20, dyeing time obtained product dyed thereby under conditions of 50 seconds.
Second step, observes this product dyed thereby, as a result finds：Ammoniation modified ramie yarn and thread product dyed thereby color even, no pattern are existing
As the yarn for being wrapped in the inside is all consistent with the yarn dyeing effect of outside；Unmodified yarn dyeing thing surface color is more equal
Even, surface no obvious pattern phenomenon, the yarn dyeing for being wrapped in the inside is uneven.
Embodiment 5
(1) pretreatment of ramee：Ramee chooses ramie yarn and thread, and 2g ramie yarn and thread is put into 200mL concentration is
15% NaOH solution, is heated to 50 DEG C, is incubated 4h, is cleaned with tap water, until eluate pH is 7.4, that is, to obtain pre-
Process yarn.
(2) method of modifying：13mL formaldehyde, 1.5mL boric acid and 150mL deionized water are added toward in 250ml three-neck flask, all
Even stirring, adds the pretreated 1g ramie yarn and thread of step (1), reaction temperature is increased to 40 DEG C, then is passed through ammonia, backflow
Stirring reaction 3 hours, after the completion of reaction, yarn is taken out, and deionized water is rinsed, and is dried yarn when eluate pH is 6-7
Dry, obtain final product ammoniation modified ramie yarn and thread.
(3) elementary analysiss are done modified yarn with unmodified yarn, obtains following result：
From elementary analysiss result：Ramie yarn and thread is through modified, and essential element carbon (C), hydrogen (H) are all without significantly
Change, and nitrogen content substantially increases, up to 11 times of amplification, and amino (- NH is described2) be successfully grafted on fiber.
The ammoniation modified application process in liquefied ammonia solvent dyeing of ramee：
The first step, (2) ammoniation modified ramie yarn and thread for obtaining and unmodified yarn the step of choose certain mass, by ammonia
Change modified ramie yarn and unmodified yarn be wound in respectively closely knit a branch of, by the reactive dye that can be dissolved in liquefied ammonia activity
Red 195 are dissolved in liquefied ammonia, ammoniation modified ramie yarn and thread and unmodified yarn are immersed in liquefied ammonia dye liquor are contaminated respectively
Color, dye dosage 12% (o.m.f), bath raio 1：20, dyeing time obtained product dyed thereby under conditions of 30 seconds.
Second step, observes this product dyed thereby, as a result finds：Ammoniation modified ramie yarn and thread product dyed thereby color even, no pattern are existing
As the yarn for being wrapped in the inside is all consistent with the yarn dyeing effect of outside；Unmodified yarn dyeing thing surface color is more equal
Even, surface no obvious pattern phenomenon, the yarn dyeing for being wrapped in the inside is uneven.
Claims (3)
1. a kind of ammoniation modified method of ramee, it is characterised in that methods described comprises the steps：
(1) pretreatment of ramee：Ramee chooses ramie yarn and thread, and 2-5g ramie yarn and thread is put into 200mL concentration is
15% NaOH solution, is heated to 50 DEG C, is incubated 4h, is cleaned with tap water, until eluate pH is 7-8, that is, to obtain pre-
Process yarn；
(2) method of modifying：10-15mL formaldehyde, 1-2mL boric acid and 150mL deionized water are added toward in 250ml three-neck flask, all
Even stirring, adds the pretreated 1-2g ramie yarn and thread of step (1), reaction temperature is increased to 40 DEG C, then is passed through ammonia, returns
Stream stirring reaction 3 hours, after the completion of reaction, yarn is taken out, and deionized water is rinsed, by yarn when eluate pH is 6-7
Dry, obtain final product ammoniation modified ramie yarn and thread；
(3) elementary analysiss are done modified yarn with unmodified yarn, obtains following result：
From elementary analysiss result：Ramie yarn and thread is through modified, essential element carbon (C), hydrogen (H) all not significantly changes
Change, and nitrogen content substantially increases, up to 9-16 times of amplification, and amino (- NH is described2) be successfully grafted on fiber.
2. the ammoniation modified method of ramee according to claim 1, it is characterised in that：In step (2) method of modifying
Reaction can be represented with following equation：
Above-mentioned reaction is reacted for Mannich, and its reaction principle is as follows：First, amino molecule is reacted with formaldehyde, is sloughed hydrone and is obtained
Imines ion intermediate；Then, the reactive hydrogen atom on imines ion intermediate attack ramee, removing proton obtains ammonification
Modified ramie yarn.
3. the ammoniation modified application side in liquefied ammonia solvent dyeing of the ramee described in a kind of claim 1-2 any one
Method, it is characterised in that methods described comprises the steps：
The first step, chooses the ammoniation modified ramie yarn and thread of certain mass and unmodified yarn, by ammoniation modified ramie yarn and thread and
Unmodified yarn is wound in closely knit a branch of respectively, and the reactive dye REACTIVE Red 195 that can be dissolved in liquefied ammonia is dissolved in liquefied ammonia
In, ammoniation modified ramie yarn and thread and unmodified yarn being immersed in liquefied ammonia dye liquor dyeed respectively, dyeing condition is：Dye
Material consumption 10-15% (o.m.f), bath raio 1：20, the dyeing time 20-50 second, obtain product dyed thereby；
Second step, observes this product dyed thereby, as a result finds, ammoniation modified ramie yarn and thread product dyed thereby color even, and no pattern phenomenon, twines
Yarn dyeing effect around yarn inside with outside is all consistent；Unmodified yarn dyeing thing surface color is more uniform, table
Face no obvious pattern phenomenon, the yarn dyeing for being wrapped in the inside is uneven.
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| CN107213875A (en) * | 2017-06-21 | 2017-09-29 | 武汉纺织大学 | A kind of modified ramie porous microsphere sorbent of Adsorption of Heavy Metals ion and preparation method and application |
| CN108532327A (en) * | 2018-04-24 | 2018-09-14 | 武汉纺织大学 | A method of improving reactive dye liquefied ammonia dye fixing rate |
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| CN110725141B (en) * | 2019-11-18 | 2022-04-22 | 武汉纺织大学 | Enzyme-dyed lyocell fiber fabric and preparation method thereof |
| CN114790656A (en) * | 2022-04-24 | 2022-07-26 | 武汉纺织大学 | Antibacterial lyocell fabric and preparation method thereof |
| CN114790656B (en) * | 2022-04-24 | 2024-05-10 | 武汉纺织大学 | Antibacterial lyocell fabric and preparation method thereof |
| CN115110307A (en) * | 2022-08-01 | 2022-09-27 | 武汉纺织大学 | Flame-retardant Lyocell fabric and preparation method thereof |
| CN115110307B (en) * | 2022-08-01 | 2024-04-26 | 武汉纺织大学 | Flame-retardant lyocell fabric and preparation method thereof |
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