CN106436278B - A kind of ammoniation modified method of ramee and its application process in liquefied ammonia solvent dyeing - Google Patents
A kind of ammoniation modified method of ramee and its application process in liquefied ammonia solvent dyeing Download PDFInfo
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- CN106436278B CN106436278B CN201610885187.7A CN201610885187A CN106436278B CN 106436278 B CN106436278 B CN 106436278B CN 201610885187 A CN201610885187 A CN 201610885187A CN 106436278 B CN106436278 B CN 106436278B
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- yarn
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 117
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000004043 dyeing Methods 0.000 title abstract description 32
- 239000002904 solvent Substances 0.000 title abstract description 21
- 230000008569 process Effects 0.000 title abstract description 15
- 240000008564 Boehmeria nivea Species 0.000 claims abstract description 79
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000003756 stirring Methods 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
- 239000004327 boric acid Substances 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 239000008399 tap water Substances 0.000 claims abstract description 8
- 235000020679 tap water Nutrition 0.000 claims abstract description 8
- 239000003643 water by type Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000000921 elemental analysis Methods 0.000 claims description 14
- 239000000835 fiber Substances 0.000 claims description 12
- 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
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 230000008859 change Effects 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 230000003321 amplification Effects 0.000 claims description 4
- 238000003199 nucleic acid amplification method Methods 0.000 claims description 4
- 238000004176 ammonification Methods 0.000 claims 1
- 239000004753 textile Substances 0.000 abstract description 9
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 abstract 3
- 238000009970 yarn dyeing Methods 0.000 description 19
- 239000000975 dye Substances 0.000 description 18
- 230000000694 effects Effects 0.000 description 13
- 239000000243 solution Substances 0.000 description 10
- 239000000985 reactive dye Substances 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
- 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
- -1 imines ion Chemical class 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
- 244000198134 Agave sisalana Species 0.000 description 1
- 235000011624 Agave sisalana Nutrition 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
- 235000004431 Linum usitatissimum Nutrition 0.000 description 1
- 240000006240 Linum usitatissimum 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
- 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
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000002860 competitive effect 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
- 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 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000001007 puffing effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010992 reflux 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
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Coloring (AREA)
Abstract
The present invention relates to a kind of ammoniation modified method of ramee and its application processes in liquefied ammonia solvent dyeing, belong to technical field of textile chemistry.The present invention first pre-processes ramee：Ramee chooses ramie yarn and thread, and ramie yarn and thread is put into the NaOH solution of 200mL a concentration of 15%, is heated to 50 DEG C, keeps the temperature 4h, is cleaned with tap water, until eluate pH is 78 to get to pretreatment yarn；Pretreatment yarn is modified again：10 15mL formaldehyde are added in 250ml three-neck flasks, 1 2mL boric acid and 150mL deionized waters, uniform stirring, are added pretreated ramie yarn and thread, reaction temperature is increased to 40 DEG C, it is passed through ammonia again, return stirring reacts 3 hours, after the completion of reaction, yarn is taken out, it is rinsed with deionized water, by drying yarn to get ammoniation modified ramie yarn and thread when eluate pH is 67.By the ammoniation modified method of ramee of the present invention in ramee liquefied ammonia solvent dyeing, the dye uniformity of ramee can be significantly improved.
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 and important people's livelihood industry and international competitive advantage of Chinese national economy
Apparent industry, ramee are one of primary raw materials of textile fabric, are occupied an important position in textile fabric.China is generation
Mainly there are ramie, sisal hemp, flax and yellow mestha etc. in most abundant one of the country of hemp resource in boundary, wherein ramie is with growth
The advantages that speed is fast, yield is high, easy survival is planted extensively in China.The fabric that ramee is made into has ventilative, moisture absorbing and sweat releasing
The advantages that, it is ideal summer high-grade clothing fabric.
In recent years, China's textile industry ecological circulation economic development contradiction becomes increasingly conspicuous, the height of water resource is relied on and
Environmental problem caused by maximum discharge seriously restricts the sustainable development of the sector.According to statistics, China's textile printing and dyeing industry year is consumed
1,700,000,000 tons of water, disposal of pollutants is up to 1,600,000,000 tons.Compared with foreign countries, the water consumption of China's textile printing and dyeing industry is the 2-3 of foreign countries
Times, energy consumption is 3-5 times of foreign countries.In order to solve the problems, such as high energy consumption, applicants studied the non-aqueous dyeings of ramee, i.e., will
Ramee is put into liquefied ammonia dicyandiamide solution and dyes, and is recycled liquefied ammonia solvent using the volatility of liquefied ammonia.
During this, applicants have discovered that a problem, i.e. ramee molecule and the wellability of liquefied ammonia molecule are poor.
Ramee has preferable compatibility with aqueous solution, this is because it contains many hydrophilic radicals, such as hydrogen-oxygen
Root etc..Applicant has studied the dyeing of ramee in liquefied ammonia system, as a result, it has been found that, profit of the ramee in liquefied ammonia solvent
It is moist poor.When ramie yarn and thread is more, the yarn dyeing effect for being wrapped in the inside is poor, it is found by the applicant that being due to ramie yarn
Line fails complete wetting in liquefied ammonia solvent, uneven so as to cause the dyeing of yarn.Under the same conditions, it is dyed in aqueous solvent
When, preferable coloring can then be obtained by being wrapped in the yarn of the inside.For this problem, applicant proposes to ramie yarn and thread
It carries out ammoniation modified, ramie surface is made to increase more amino.When the amino of ramee is more, according to " similar to mix " former
The characteristics of can generating hydrogen bond or Van der Waals force between reason and ramee and amino molecule, ramee will preferably infiltrate
In liquefied ammonia solvent, to realize the dyeing in liquefied ammonia solvent.
Currently, the ammoniation modified report of ramee is less, wherein there is an amination modifying about ramee
Patent report, application No. is 88100237.2 patent applications to disclose a kind of process for ammoniation modifying of ramie fibre, which uses
Sodium hydroxide solution carries out the crystalline substance that disappears to ramee, then use 1- chlorine-2-hydroxyl propyl tri alkyl ammomium chlorides for aminating agent into
Row aminating reaction, the reaction have effectively achieved the amido that electrically charged cation is introduced on ramee surface, chemistry knot
Structure formula isBut the present invention is to introduce uncharged amino in fiber surface, chemical structural formula is-NH2, with
The former has the difference of essence.
Requirement of the domestic and international market to ecological textile and environmental protection is higher and higher, the need of few water or waterless staining technique
It asks increasing, in order to realize such novel technical method, there are several technical barriers to need further to break through in the process.This hair
Bright application is exactly to realize that ramee dyes in liquefied ammonia dicyandiamide solution and invents.
Invention content
The present invention is directed to problem and the shortcomings of the prior art pointed in background technology, it is an object of the invention to
A kind of ammoniation modified method for providing ramee and its application process in liquefied ammonia solvent dyeing make ramie surface increase more
More amino.It, can be between principle and ramee and amino molecule according to " similar to mix " when the amino of ramee is more
The characteristics of generating hydrogen bond or Van der Waals force, ramee will preferably infiltrate in liquefied ammonia solvent, to realize liquefied ammonia solvent
In dyeing.
In order to realize that the above-mentioned purpose of the present invention, inventor pass through a large amount of experimental study, it is fine to have developed a kind of ramie
The ammoniation modified method of dimension, which is characterized in that described method includes following steps：
(1) pretreatment of ramee：Ramee chooses ramie yarn and thread, and 2-5g ramie yarn and threads are put into 200mL concentration
For 15% NaOH solution, be heated to 50 DEG C, keep the temperature 4h, cleaned with tap water, until eluate pH be 7-8 to get to
Pre-process yarn；This step is to carry out alkali process to ramee, to make ramee occur to moisten puffing phenomenon, makes cellulose
Become high resilience and gloss, while the low polymerization degree in cellulose being made to be partly dissolved, to improve the equal of molecular weight cellulose
One property makes the physicochemical change of fiber and structure variation chemically react ability to improve fiber itself；
(2) method of modifying：10-15mL formaldehyde, 1-2mL boric acid and 150mL deionizations are added in 250ml three-neck flasks
Water, uniform stirring are added the pretreated 1-2g ramie yarn and threads of step (1), reaction temperature are increased to 40 DEG C, then be passed through ammonia
Gas, return stirring react 3 hours, after the completion of reaction, yarn are taken out, is rinsed with deionized water, will when eluate pH is 6-7
Drying yarn is to get ammoniation modified ramie yarn and thread；
(3) modified yarn and unmodified yarn are done into elemental analysis, obtains following result：
From elemental analysis result：Ramie yarn and thread is by modified, and essential element carbon (C), hydrogen (H) are without apparent
Variation, and nitrogen content obviously increases, up to 9-16 times of amplification, illustrates amino (- NH2) be successfully grafted on fiber.
Further, the reaction in above-mentioned technical proposal in step (2) method of modifying can be indicated with following equation：
Above-mentioned reaction is reacted for Mannich, and 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 obtain
Ammoniation modified ramie yarn and thread.
The present invention also provides a kind of ammoniation modified application processes in liquefied ammonia solvent dyeing of above-mentioned ramee, special
Sign is that described method includes following 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 will be dissolved in liquefied ammonia is dissolved in
In liquefied ammonia, ammoniation modified ramie yarn and thread and unmodified yarn is immersed in liquefied ammonia dye liquor dyes respectively, dyeing condition
For：Dye dosage 10-15% (o.m.f), bath raio 1：20, dyeing time 20-50 seconds obtains product dyed thereby；
Second step observes this product dyed thereby, as a result, it has been found that, ammoniation modified ramie yarn and thread product dyed thereby color is uniform, and no pattern is existing
As yarn and the yarn dyeing effect of outside for being wrapped in the inside are consistent；Unmodified yarn dyeing object surface color is more equal
Even, without apparent pattern phenomenon, the yarn dyeing for being wrapped in the inside is uneven on surface.
Compared with prior art, the present invention has following advantageous effect：
(1) present invention carries out ramee ammoniation modified, and ramee surface is made to increase more amino.When ramie fibre
When the amino of dimension is more, hydrogen bond or Van der Waals force can be generated according to " similar to mix " between principle and ramee and amino molecule
The characteristics of, ramee will preferably infiltrate in liquefied ammonia solvent, to realize the dyeing in liquefied ammonia solvent；
(2) ammoniation modified ramie yarn and thread has good wellability in liquefied ammonia in the present invention, is ramie yarn and thread in liquid
Dyeing in ammonia provides condition, solves the problems such as aberration is inhomogenous in ramie yarn and thread dyeing course；Its application process has dye
Color processing step is few, and dyeing time is short, and dyestuff is can be recycled after dye, and the advantages that reducing environmental pollution is, it can be achieved that ramie yarn and thread
Non-aqueous dyeing requirement in dyeing course.
Specific implementation mode
Form is described in further detail the above of the present invention again by the following examples, but should not manage this
Solution is only limitted to embodiment below for the range of the above-mentioned theme of the present invention, and all technologies 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 it is a concentration of that 2g ramie yarn and threads are put into 200mL
15% NaOH solution, is heated to 50 DEG C, keeps the temperature 4h, is cleaned with tap water, until eluate pH is 7.6 to get to pre-
Handle yarn.
(2) method of modifying：10mL formaldehyde, 1mL boric acid and 150mL deionized waters are added in 250ml three-neck flasks, uniformly
Stirring is added the pretreated 1g ramie yarn and threads of step (1), reaction temperature is increased to 40 DEG C, then be passed through ammonia, reflux is stirred
Reaction 3 hours is mixed, after the completion of reaction, yarn is taken out, is rinsed with deionized water, by drying yarn when eluate pH is 6-7,
Up to ammoniation modified ramie yarn and thread.
(3) modified yarn and unmodified yarn are done into elemental analysis, obtains following result：
From elemental analysis result：Ramie yarn and thread is by modified, and essential element carbon (C), hydrogen (H) are without apparent
Variation, and nitrogen content obviously increases, and increases about 13 times of multiple, illustrates amino (- NH2) be successfully grafted on fiber.
The ammoniation modified application process in liquefied ammonia solvent dyeing of ramee：
The ammoniation modified ramie yarn and thread and unmodified yarn that the step of first step, selection certain mass (2) obtains, by ammonia
Change modified ramie yarn and unmodified yarn is wound in closely knit a branch of, the reactive dye activity that will be dissolved in liquefied ammonia respectively
Red 195 are dissolved in liquefied ammonia, ammoniation modified ramie yarn and thread and unmodified yarn are immersed in liquefied ammonia dye liquor contaminate respectively
Color, dye dosage 15% (o.m.f), bath raio 1：20, dyeing time obtains product dyed thereby under conditions of 20 seconds.
Second step observes this product dyed thereby, as a result, it has been found that：Ammoniation modified ramie yarn and thread product dyed thereby color is uniform, and no pattern is existing
As yarn and the yarn dyeing effect of outside for being wrapped in the inside are consistent；Unmodified yarn dyeing object surface color is more equal
Even, without apparent pattern phenomenon, the yarn dyeing for being wrapped in the inside is uneven on surface.
Embodiment 2
(1) pretreatment of ramee：Ramee chooses ramie yarn and thread, and it is a concentration of that 2g ramie yarn and threads are put into 200mL
15% NaOH solution, is heated to 50 DEG C, keeps the temperature 4h, is cleaned with tap water, until eluate pH is 7.3 to get to pre-
Handle yarn.
(2) method of modifying：12mL formaldehyde, 1.5mL boric acid and 150mL deionized waters are added in 250ml three-neck flasks,
Even stirring is added the pretreated 1g ramie yarn and threads of step (1), reaction temperature is increased to 40 DEG C, then be passed through ammonia, flows back
It is stirred to react 3 hours, after the completion of reaction, yarn is taken out, is rinsed with deionized water, dry yarn when eluate pH is 6-7
It does to get ammoniation modified ramie yarn and thread.
(3) modified yarn and unmodified yarn are done into elemental analysis, obtains following result：
From elemental analysis result：Ramie yarn and thread is by modified, and essential element carbon (C), hydrogen (H) are without apparent
Variation, and nitrogen content obviously increases, and increases about 11 times of multiple, illustrates amino (- NH2) be successfully grafted on fiber.
The ammoniation modified application process in liquefied ammonia solvent dyeing of ramee：
The ammoniation modified ramie yarn and thread and unmodified yarn that the step of first step, selection certain mass (2) obtains, by ammonia
Change modified ramie yarn and unmodified yarn is wound in closely knit a branch of, the reactive dye activity that will be dissolved in liquefied ammonia respectively
Red 195 are dissolved in liquefied ammonia, ammoniation modified ramie yarn and thread and unmodified yarn are immersed in liquefied ammonia dye liquor contaminate respectively
Color, dye dosage 10% (o.m.f), bath raio 1：20, dyeing time obtains product dyed thereby under conditions of 30 seconds.
Second step observes this product dyed thereby, as a result, it has been found that：Ammoniation modified ramie yarn and thread product dyed thereby color is uniform, and no pattern is existing
As yarn and the yarn dyeing effect of outside for being wrapped in the inside are consistent；Unmodified yarn dyeing object surface color is more equal
Even, without apparent pattern phenomenon, the yarn dyeing for being wrapped in the inside is uneven on surface.
Embodiment 3
(1) pretreatment of ramee：Ramee chooses ramie yarn and thread, and it is a concentration of that 2g ramie yarn and threads are put into 200mL
15% NaOH solution, is heated to 50 DEG C, keeps the temperature 4h, is cleaned with tap water, until eluate pH is 7.1 to get to pre-
Handle yarn.
(2) method of modifying：12mL formaldehyde, 1.5mL boric acid and 150mL deionized waters are added in 250ml three-neck flasks,
Even stirring is added the pretreated 1g ramie yarn and threads of step (1), reaction temperature is increased to 40 DEG C, then be passed through ammonia, flows back
It is stirred to react 3 hours, after the completion of reaction, yarn is taken out, is rinsed with deionized water, dry yarn when eluate pH is 6-7
It does to get ammoniation modified ramie yarn and thread.
(3) modified yarn and unmodified yarn are done into elemental analysis, obtains following result：
From elemental analysis result：Ramie yarn and thread is by modified, and essential element carbon (C), hydrogen (H) are without apparent
Variation, and nitrogen content obviously increases, and increases about 9 times of multiple, illustrates amino (- NH2) be successfully grafted on fiber.
The ammoniation modified application process in liquefied ammonia solvent dyeing of ramee：
The ammoniation modified ramie yarn and thread and unmodified yarn that the step of first step, selection certain mass (2) obtains, by ammonia
Change modified ramie yarn and unmodified yarn is wound in closely knit a branch of, the reactive dye activity that will be dissolved in liquefied ammonia respectively
Red 195 are dissolved in liquefied ammonia, ammoniation modified ramie yarn and thread and unmodified yarn are immersed in liquefied ammonia dye liquor contaminate respectively
Color, dye dosage 15% (o.m.f), bath raio 1：20, dyeing time obtains product dyed thereby under conditions of 40 seconds.
Second step observes this product dyed thereby, as a result, it has been found that：Ammoniation modified ramie yarn and thread product dyed thereby color is uniform, and no pattern is existing
As yarn and the yarn dyeing effect of outside for being wrapped in the inside are consistent；Unmodified yarn dyeing object surface color is more equal
Even, without apparent pattern phenomenon, the yarn dyeing for being wrapped in the inside is uneven on surface.
Embodiment 4
(1) pretreatment of ramee：Ramee chooses ramie yarn and thread, and it is a concentration of that 2g ramie yarn and threads are put into 200mL
15% NaOH solution, is heated to 50 DEG C, keeps the temperature 4h, is cleaned with tap water, until eluate pH is 7.5 to get to pre-
Handle yarn.
(2) method of modifying：15mL formaldehyde, 2mL boric acid and 150mL deionized waters are added in 250ml three-neck flasks, uniformly
Stirring is added the pretreated 1.5g ramie yarn and threads of step (1), reaction temperature is increased to 40 DEG C, then be passed through ammonia, flows back
It is stirred to react 3 hours, after the completion of reaction, yarn is taken out, is rinsed with deionized water, dry yarn when eluate pH is 6-7
It does to get ammoniation modified ramie yarn and thread.
(3) modified yarn and unmodified yarn are done into elemental analysis, obtains following result：
From elemental analysis result：Ramie yarn and thread is by modified, and essential element carbon (C), hydrogen (H) are without apparent
Variation, and nitrogen content obviously increases, up to 16 times of amplification, illustrates amino (- NH2) be successfully grafted on fiber.
The ammoniation modified application process in liquefied ammonia solvent dyeing of ramee：
The ammoniation modified ramie yarn and thread and unmodified yarn that the step of first step, selection certain mass (2) obtains, by ammonia
Change modified ramie yarn and unmodified yarn is wound in closely knit a branch of, the reactive dye activity that will be dissolved in liquefied ammonia respectively
Red 195 are dissolved in liquefied ammonia, ammoniation modified ramie yarn and thread and unmodified yarn are immersed in liquefied ammonia dye liquor contaminate respectively
Color, dye dosage 15% (o.m.f), bath raio 1：20, dyeing time obtains product dyed thereby under conditions of 50 seconds.
Second step observes this product dyed thereby, as a result, it has been found that：Ammoniation modified ramie yarn and thread product dyed thereby color is uniform, and no pattern is existing
As yarn and the yarn dyeing effect of outside for being wrapped in the inside are consistent；Unmodified yarn dyeing object surface color is more equal
Even, without apparent pattern phenomenon, the yarn dyeing for being wrapped in the inside is uneven on surface.
Embodiment 5
(1) pretreatment of ramee：Ramee chooses ramie yarn and thread, and it is a concentration of that 2g ramie yarn and threads are put into 200mL
15% NaOH solution, is heated to 50 DEG C, keeps the temperature 4h, is cleaned with tap water, until eluate pH is 7.4 to get to pre-
Handle yarn.
(2) method of modifying：13mL formaldehyde, 1.5mL boric acid and 150mL deionized waters are added in 250ml three-neck flasks,
Even stirring is added the pretreated 1g ramie yarn and threads of step (1), reaction temperature is increased to 40 DEG C, then be passed through ammonia, flows back
It is stirred to react 3 hours, after the completion of reaction, yarn is taken out, is rinsed with deionized water, dry yarn when eluate pH is 6-7
It does to get ammoniation modified ramie yarn and thread.
(3) modified yarn and unmodified yarn are done into elemental analysis, obtains following result：
From elemental analysis result：Ramie yarn and thread is by modified, and essential element carbon (C), hydrogen (H) are without apparent
Variation, and nitrogen content obviously increases, up to 11 times of amplification, illustrates amino (- NH2) be successfully grafted on fiber.
The ammoniation modified application process in liquefied ammonia solvent dyeing of ramee：
The ammoniation modified ramie yarn and thread and unmodified yarn that the step of first step, selection certain mass (2) obtains, by ammonia
Change modified ramie yarn and unmodified yarn is wound in closely knit a branch of, the reactive dye activity that will be dissolved in liquefied ammonia respectively
Red 195 are dissolved in liquefied ammonia, ammoniation modified ramie yarn and thread and unmodified yarn are immersed in liquefied ammonia dye liquor contaminate respectively
Color, dye dosage 12% (o.m.f), bath raio 1：20, dyeing time obtains product dyed thereby under conditions of 30 seconds.
Second step observes this product dyed thereby, as a result, it has been found that：Ammoniation modified ramie yarn and thread product dyed thereby color is uniform, and no pattern is existing
As yarn and the yarn dyeing effect of outside for being wrapped in the inside are consistent；Unmodified yarn dyeing object surface color is more equal
Even, without apparent pattern phenomenon, the yarn dyeing for being wrapped in the inside is uneven on surface.
Claims (2)
1. a kind of ammoniation modified method of ramee, which is characterized in that described method includes following steps：
(1) pretreatment of ramee：Ramee chooses ramie yarn and thread, and it is a concentration of that 2-5g ramie yarn and threads are put into 200mL
15% NaOH solution, is heated to 50 DEG C, keeps the temperature 4h, is cleaned with tap water, until eluate pH is 7-8 to get to pre-
Handle yarn；
(2) method of modifying：10-15mL formaldehyde, 1-2mL boric acid and 150mL deionized waters are added in 250ml three-neck flasks,
Even stirring is added the pretreated 1-2g ramie yarn and threads of step (1), reaction temperature is increased to 40 DEG C, then be passed through ammonia, returns
Stream is stirred to react 3 hours, after the completion of reaction, and yarn is taken out, is rinsed with deionized water, by yarn when eluate pH is 6-7
Drying is to get ammoniation modified ramie yarn and thread；
(3) modified yarn and unmodified yarn are done into elemental analysis, obtains following result：
From elemental analysis result：By modified, essential element carbon (C), hydrogen (H) do not become significantly ramie yarn and thread
Change, and nitrogen content obviously increases, up to 9-16 times of amplification, illustrates amino (- NH2) 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 indicated with following equation：
Above-mentioned reaction is reacted for Mannich, and 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 obtain ammonification
Modified ramie yarn.
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| CN108660517A (en) * | 2017-09-14 | 2018-10-16 | 曾庆福 | The energy saving and environment friendly keen-witted and capable ramie stripes production system of one kind and its production technology |
| CN108532327B (en) * | 2018-04-24 | 2023-08-11 | 武汉纺织大学 | Method for improving reactive dye liquid ammonia dyeing fixation rate |
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| CN103242454A (en) * | 2013-05-13 | 2013-08-14 | 宜兴市通达化学有限公司 | Method for preparing high-substitution degree ammonium carboxymethyl cellulose by means of mixed strong acid |
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