CN108588881A - A kind of preparation method of the regenerated celulose fibre containing natural dye - Google Patents
A kind of preparation method of the regenerated celulose fibre containing natural dye Download PDFInfo
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- CN108588881A CN108588881A CN201810278240.6A CN201810278240A CN108588881A CN 108588881 A CN108588881 A CN 108588881A CN 201810278240 A CN201810278240 A CN 201810278240A CN 108588881 A CN108588881 A CN 108588881A
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- Prior art keywords
- natural dye
- gel
- sol
- preparation
- regenerated celulose
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Classifications
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
- D01F2/16—Addition of dyes to the spinning solution
Abstract
The invention discloses a kind of preparation methods of the regenerated celulose fibre containing natural dye, specifically the natural dye collosol and gel being prepared using sol-gal process is made after being mixed with rayon spinning liquid after dispersion liquid and carries out wet spinning, regenerated celulose fibre is made.Original liquid coloring fiber produced by the present invention has preferably every color fastness, while having better feel, solves the problems, such as that current natural dye is taken by unqualified the brought production of every color fastness.
Description
Technical field
The present invention relates to textile industry raw material and its manufacturing methods, and in particular to a kind of regeneration containing natural dye
The preparation method of cellulose fibre.
Background technology
Natural dye is broadly divided into three categories:Natural plant dye, natural animal dyestuff and natural mineral matter dyestuff.Naturally
Vegetable colour mainly extracted from the root of various plants, leaf, stem and fruit, bark and flower, as ginger, pomegranate, it is indigo,
Yellow Fructus Gardeniae, tea tree, mulberry tree etc.;The type of natural animal dyestuff is less, usually extracted from cochineal and shellfish and
Come, such as kermes, shellac, alkermes;Natural mineral matter dyestuff is the colored inorganic object extracted from various mineral
Matter, such as manganese brown, chrome yellow, ultramarine.
In recent years, part chemical dye containing toxic component because that can cause skin allergy occur, redness, inflammation, suppurate
Symptom or even some chemical dyes contain carcinogen;Simultaneously at present the raw material of many chemical dyes all derive from coal and
Oil.Coal, oil are more in many sector applications, and consumption is very fast, non-renewable, and excessive use can cause resource exhaustion;And
And the treatment of dyeing wastewater difficulty that chemical dye generates in dyeing course is larger, cost is higher, is not easy to recycle, and is easy to make
At environmental pollution.And natural dye is environmental protection, healthy dyestuff, biological degradability is good, good with ecological environment compatibility, and
Nontoxic, to no skin irritation and carcinogenicity, and its source is renewable, while natural dye dying waste water not will produce
The water pollution problems that waste water from dyestuff is caused is learned, the intractabilities such as waste water decoloring are smaller, have good research and development foreground.
But that there is also dye-uptakes is low, every color fastness is low and expensive etc. many for the dyeing of natural dye at present
The relatively low problem of disadvantage, especially color fastness, significantly limits the application of natural dye.
Invention content
In view of the deficiencies of the prior art, the object of the present invention is to provide a kind of regeneration safe and environment-friendly, that color fastness is excellent is fine
The preparation method of cellulose fiber, by the spinning solution that adds natural dye after sol-gel technique coats, spinning system
Obtain the regenerated celulose fibre with preferable properties.
The present invention realizes in the following way:
A kind of preparation method of the regenerated celulose fibre containing natural dye, includes the following steps:
Step 1, the preparation of rayon spinning liquid;
Step 2, the natural dye sol-gel and dispersant that are prepared using sol-gel method, solvent are mixed,
Obtain natural dye sol-gel dispersion liquid;
Step 3, after natural dye sol-gel dispersion liquid being mixed with rayon spinning liquid carry out wet spinning to get.
Further, sol-gel method described in step 2 is first that the mixing of metal alkoxide, solvent and natural dye is laggard
Row hydrolysis condensation reaction, then colloidal sol obtained is aged to obtain wet gel, it is then freeze-dried, natural dye is obtained after crushing
Sol-gel.
Further, metal alkoxide is silicon ethyl alcohol or isopropyl titanate in the step 2.
Further, the solvent is ethyl alcohol, isopropanol or butanol.
Further, the natural dye is natural plant dye or natural minerals dyestuff, and natural plant dye is selected from madder
Grass, safflower, Asian puccoon, bush, indigo, pomegranate, Yellow Fructus Gardeniae, tea, Song indigo plants, hispid arthraxon, persimmon, Asian puccoon or ink tree extract, day
Right mineral dye is selected from cinnabar, malachite green, copper oxide or ferroso-ferric oxide.
Further, the mass ratio of metal alkoxide, natural dye and solvent is 10~20:5~10:70~85.
Further, the mass fraction of natural dye sol-gel is in the natural dye sol-gel dispersion liquid
10%~
20%, solvent is water.
Further, the dispersant is one kind in calgon, tristerin or stearate, dosage
It is the 1%~3% of natural dye sol-gel mass fraction.
Further, the grain size of the natural dye sol-gel is 0.1~1 μm.
Further, in step 3 dosage of natural dye sol-gel account for first fibre content in rayon spinning liquid 10%~
15%.
Heretofore described first fibre refers to:Alpha cellulose is also known as alpha-cellulose.Cellulosic material is dipped at 20 DEG C
In 17.5%~18% sodium hydroxide solution after 45 minutes undissolved part.
The present invention utilizes the principle of sol-gel cladding, and natural dye sol-gel powder is made after natural dye is coated
The regenerated celulose fibre of original liquid coloring is prepared afterwards with viscose rayon spinning solution co-blended spinning in end.With utilize natural dye
The fiber of dyeing is compared, and original liquid coloring fiber of the invention has preferably every color fastness, while having better feel, solves
Current natural dye determined since problem is taken in unqualified the brought production of every color fastness.In addition, using sol-gel by day
The form and aspect and color and luster of natural dye are not influenced not only after right coating dye, while natural dye can also be protected from external environment
The variation of color and luster and form and aspect caused by destruction, such as the acid-fast alkali-proof of natural dye are poor, especially the spinning of viscose rayon
Silk process concentrated acid concentrated base can seriously destroy natural dye structure, lead to dye discoloration or colour killing, and utilize sol-gel by day
After right coating dye, it can both ensure that dye structure is not destroyed, and not will produce discoloration, the form and aspect and color of dyestuff will not be changed
Light is more conducive to the use condition and application range for widening natural dye, improves current natural dye and is limited by various conditions
The case where processed.
Specific implementation mode
Embodiment 1
The preparation method of regenerated celulose fibre containing madder
Step 1, the preparation of rayon spinning liquid
Raw material is the wood pulps that the degree of polymerization is 500~600, and first fibre content is more than 90%, according to following process route system
Glue:Dipping, squeezing, crushing, experienced, yellow, continuous-dissolution, filtering, deaeration.
It is 5.8% that gained rayon spinning liquid first fibre content, which is 9.0%, NaOH mass fractions, and viscosity is (falling ball method) 60s,
Ripe degree is (10%NH4Cl)8.9mL。
Step 2, the preparation of natural dye sol-gel powder dispersion system
In reaction kettle, the sol-gel dispersion system that mass fraction is 10%, 15%, 20% is prepared with distilled water, it is molten
Silicon ethyl alcohol in prepared by glue-gel rubber system, madder, ethyl alcohol component ratio be 10:5:85, addition accounts for sol-gel powder quality 2%
Glyceryl tristearate dispersant, be sufficiently stirred and can be obtained more uniform madder sol-gel dispersion liquid.Using sheet frame
Filter is filtered through the double-deck fine cloth, and pressure is in 0.2Mpa hereinafter, obtaining uniform madder sol-gel dispersion liquid.
Step 3, mixing and wet spinning of the viscose solution with madder sol-gel dispersion lotion
Quantitatively madder sol-gel dispersion liquid is added in viscose solution using proportioning pump, and is uniformly mixed.Madder is molten
Glue-gel dispersion liquid uses syringe pump in the speed injection to dynamic mixer of 6 liters/min, the flow of viscose solution is 50
Liter/min stands 1h under room temperature.Wherein, the quality of madder sol-gel is the 3% of first fibre weight.
The mixed solution of madder sol-gel dispersion liquid and viscose glue is sent into wet spinning process and carries out spinning.Spinning head
Specification is 21000 holes × 0.06mm, and spinning speed 55m/min, coagulation bath temperature is 52 DEG C, and plasticizing bath temperature is 95 DEG C.It is solidifying
Gu bath group becomes:Sulfuric acid 115g/L, sodium sulphate 325g/L, zinc sulfate 11.5g/L.
Embodiment 2
The preparation method of regenerated celulose fibre containing Asian puccoon
Step 1, the preparation of rayon spinning liquid
Raw material is the wood pulps that the degree of polymerization is 500~600, and first fibre content is more than 90%, according to following process route system
Glue:Dipping, squeezing, crushing, experienced, yellow, continuous-dissolution, filtering, deaeration.
It is 5.8% that gained rayon spinning liquid first fibre content, which is 9.0%, NaOH mass fractions, and viscosity is (falling ball method) 60s,
Ripe degree is (10%NH4Cl)8.9mL。
Step 2, the preparation of natural dye sol-gel powder dispersion system
In reaction kettle, the sol-gel dispersion system that mass fraction is 10%, 15%, 20% is prepared with distilled water, it is molten
Silicon ethyl alcohol in prepared by glue-gel rubber system, Asian puccoon, ethyl alcohol component ratio be 10:5:85, addition accounts for sol-gel powder quality 2%
Glyceryl tristearate dispersant, be sufficiently stirred and can be obtained more uniform Asian puccoon sol-gel dispersion liquid.Using sheet frame
Filter is filtered through the double-deck fine cloth, and pressure is in 0.2Mpa hereinafter, obtaining uniform Asian puccoon sol-gel dispersion liquid.
Step 3, mixing and wet spinning of the viscose solution with Asian puccoon sol-gel dispersion lotion
Quantitatively Asian puccoon sol-gel dispersion liquid is added in viscose solution using proportioning pump, and is uniformly mixed.Asian puccoon is molten
Glue-gel dispersion liquid uses syringe pump in the speed injection to dynamic mixer of 6 liters/min, the flow of viscose solution is 50
Liter/min stands 1h under room temperature.Wherein, the quality of Asian puccoon sol-gel is the 3% of first fibre weight.
The mixed solution of Asian puccoon sol-gel dispersion liquid and viscose glue is sent into wet spinning process and carries out spinning.Spinning head
Specification is 21000 holes × 0.06mm, and spinning speed 55m/min, coagulation bath temperature is 52 DEG C, and plasticizing bath temperature is 95 DEG C.It is solidifying
Gu bath group becomes:Sulfuric acid 115g/L, sodium sulphate 325g/L, zinc sulfate 11.5g/L.
Embodiment 3
The preparation method of regenerated celulose fibre containing malachite green
Step 1, the preparation of rayon spinning liquid
Raw material is the wood pulps that the degree of polymerization is 500~600, and first fibre content is more than 90%, according to following process route system
Glue:Dipping, squeezing, crushing, experienced, yellow, continuous-dissolution, filtering, deaeration.
It is 5.8% that gained rayon spinning liquid first fibre content, which is 9.0%, NaOH mass fractions, and viscosity is (falling ball method) 60s,
Ripe degree is (10%NH4Cl)8.9mL。
Step 2, the preparation of natural dye sol-gel powder dispersion system
In reaction kettle, the sol-gel dispersion system that mass fraction is 10%, 15%, 20% is prepared with distilled water, it is molten
Silicon ethyl alcohol in prepared by glue-gel rubber system, malachite green, ethyl alcohol component ratio be 10:5:85, addition accounts for sol-gel powder matter
The glyceryl tristearate dispersant of amount 2%, is sufficiently stirred and can be obtained more uniform madder sol-gel dispersion liquid.It adopts
It is filtered through the double-deck fine cloth with sheet frame filter, pressure is in 0.2Mpa hereinafter, obtaining uniform malachite sol-gel dispersion liquid.
Step 3, mixing and wet spinning of the viscose solution with malachite sol-gel dispersion lotion
Quantitatively malachite sol-gel dispersion liquid is added in above-mentioned for use viscose solution using proportioning pump, and is mixed
It closes uniform.Malachite sol-gel dispersion liquid uses syringe pump in the speed injection to dynamic mixer of 6 liters/min, viscose glue
The flow of solution is 50 liters/min, and 1h is stood under room temperature.Wherein, the quality of malachite sol-gel is the 3% of first fibre weight.
The mixed solution of malachite sol-gel dispersion liquid and viscose glue is sent into wet spinning process and carries out spinning.Spinneret
Head specification is 21000 holes × 0.06mm, and spinning speed 55m/min, coagulation bath temperature is 52 DEG C, and plasticizing bath temperature is 95 DEG C.
Coagulation bath composition is:Sulfuric acid 115g/L, sodium sulphate 325g/L, zinc sulfate 11.5g/L.
Embodiment 4
Preparation method containing indigo regenerated celulose fibre
Step 1, the preparation of rayon spinning liquid
Raw material is the wood pulps that the degree of polymerization is 500~600, and first fibre content is more than 90%, according to following process route system
Glue:Dipping, squeezing, crushing, experienced, yellow, continuous-dissolution, filtering, deaeration.
It is 5.8% that gained rayon spinning liquid first fibre content, which is 9.0%, NaOH mass fractions, and viscosity is (falling ball method) 60s,
Ripe degree is (10%NH4Cl)8.9mL。
Step 2, the preparation of natural dye sol-gel powder dispersion system
In reaction kettle, the sol-gel dispersion system that mass fraction is 10%, 15%, 20% is prepared with distilled water, it is molten
Silicon ethyl alcohol, indigo, ethyl alcohol component ratio are 10 in prepared by glue-gel rubber system:5:85, addition accounts for sol-gel powder quality 2%
Glyceryl tristearate dispersant, be sufficiently stirred and can be obtained more uniform indigosol-gel dispersion liquid.Using sheet frame
Filter is filtered through the double-deck fine cloth, and pressure is in 0.2Mpa hereinafter, obtaining uniform indigosol-gel dispersion liquid.
Step 3, mixing and wet spinning of the viscose solution with indigosol-gel dispersion lotion
Quantitatively indigosol-gel dispersion liquid is added in above-mentioned for use viscose solution using proportioning pump, and is mixed
Uniformly.Indigosol-gel dispersion liquid uses syringe pump in the speed injection to dynamic mixer of 6 liters/min, viscose solution
Flow be 50 liters/min, stand 1h under room temperature.Wherein, the quality of indigosol-gel is the 3% of first fibre weight.
The mixed solution of indigosol-gel dispersion liquid and viscose glue is sent into wet spinning process and carries out spinning.Spinning head
Specification is 21000 holes × 0.06mm, and spinning speed 55m/min, coagulation bath temperature is 52 DEG C, and plasticizing bath temperature is 95 DEG C.It is solidifying
Gu bath group becomes:Sulfuric acid 115g/L, sodium sulphate 325g/L, zinc sulfate 11.5g/L.
The fiber that spinning in above-described embodiment is obtained is by spinning, weaving, the fabric of the fiber such as dyeing and finishing, to fabric into
Row items color fastness test, obtained result are as follows:
Fabric | It is acidproof | It is alkaline-resisting | It is water-fast | Dry fastness | Fastness to wet rubbing | Light fastness |
Embodiment 1 | 4 | 4 | 4-5 | 3-4 | 3 | 3-4 |
Embodiment 2 | 4 | 4-5 | 4-5 | 3-4 | 3 | 3-4 |
Embodiment 3 | 4 | 4 | 4 | 4 | 3-4 | 3-4 |
Embodiment 4 | 4 | 4 | 4 | 4 | 3 | 3-4 |
From the test result of upper table can be seen that by after natural dye sol gel with rayon spinning liquid co-blended spinning
Fabric made of colored fibre obtained has preferable every fastness properties, the index that can reach national regulations to want afterwards
It asks.
Claims (10)
1. a kind of preparation method of the regenerated celulose fibre containing natural dye, it is characterised in that:Include the following steps:
Step 1, the preparation of rayon spinning liquid;
Step 2, the natural dye sol-gel and dispersant that are prepared using sol-gel method, solvent are mixed, is obtained
Natural dye sol-gel dispersion liquid;
Step 3, after natural dye sol-gel dispersion liquid being mixed with rayon spinning liquid carry out wet spinning to get.
2. the preparation method of the regenerated celulose fibre according to claim 1 containing natural dye, it is characterised in that:Step
Sol-gel method described in rapid 2 is first will to carry out hydrolysis condensation reaction after the mixing of metal alkoxide, solvent and natural dye, then incite somebody to action
Colloidal sol obtained is aged to obtain wet gel, is then freeze-dried, and natural dye sol-gel is obtained after crushing.
3. the preparation method of the regenerated celulose fibre according to claim 2 containing natural dye, it is characterised in that:Institute
It is silicon ethyl alcohol or isopropyl titanate to state metal alkoxide.
4. the preparation method of the regenerated celulose fibre according to claim 2 containing natural dye, it is characterised in that:Institute
It is ethyl alcohol, isopropanol or butanol to state solvent.
5. the preparation method of the regenerated celulose fibre according to claim 2 containing natural dye, it is characterised in that:Institute
It is natural plant dye or natural minerals dyestuff to state natural dye, and natural plant dye is selected from madder, safflower, Asian puccoon, bush, indigo
Indigo plant, pomegranate, Yellow Fructus Gardeniae, tea, Song indigo plants, hispid arthraxon, persimmon, Asian puccoon or ink tree extract, natural minerals dyestuff be selected from cinnabar, hole
Sparrow malachite green, copper oxide or ferroso-ferric oxide.
6. the preparation method of the regenerated celulose fibre according to claim 2 containing natural dye, it is characterised in that:Gold
The mass ratio for belonging to alkoxide, natural dye and solvent is 10~20:5~10:70~85.
7. the preparation method of the regenerated celulose fibre according to claim 1 containing natural dye, it is characterised in that:Institute
The mass fraction for stating natural dye sol-gel in natural dye sol-gel dispersion liquid is 10%~20%, and solvent is water.
8. the preparation method of the regenerated celulose fibre according to claim 1 containing natural dye, it is characterised in that:Institute
It is one kind in calgon, tristerin or stearate to state dispersant, and dosage is natural dye sol-gel
The 1%~3% of mass fraction.
9. the preparation method of the regenerated celulose fibre according to claim 1 containing natural dye, it is characterised in that:Institute
The grain size for stating natural dye sol-gel is 0.1~1 μm.
10. the preparation method of the regenerated celulose fibre according to claim 1 containing natural dye, it is characterised in that:
The dosage of natural dye sol-gel accounts for 10%~15% of first fibre content in rayon spinning liquid in step 3.
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CN201810278240.6A CN108588881A (en) | 2018-03-30 | 2018-03-30 | A kind of preparation method of the regenerated celulose fibre containing natural dye |
PCT/CN2018/097861 WO2019184170A1 (en) | 2018-03-30 | 2018-08-01 | Method for manufacturing regenerated cellulose fiber using natural dye |
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CN201810278240.6A CN108588881A (en) | 2018-03-30 | 2018-03-30 | A kind of preparation method of the regenerated celulose fibre containing natural dye |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN115652458A (en) * | 2022-11-15 | 2023-01-31 | 杭州唯铂莱生物科技有限公司 | Antibacterial blend fiber and preparation method thereof |
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JPH0544159A (en) * | 1991-08-05 | 1993-02-23 | Nagase Sangyo Kk | Coloring of fiber |
CN101713103A (en) * | 2009-12-17 | 2010-05-26 | 河北吉藁化纤有限责任公司 | Production method of colored bamboo pulp viscose fiber |
CN105482562A (en) * | 2015-12-30 | 2016-04-13 | 江南大学 | Preparation method of N-methyl morpholine-N-oxide-based color paste |
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DE19818891A1 (en) * | 1998-04-28 | 1999-11-04 | Wolff Walsrode Ag | Process for the production of transparent colored cellulose casings |
CN1233887C (en) * | 2004-03-31 | 2005-12-28 | 宜宾丝丽雅股份有限公司 | Method for fabricating colored viscose fiber |
CN100494524C (en) * | 2007-05-17 | 2009-06-03 | 山东海龙股份有限公司 | Method for preparing cellulose and silicon dioxide composite coloured fiber and coloured fiber made thereby |
CN105970329B (en) * | 2016-05-26 | 2018-09-18 | 罗莱生活科技股份有限公司 | A kind of preparation method of colour viscose rayon |
CN106245375B (en) * | 2016-09-21 | 2018-06-01 | 佛山市南海德耀翔胜纺织有限公司 | A kind of dyestuff and its preparation and colouring method based on cellulose base aeroge |
-
2018
- 2018-03-30 CN CN201810278240.6A patent/CN108588881A/en active Pending
- 2018-08-01 WO PCT/CN2018/097861 patent/WO2019184170A1/en active Application Filing
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0544159A (en) * | 1991-08-05 | 1993-02-23 | Nagase Sangyo Kk | Coloring of fiber |
CN101713103A (en) * | 2009-12-17 | 2010-05-26 | 河北吉藁化纤有限责任公司 | Production method of colored bamboo pulp viscose fiber |
CN105482562A (en) * | 2015-12-30 | 2016-04-13 | 江南大学 | Preparation method of N-methyl morpholine-N-oxide-based color paste |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN115652458A (en) * | 2022-11-15 | 2023-01-31 | 杭州唯铂莱生物科技有限公司 | Antibacterial blend fiber and preparation method thereof |
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Application publication date: 20180928 |