CN104480558B - It is a kind of can salt-free dyeing regenerated celulose fibre preparation method - Google Patents
It is a kind of can salt-free dyeing regenerated celulose fibre preparation method Download PDFInfo
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Abstract
The present invention relates to textile industry raw material and its manufacturing method, especially it is a kind of can salt-free dyeing regenerated celulose fibre preparation method.Injection technique prepares regenerated celulose fibre with spinning solution blend spinning between this method is mixed or spun before cationic starch solution is taken spinning during preparing regenerated celulose fibre, and crosslinking agent is added in the process and to crosslink between cationic starch and cellulose macromolecule chain and reacts, it is allowed to anchor on fiber macromolecular chain.Contain a large amount of cation group on the regenerated celulose fibre being prepared, it is more preferable to the adsorption effect of the dye matrix with negative electrical charge, promote dye it is not necessary that electrolyte is added in dyeing course, reducing production cost, while energy saving, pollution of the use to environment of excessive inorganic salts is decreased.
Description
Technical field
The present invention relates to textile industry raw material and its manufacturing method, especially it is a kind of can salt-free dyeing regenerated fiber
The preparation method of cellulose fiber.
Background technology
Starch is a kind of poly- polysaccharose substance stored in vegetable kingdom, it is generally with a diameter of 1-10 microns or bigger one
A little particulate forms exists, these particles are mainly deposited in the seed, stem tuber or root of plant.Although starch source spreads all over
Entire plant world, but only a few crop is widely used in the production of commodity starch, and corn is to produce starch most
Main source, it is other to also have wheat, potato, cassava and sweet potato etc..Starch is a kind of high glycan from structure, mainly with
The basic ring that glucose remains base is keyed by α-D- (1 → 4).
Cationic starch be with the hydroxyl in various organic amine compounds and starch molecule containing halogen or epoxy group into
Row etherification reaction, a kind of of generation contain the starch ether derivative that positive charge is carried on amino, nitrogen-atoms.Cationic starch is main
There are tertiary amine salt and quaternary ammonium salt, as the polymer substance with hydrophilic group, not only raw material sources are wide, non-toxic, inexpensive for it,
And product fully biodegradable, it is environmentally safe.Cationic starch is used as detergent additive, has to skin irritation
The characteristics such as low, biological drop property is good, toxicity is low.Cationic starch has many advantages, be therefore widely used in papermaking, weaving,
Oil field, mining industry, sewage disposal, adhesive, cosmetics (lasting agent) and other industry.Low-substituted Cationic Starch is mainly used
In paper industry, cationic starch with high substitution degree is mainly used for water process and anion exchange etc..
Cation-modified regenerated celulose fibre is a kind of by introducing band just in regenerated celulose fibre molecular structure
The group regenerated celulose fibre of charge, to keep entire fiber surface positively charged, and when being dyed due to dyestuff band
Negative electrical charge is easy to have an effect without adding salt to promote to contaminate with positively charged fiber.
Cellulose fiber cation is mostly used into two kinds of approach at present, first, directly to fiber by the way of post-processing
Graft modification is carried out, second is that carrying out graft modification to spinning material in the spinning preparation process of fiber.Former approach is simple, at
This is cheap, but effect is only limitted to surface, and the durability acted on is poor；Latter process is complicated, and technology requires height, but handles
Effect is thorough, and persistence is good, and the two cuts both ways.
The modifying agent that existing cellulose fiber cation modification technology mostly uses for epoxychloropropane aminate and
The method that its derivative passes through the method and cellulose macromolecule chain combination of graft modification.The regeneration being prepared by this method
Fiber is known as modified uniform and complete, and obtained fiber has the characteristics of level dyeing and thoroughly dye.But also have complex process, reaction condition
Harshness, the disadvantages such as grafting rate is low.
Cationic starch is derived from a wealth of sources as one kind, cheap, the environment friendly and pollution-free raw material of industry, many industry all
Have and be extremely widely applied, such as papermaking, weaving, mining industry, sewage disposal, washing chemical industry.But it is used as spinning additive
Make modifying agent, but not yet meets pertinent literature and report.
Invention content
The technical problem to be solved by the present invention is to：It is existing during being cationized to regenerated celulose fibre
Modification be not thorough, be only limitted to the problems such as surface, complex process, it is proposed that it is a kind of can salt-free dyeing regenerated celulose fibre system
Preparation Method, between this method is mixed or spun before cationic starch solution is taken spinning during preparing regenerated celulose fibre
Injection technique prepares regenerated celulose fibre with spinning solution blend spinning, and crosslinking agent is added in the process and makes cationic shallow lake
It crosslinks and reacts between powder and cellulose macromolecule chain, be allowed to anchor on fiber macromolecular chain.
Technical solution：
It is a kind of can salt-free dyeing regenerated celulose fibre preparation method, include the following steps：Cationic starch is led to
It crosses the mode injected between mixing or spinning before spinning to mix with regenerated celulose fibre, and crosslinking agent is added to make ionic starch and fiber
Reaction is crosslinked between element, and the regenerated celulose fibre of cationic starch modification is prepared.
The cationic starch is to be added as a solution；Preferably aqueous solution；Cationic starch is in the solution
Content is 10~20wt%.
The additive amount of the cationic starch is 5~30wt% of the first fibre content of regenerated celulose fibre.
The degree of substitution of the cationic starch is 0.03~0.05, and viscosity is 500~1500mpaS.
The crosslinking agent is the mixing of one or both of glutaraldehyde or glyoxal；Dosage of crosslinking agent is regenerated fiber
3~5wt% of the first fibre content of cellulose fiber.
The dry of the regenerated celulose fibre that the cationic starch is modified is 2.1~2.4cN/dtex by force；It is wet it is strong by 1.3~
1.7cN/dtex；It is dry to stretch 16.0~20.0%.
Advantageous effect
The modifying agent used in the preparation process of cation-dyeable regenerated celulose fibre in the present invention is cationic shallow lake
Powder derives from a wealth of sources, cheap, and it is controllable that each side's surface properties are adjustable, while having reaction condition mildly and environment friendly and pollution-free excellent
Point.Contain a large amount of cation group, the suction to the dye matrix with negative electrical charge on the regenerated celulose fibre being prepared
Attached effect is more preferable, promotees dye it is not necessary that electrolyte is added in dyeing course, is reducing production cost, while energy saving,
Reduce pollution of the use to environment of excessive inorganic salts.
Specific implementation mode
Below by specific implementation mode, invention is further described in detail.But those skilled in the art will manage
Solution, the following example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.Specific skill is not specified in embodiment
Art or condition person (such as write according to technology described in document in the art or condition with reference to Zhao Tao《Dyeing and finishing technology with
Principle》, China Textiles Press, 2009) or carry out according to product description.Production firm is not specified in agents useful for same or instrument
Person, being can be with conventional products that are commercially available.
The value expressed using range format should be interpreted as not only in a flexible way including clearly enumerating as range
The numerical value of limit value, but also include all single numbers or the subinterval covered in the range, like each numerical value and sub-district
Between be expressly recited out.For example, the concentration range of " about 0.1% to about 5% " should be understood as including not only clearly enumerating
About 0.1% to about 5% concentration, 4%) and son further include the single concentration in how (e.g., 1%, 2%, 3% and
Section (for example, 0.1% to 0.5%, 1% to 2.2%, 3.3% to 4.4%).
The present invention is changed using the method for being directly added into cationic starch to what regenerated celulose fibre was cationized
Property, without the method using amination reagent modified cellulose, the reason is that the addition of cationic starch is avoided and is tried using amination
The directly modified spinning solution of agent is influence of the conditions such as required temperature, pH to spinning solution property, in addition cationic starch with
Cellulose belongs to glucose system derivative, and compatibility is good.As the cationic starch and fibre with glucose for most basic unit
The plain structure of dimension is similar, and property is close, there is good intersolubility, itself therebetween can hydrogen bond be combined, crosslinking agent
Introducing makes combination between the two more secured, modification efficiency higher, and effect is more preferable.The introducing of cationic starch can be
Mixed with regenerated celulose fibre before carrying out spinning, can also be during spinning process by way of injection and regenerated fiber
Cellulose fiber mixes.Cationic starch is the e.g. aqueous solution preferably through being added as a solution, and cationic starch is molten
Content in liquid is 10~20wt%.The additive amount of cationic starch be regenerated celulose fibre first fibre content 5~
30wt%, more preferably 10~20wt%.The degree of substitution of the cationic starch is 0.03~0.05, cationic starch solution
Viscosity be 500~1500mpaS.
The preferred glutaraldehyde of crosslinking agent of the present invention and glyoxal are hydroxyl crosslinking agent, but cationic starch and fiber
Hydroxyl in plain macromolecular structure reacts, and more secured, utilization ratio higher is combined to obtain both to make；Dosage of crosslinking agent
For the 1~8wt%, more preferable 3~5wt% of the first fibre content of regenerated celulose fibre.
Dry by modification regeneration cellulose fibre obtained by the above method is 2.1~2.4cN/dtex by force；It is wet it is strong by 1.3~
1.7cN/dtex；It is dry to stretch 16.0~20.0%.
In following embodiment using regenerated celulose fibre can be prepared by way of routine, routine
Steps flow chart is：Dipping, squeezing, crushing, experienced, yellow, continuous-dissolution, filtering, deaeration.After obtained rayon spinning liquid,
Its viscosity is measured by falling ball method, falling ball method refers to time of the 2mm steel balls from the viscose solution needed for the 20cm of whereabouts.
After regenerated celulose fibre has been prepared, by measuring its dyeability, below in an example, adopt
With R-04 dyestuffs to stock-dye, dye uptake % is measured.Dye dosage is 2% (o.w.f), bath raio 50:1,60 DEG C,
30min。
Embodiment 1
The preparation of rayon spinning liquid：
Raw material is the Cotton Pulp that the degree of polymerization is 500~600, and first fibre content is more than 90%, and according to following process route
Glue：Dipping, squeezing, crushing, experienced, yellow, continuous-dissolution, filtering, deaeration.It is fabricated rayon spinning according to above-mentioned technique
Liquid first fibre content is that 8.9%, NaOH mass fractions are 6.0, and viscosity is (falling ball method) 59s, and ripe degree is (10%NH4Cl)
8.8ml。
The preparation of cationic starch solution：
In reaction kettle, the cationic starch solution that mass fraction is 10% is prepared with distilled water, being sufficiently stirred can obtain
Obtain more uniform cationic starch solution.It is filtered through the double-deck fine cloth using sheet frame filter, pressure is in 0.2Mpa hereinafter, obtaining
Even cationic starch solution.
The mixing of viscose glue stoste and cationic starch solution：
Quantitatively cationic starch solution is added in above-mentioned for use viscose solution using proportioning pump, and is uniformly mixed,
As mixture.Cationic starch solution uses syringe pump in the speed injection to dynamic mixer of 6 liters/min, while to mixed
Be added in clutch and account for the glutaraldehyde of first fibre quality 3%, it is made to be uniformly mixed with spinning solution, the flow of viscose solution for 50 liters/
Min stands 1h under room temperature.Wherein, the quality of cationic starch is 0%, 5%, 8%, 15%, 20%, the 30% of first fibre weight.
Wherein 0% additive amount refers to that cationic starch is not added during spinning, is reference examples.
Wet spinning：
It is sent into wet spinning process after cationic starch solution is fully reacted with the mixed solution of viscose glue and carries out spinning.Spray
Silk 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
℃.Coagulation bath composition is：Sulfuric acid 115g/L, sodium sulphate 325g/L, zinc sulfate 11.5g/L.
The leading indicator of fiber by above-mentioned steps preparation is as follows.
| Cationic starch additive amount | 0% | 5% | 8% | 15% | 20% | 30% |
| Fiber number dtex | 1.68 | 1.68 | 1.69 | 1.69 | 1.69 | 1.68 |
| Do strong cN/dtex | 1.98 | 1.96 | 2.01 | 2.31 | 2.10 | 1.92 |
| Wet strong cN/dtex | 1.32 | 1.36 | 1.49 | 1.58 | 1.38 | 1.39 |
| It is dry to stretch % | 16.1 | 15.9 | 16.7 | 17.9 | 17.1 | 15.9 |
| Dye uptake % | 65.2 | 75.5 | 88.3 | 92.4 | 94.5 | 91.1 |
As can be seen from the table, it after by introducing cationic starch in regenerated celulose fibre, can significantly carry
High rate of dyeing, and modified fibre has preferably elasticity and strength character.
Reference examples 1
The modification regeneration cellulose fibre being prepared using the directly modified spinning solution of amination reagent.Testing result：It is fine
Spend 1.69dtex；Do strong 1.97cN/dtex；Wet strong 1.35cN/dtex；It is dry to stretch 17.1%；Dye uptake 68.3%.
Reference examples 2
Regenerated celulose fibre is modified using post processing mode.Testing result：Fiber number 1.68dtex；It is dry strong
1.96cN/dtex；Wet strong 1.41cN/dtex；It is dry to stretch 15.8%；Dye uptake 72.5%.
Embodiment 2
The preparation of rayon spinning liquid：
Raw material is the hemp dissolving pulp that the degree of polymerization is 500~600, and first fibre content is more than 90%, and according to following process route
Glue：Dipping, squeezing, crushing, experienced, yellow, continuous-dissolution, filtering, deaeration.It is fabricated rayon spinning according to above-mentioned technique
Liquid first fibre content is that 8.8%, NaOH mass fractions are 6.0, and viscosity is (falling ball method) 55s, and ripe degree is (10%NH4Cl)
8.7ml。
The preparation of cationic starch solution：
In reaction kettle, the cationic starch solution that mass fraction is 15% is prepared with distilled water, being sufficiently stirred can obtain
Obtain more uniform cationic starch solution.It is filtered through the double-deck fine cloth using sheet frame filter, pressure is in 0.2Mpa hereinafter, obtaining
Even cationic starch solution.
The mixing of viscose glue stoste and cationic starch solution：
Quantitatively cationic starch solution is added in above-mentioned for use viscose solution using proportioning pump, and is uniformly mixed.
Cationic starch solution uses syringe pump in the speed injection to dynamic mixer of 6 liters/min, while respectively into mixer
The glutaraldehyde for the first fibre quality 1%, 3%, 4%, 5%, 8% for accounting for regenerated celulose fibre is added, it is made to be mixed with spinning solution
Uniformly, the flow of viscose solution is 50 liters/min, and 1h is stood under room temperature.Wherein, the quality of cationic starch is regenerated cellulose
The 15% of the first fibre weight of fiber.
Wet spinning：After cationic starch solution is fully reacted with the mixed solution of viscose glue be sent into wet spinning process into
Row spinning.Spinning head specification is 21000 holes × 0.06mm, and spinning speed 55m/min, coagulation bath temperature is 52 DEG C, plasticizing-bath
Temperature is 95 DEG C.Coagulation bath composition is：Sulfuric acid 115g/L, sodium sulphate 325g/L, zinc sulfate 11.5g/L.
The leading indicator of fiber by above-mentioned steps preparation is as follows.
| Crosslinking agent additive amount | 1% | 3% | 4% | 5% | 8% |
| Fiber number dtex | 1.68 | 1.69 | 1.69 | 1.69 | 1.68 |
| Do strong cN/dtex | 1.91 | 2.04 | 2.39 | 2.05 | 1.93 |
| Wet strong cN/dtex | 1.36 | 1.49 | 1.62 | 1.38 | 1.39 |
| It is dry to stretch % | 15.7 | 15.5 | 18.3 | 16.5 | 16.3 |
| Dye uptake % | 85.6 | 86.4 | 91.5 | 90.5 | 83.5 |
It can be seen from the table, the regulation and control of the dosage of crosslinking agent can be significantly increased into rate of dyeing, and change in preferred scope
Property fiber have preferably elasticity and strength character.
Embodiment 3
The preparation of rayon spinning liquid：
Raw material is the bamboo pulp that the degree of polymerization is 500~600, and first fibre content is more than 90%, and according to following process route
Glue：
It is 5.9 that according to above-mentioned technique, to be fabricated rayon spinning liquid first fibre content, which be 9.1%, NaOH mass fractions, viscosity
For (falling ball method) 59s, ripe degree is (10%NH4Cl)8.9ml。
The preparation of cationic starch solution：
In reaction kettle, the cation that mass fraction is respectively 5%, 10%, 15%, 20%, 25% is prepared with distilled water
Starch solution is sufficiently stirred and can be obtained more uniform cationic starch solution.It is filtered through the double-deck fine cloth using sheet frame filter,
Pressure is in 0.2Mpa hereinafter, obtaining uniform cationic starch solution.
The mixing of viscose glue stoste and cationic starch solution：
Quantitatively cationic starch solution is added in above-mentioned for use viscose solution using proportioning pump, and is uniformly mixed.
Cationic starch solution uses syringe pump in the speed injection to dynamic mixer of 6 liters/min, while being added into mixer
The glutaraldehyde for accounting for first fibre quality 5%, makes it be uniformly mixed with spinning solution, and the flow of viscose solution is 50 liters/min, under room temperature
Stand 1h.Wherein, the quality of cationic starch is the 20% of first fibre weight.
Wet spinning：
It is sent into wet spinning process after cationic starch solution is fully reacted with the mixed solution of viscose glue and carries out spinning.Spray
Silk 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
℃.Coagulation bath composition is：Sulfuric acid 115g/L, sodium sulphate 325g/L, zinc sulfate 11.5g/L.
The leading indicator of fiber by above-mentioned steps preparation is as follows.
| Cationic starch concentration | 5% | 10% | 15% | 20% | 25% |
| Fiber number dtex | 1.69 | 1.68 | 1.68 | 1.68 | 1.69 |
| Do strong cN/dtex | 1.90 | 2.01 | 2.24 | 2.11 | 1.88 |
| Wet strong cN/dtex | 1.32 | 1.45 | 1.60 | 1.35 | 1.32 |
| It is dry to stretch % | 14.7 | 15.8 | 18.1 | 16.2 | 16.1 |
| Dye uptake % | 85.6 | 86.4 | 91.5 | 90.5 | 83.5 |
It can be seen from the table, the regulation and control of cationic starch concentration can be significantly increased into rate of dyeing in preferred scope, and
Modified fibre has preferably elasticity and strength character.
Embodiment 4
The preparation of rayon spinning liquid：
Raw material is the bamboo pulp that the degree of polymerization is 500~600, and first fibre content is more than 90%, and according to following process route
Glue：
It is 5.9 that according to above-mentioned technique, to be fabricated rayon spinning liquid first fibre content, which be 9.1%, NaOH mass fractions, viscosity
For (falling ball method) 59s, ripe degree is (10%NH4Cl)8.9ml。
The preparation of cationic starch solution：
First, cationic starch is modified：Cationic starch is dissolved in deionized water, mass concentration control exists
10wt%, after 80 DEG C or so are gelatinized 30min, initiator is first added under nitrogen protection makes it be adsorbed in advance with starch, adds
Acrylamide monomer (quality is the 20% of cationic starch), carries out graft copolymerization 3 hours at 50 DEG C, adds 95%
Ethyl alcohol modified cationic starch is precipitated, at 50 DEG C be dried in vacuo 48h to get modified cationic starch.Again anti-
It answers in kettle, prepares the modified cationic starch solution that mass fraction is 15% with distilled water, be sufficiently stirred and can be obtained more
Even modified cationic starch solution.It is filtered through the double-deck fine cloth using sheet frame filter, pressure is in 0.2Mpa hereinafter, obtaining uniform
Modified cationic starch solution.
The mixing of viscose glue stoste and cationic starch solution：
Quantitatively cationic starch solution is added in above-mentioned for use viscose solution using proportioning pump, and is uniformly mixed.
Cationic starch solution uses syringe pump in the speed injection to dynamic mixer of 6 liters/min, while being added into mixer
The glutaraldehyde for accounting for first fibre quality 5%, makes it be uniformly mixed with spinning solution, and the flow of viscose solution is 50 liters/min, under room temperature
Stand 1h.Wherein, the quality of cationic starch is the 20% of first fibre weight.
Wet spinning：
It is sent into wet spinning process after cationic starch solution is fully reacted with the mixed solution of viscose glue and carries out spinning.Spray
Silk 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
℃.Coagulation bath composition is：Sulfuric acid 115g/L, sodium sulphate 325g/L, zinc sulfate 11.5g/L.Testing result：Fiber number 1.68dtex；
Do strong 2.38cN/dtex；Wet strong 1.79cN/dtex；It is dry to stretch 19.7%；Dye uptake 93.6%.It can from embodiment 4
Go out, after being modified to cationic starch, fibrous elasticity and intensity and rate of dyeing can be further improved.
Claims (4)
1. it is a kind of can salt-free dyeing regenerated celulose fibre preparation method, which is characterized in that include the following steps：By raw material
Cotton Pulp successively after spinning solution is made in dipping, squeezing, crushing, experienced, yellow, continuous-dissolution, filtering, deaeration, then by sun from
Sub- starch is mixed by way of being injected between mixing or spinning before spinning with spinning solution, and crosslinking agent is added makes cationic starch and spinning
Reaction is crosslinked between cellulose in liquid, and the regenerated celulose fibre that cationic starch is modified is made after spinning；
The additive amount of the cationic starch is 5~30wt% of first fibre content in spinning solution；
The crosslinking agent is the mixing of one or both of glutaraldehyde or glyoxal, and dosage of crosslinking agent is that first fibre contains in spinning solution
3~5wt% of amount；
The cationic starch is to be added in form of an aqueous solutions.
2. it is according to claim 1 can salt-free dyeing regenerated celulose fibre preparation method, it is characterised in that：Sun from
The content of sub- starch in the solution is 10~20wt%.
3. it is according to claim 1 can salt-free dyeing regenerated celulose fibre preparation method, it is characterised in that：It is described
Cationic starch degree of substitution be 0.03~0.05, viscosity be 500~1500mPa s.
4. it is according to claim 1 can salt-free dyeing regenerated celulose fibre preparation method, it is characterised in that：It is described
The dry of the regenerated celulose fibre that cationic starch is modified is 2.1~2.4cN/ dtex by force；Wet strong 1.3~1.7cN/ dtex；
It is dry to stretch 16.0~20.0%.
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| CN111394818B (en) * | 2020-04-07 | 2022-09-30 | 江苏金太阳纺织科技股份有限公司 | Liquorice regenerated cellulose fiber and preparation method thereof |
| CN114134586B (en) * | 2021-11-22 | 2023-10-10 | 唐山三友集团兴达化纤有限公司 | Acid dye-dyeable viscose fiber and preparation method thereof |
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