CN106544745A - A kind of production method of cellulose carbamate fibre long filament - Google Patents
A kind of production method of cellulose carbamate fibre long filament Download PDFInfo
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Abstract
The present invention relates to a kind of production method of cellulose carbamate fibre long filament, belongs to cellulose carbamate fibre production technical field.The present invention is by the activation of specific cellulose, the preparation of cellulose carbamate, the preparation of cellulose carbamate solution and spinning process, form a higher intact fibre element carbamate fibre long filament production process of completeness, the spinning solution good spinnability of preparation, final products performance is good, industrialization large-scale production is especially suitable for, production cost, production efficiency and product quality is taken into account.
Description
Technical field
The present invention relates to a kind of production method of regenerated celulose fibre, it is more particularly related to a kind of production method of cellulose carbamate fibre long filament, belongs to cellulose carbamate fibre production technical field.
Background technology
Cellulose fibre is the chemical fibre made by as raw material of constantly regenerating natural fiber with nature.The production of cellulose fibre now is mainly viscose process, and the product produced is viscose rayon.
The one kind of viscose rayon for regenerated celulose fibre, is to put into one of chemical fibre of industrialized production earliest.The good hygroscopicity of viscose rayon, comfortable and easy to wear, spinnability is excellent, Chang Yumian, hair or various synthetic fibers blending, intertexture, for all kinds of clothing and decorative textile product.The high tenacity staple fibre prepared using different raw materials and spinning technique, can be used for the industrial goods such as tire cord, conveyer belt.China is the first big producing country of viscose rayon at present, but state's cellulose fibres overwhelming majority is also according to traditional old technique productions at present, viscose glue is made including operations such as dipping, squeezing, crushing, aging, yellow, dissolving, maturation, filtration, deaerations, then viscose rayon is made by wet spinning.
In viscose rayon traditional handicraft, the yellowing processes of cellulose will expend substantial amounts of Carbon bisulfide, and also give off the hydrogen sulfide of suitable share and irretrievable Carbon bisulfide in spinning phase, can cause sizable pollution to environment.In addition, traditional viscose process high cost, time-consuming for production technology, causes to spend big, and production efficiency is not but high.
Therefore, in recent years the research of viscose rayon technique is increasingly turned to it is environmentally friendly and can improve production efficiency, reduce coming on the novel process of production cost, and generate some new forming techniques.As cellulose elementary cell has three hydroxyls, it is readily formed intramolecular and intermolecular hydrogen bonding, degree of crystallinity is very high, so cellulose is difficult to be dissolved in general inorganic and organic solvent, needs using special solvent or by its derivatization modified to be just easy to processing and utilize.Cellulose derivatization mainly includes esterification, etherificate and graft copolymerization etc..Wherein, cellulose generates cellulose carbamate with urea reaction, process is relatively simple, good spinning property, environmental pollution are little, the fabric function admirable of gained, and carbamide abundance and nontoxic, price is also relatively cheap, and product cellulose carbamate is stable in properties, can be stored for a long time under ambient temperature and moisture environment.
State Intellectual Property Office discloses Publication No. CN104072622A in 2014.10.1, the invention of entitled " preparation of cellulose carbamate and its dissolution in low temperature spinning process ", a kind of preparation of cellulose carbamate of the disclosure of the invention and its dissolution in low temperature spinning process, cellulose is added to into sodium hydroxide solution, stir and soak, then cellulose is taken out and is washed to neutrality, obtain alkalinized celluloses, add carbamide, stir, heat in being put into baking oven, react and be dried, obtain cellulose carbamate, cellulose carbamate is ground into powder to be added in mixing kettle, and add sodium hydroxide, thiourea, the double solventss of deionized water, it is uniformly mixed；Raw material in mixing kettle is sprayed by the spinneret orifice of spinneret after extrusion, deaeration, filtration, solid is frozen in sequentially entering the first coagulating tank and the second gelation groove, then after tank washing is stretched, be wound in cellulose carbamate fibre by filament spinning component.
Above invention discloses cellulose and prepare cellulose carbamate as raw material with carbamide, then prepare cellulose carbamate solution, all processes of last spinning again.But, the process is simultaneously suitably applied industrialization large-scale production, and the spinning solution spinnability of preparation is poor, and spinning technique through corresponding optimization, does not also cause final products performance not good.
State Intellectual Property Office discloses Publication No. CN101597336 in 2009.12.9, the invention of entitled " microwave synthesis method of cellulose carbamate ", a kind of technology of microwave heating synthesis method of fiber carbamate of the disclosure of the invention.Its method is cellulose to be immersed in aqueous solution of urea to make which fully adsorb carbamide first, and filters, is dried to obtain the homogeneous mixture of cellulose/carbamide.Then cellulose/urea admixture is placed in into reacting by heating in microwave oven and cellulose carbamate is obtained.The solvent-free pollution of cellulose carbamate synthetic technology provided by the present invention, it is not necessary to add organic solvent and any catalyst, response speed is fast, and energy consumption is low.Synthesized cellulose carbamate product has good dissolubility in the range of -10～5 DEG C in 6～10wt%NaOH aqueous solutions, can prepare concentrated solution that is stable, transparent and being suitable for industrial spinning and masking.
State Intellectual Property Office discloses Publication No. CN102691125A in 2012.9.26, the invention of entitled " a kind of method that regenerated celulose fibre is prepared by cellulose carbamate ", the invention is related to a kind of method for preparing regenerated celulose fibre by cellulose carbamate, the method is that solvent compositions are the sodium hydroxide containing 6～10wt%, the aqueous solution of 0.1～3wt% Zinc Oxide dissolving cellulose carbamate with a kind of solvent compositions.A certain amount of cellulose carbamate is dispersed in the solvent compositions, less than -10 DEG C are refrigerated under cryogenic conditions, take out and thaw under conditions of not higher than 50 DEG C, carry out wet spinning, strand obtains regenerated celulose fibre through solidification, washing, after being dried.Cellulose carbamate dissolving difficulty and unstable this two hang-up of solution in conventional technique is this method solved, is worth with very high industrial applications.
State Intellectual Property Office discloses Publication No. CN103980368A in 2014.8.13, the invention of entitled " a kind of method that liquid and solid phase reaction prepares cellulose carbamate ", the invention utilize cellulose pulp or through the cellulose pulp and carbamide of activation processing be raw material, the high boiling point such as dimethylformamide (DMF) or dimethyl acetylamide (DMAc), dimethyl sulfoxide (DMSO), N-Methyl pyrrolidone (NMP) is non-proton and intensive polar solvent in carry out esterification synthesis method of fiber carbamate.During liquid and solid phase reaction method prepares cellulose carbamate, from solvent toxicity is little, easy recovery, make preparation process easy, environmental protection, safely and controllably, prepared cellulose carbamate forms good stable solution in being dissolved in NaOH solution, can be used for the preparation of regenerated celulose fibre or film etc..
Above-mentioned three patents are directed to some of whole cellulose carbamate fibre production link and step, but are all not involved with whole technical process, it is impossible to realize industrialization large-scale production.
The content of the invention
Present invention seek to address that the technique of existing production cellulose carbamate fibre cannot adapt to the problem of industrialization large-scale production, a kind of production method of cellulose carbamate fibre long filament is provided, the method is adapted to industrialization large-scale production, the spinning solution good spinnability of preparation, final products performance are good.
In order to realize foregoing invention purpose, its specific technical scheme is as follows：
A kind of production method of cellulose carbamate fibre long filament, it is characterised in that：Comprise the following steps that：
The activation of A, cellulose
First cellulose is dried, then dried cellulose is added to into immersion in liquefied ammonia so as to after activation, obtain activated cellulose；
The preparation of B, cellulose carbamate
The mixture of carbamide and thiourea is added in activated cellulose, the mixture of activated cellulose, carbamide and thiourea is obtained after immersion, then which is heated, carried out esterification, obtain cellulose carbamate；
The preparation of C, cellulose carbamate solution
Cellulose carbamate is added in solution of the sodium hydroxide with aluminium oxide, at -10～0 DEG C, 2～4h of freezing reaction, after the completion of reaction, rises to room temperature and obtain cellulose carbamate solution, i.e. spinning solution；
D, spinning
Spinning solution in step C is made into cellulose carbamate fibre long filament by wet spinning.
In step, described cellulose is the wood pulp of the degree of polymerization 400～600 to the present invention.
In step, the temperature of described drying is 50～70 DEG C to the present invention, and drying time is 1～3h, and moisture content≤10% of cellulose is caused after being dried.
In step, the temperature of described immersion is -70～-50 DEG C to the present invention, and soak time is 30～60min.
In stepb, described carbamide is the urea liquid of 20～40% concentration to the present invention, and the carbamide is (2～4) with the mass ratio of activated cellulose:1.
In stepb, described thiourea is the thiourea solution of 5～10% concentration to the present invention, and the thiourea is (0.5～1) with the mass ratio of activated cellulose:1.
In stepb, the temperature of described heating is 140～160 DEG C to the present invention, and the reacting by heating time is 2～4h.
In step C, in the solution of described sodium hydroxide and aluminium oxide, the mass concentration of sodium hydroxide is 8～12% to the present invention, and the mass concentration of aluminium oxide is 1～2%, and dissolving obtains the cellulose carbamate solution that mass concentration is 6～10%.
In step D, in described spinning process, the composition and proportioning of coagulating bath are H to the present invention2SO4 120～140g/L, ZnSO4 9～12g/L, Na2SO4 220～240g/L, Al2(SO4)3 6～8g/L.
The Advantageous Effects that the present invention brings：
1st, the present invention solves the problems, such as that the method for existing production cellulose carbamate fibre cannot adapt to industrialization large-scale production.The present invention provides a kind of production method of cellulose carbamate fibre long filament, by specific processing step and technological parameter, form a higher intact fibre element carbamate fibre long filament production process of completeness, the spinning solution good spinnability of preparation, final products performance is good, industrialization large-scale production is especially suitable for, production cost, production efficiency and product quality is taken into account.
2nd, it is currently preferred, the wood pulp of cellulose in step for the degree of polymerization 400～600.Raw material of wood pulp source is wide, and the degree of polymerization is relatively low, and above-mentioned raw materials select the dissolving selected beneficial to cellulose carbamate with polymerization scope, enables to the spinnability of stock solution preferably, and the intensity of product is preferable.
3rd, currently preferred, the temperature of drying in step is 50～70 DEG C, and drying time is 1～3h, and moisture content≤10% of cellulose is caused after being dried.Being selected to of the selection of above-mentioned Drying Technology Parameter and last cellulose moisture content causes the activation of follow-up liquefied ammonia more preferable.
4th, currently preferred, the temperature of immersion in step is -70～-50 DEG C, and soak time is 30～60min.The degree of crystallinity of cellulose can be preferably reduced using liquefied ammonia immersion treatment according to above-mentioned technological parameter, it is intermolecular beneficial to carbamide and thiourea reagent infiltrated fiber element, improve the activity of cellulose.
5th, currently preferred, carbamide in stepb is the urea liquid of 20～40% concentration, and the carbamide is (2～4) with the mass ratio of activated cellulose:1.Above-mentioned urea concentration scope and both proportion immersion celluloses can make cellulose carbamate have suitable nitrogen content 2～4%.
6th, currently preferred, the temperature of heating in stepb is 140～160 DEG C, and the reacting by heating time is 2～4h.Being selected to of above-mentioned special process parameter ensures that cellulose carbamate has suitable nitrogen content, also so that cellulose oxidation degraded is not obvious.
7th, currently preferred, in sodium hydroxide in step C and the solution of aluminium oxide, the mass concentration of sodium hydroxide is 8～12%, and the mass concentration of aluminium oxide is 1～2%, and dissolving obtains the cellulose carbamate solution that mass concentration is 6～10%.The present invention adds aluminium oxide so that the dissolubility of cellulose carbamate and stability are improved.The dissolubility for being selected to guarantee cellulose carbamate of above-mentioned special process parameter is higher, and the viscosity of solution is adapted to spinning, and the stability of solution is preferable.
8th, currently preferred, in spinning process in step D, the composition and proportioning of coagulating bath are H2SO4
120～140g/L, ZnSO4 9～12g/L, Na2SO4 220～240g/L, Al2(SO4)3 6～8g/L.The selection of above-mentioned specific process parameters range is for cellulose carbamate solution（Spinning solution）Be optimized, cellulose carbamate can rapid shaping, the performance of final continuous yarn product is more preferable.Wherein add aluminum sulfate improve the intensity and degree of stretching of cellulose carbamate long filament.
Specific embodiment
Embodiment 1
A kind of production method of cellulose carbamate fibre long filament, comprises the following steps that：
The activation of A, cellulose
First cellulose is dried, then dried cellulose is added to into immersion in liquefied ammonia so as to after activation, obtain activated cellulose；
The preparation of B, cellulose carbamate
The mixture of carbamide and thiourea is added in activated cellulose, the mixture of activated cellulose, carbamide and thiourea is obtained after immersion, then which is heated, carried out esterification, obtain cellulose carbamate；
The preparation of C, cellulose carbamate solution
Cellulose carbamate is added in solution of the sodium hydroxide with aluminium oxide, at -10 DEG C, freezing reaction 2h, after the completion of reaction, rises to room temperature and obtain cellulose carbamate solution, i.e. spinning solution；
D, spinning
Spinning solution in step C is made into cellulose carbamate fibre long filament by wet spinning.
The cellulose carbamate fibre long filament similar nature that the above-mentioned techniques of Jing are prepared can meet the use requirement of viscose fiber filament in viscose fiber filament, and without residual sulfur, dye uniformity is better than viscose fiber filament.Additionally, the production process of cellulose carbamate fibre long filament does not use CS2, do not produce SO2、H2The toxic and harmfuls such as S, than viscose rayon environmental protection.
The index parameter of cellulose carbamate fibre long filament that this technique is prepared is shown in Table 1 with the index parameter of viscose fiber filament.
Table 1
| Project | Cellulose carbamate fibre | Viscose rayon |
| Dry fracture strength >= | 1.65 | 1.70 |
| Dry elongation at break >= | 19% | 18% |
| The dry extension at break coefficient of variation≤ | 8.0% | 10% |
| Line density deviation | ±2.0 | ±2.5 |
| The line density coefficient of variation≤ | 3.0% | 3.0% |
| Monofilament radical deviation≤ | 3.0 | 3.0% |
| Residual sulfur content (mg/100g)≤ | 0 | 10 |
| Dye uniformity (gray card level) >= | 4 | 3 |
Embodiment 2
A kind of production method of cellulose carbamate fibre long filament, comprises the following steps that：
The activation of A, cellulose
First cellulose is dried, then dried cellulose is added to into immersion in liquefied ammonia so as to after activation, obtain activated cellulose；
The preparation of B, cellulose carbamate
The mixture of carbamide and thiourea is added in activated cellulose, the mixture of activated cellulose, carbamide and thiourea is obtained after immersion, then which is heated, carried out esterification, obtain cellulose carbamate；
The preparation of C, cellulose carbamate solution
Cellulose carbamate is added in solution of the sodium hydroxide with aluminium oxide, at 0 DEG C, freezing reaction 4h, after the completion of reaction, rises to room temperature and obtain cellulose carbamate solution, i.e. spinning solution；
D, spinning
Spinning solution in step C is made into cellulose carbamate fibre long filament by wet spinning.
Embodiment 3
A kind of production method of cellulose carbamate fibre long filament, comprises the following steps that：
The activation of A, cellulose
First cellulose is dried, then dried cellulose is added to into immersion in liquefied ammonia so as to after activation, obtain activated cellulose；
The preparation of B, cellulose carbamate
The mixture of carbamide and thiourea is added in activated cellulose, the mixture of activated cellulose, carbamide and thiourea is obtained after immersion, then which is heated, carried out esterification, obtain cellulose carbamate；
The preparation of C, cellulose carbamate solution
Cellulose carbamate is added in solution of the sodium hydroxide with aluminium oxide, at -5 DEG C, freezing reaction 3h, after the completion of reaction, rises to room temperature and obtain cellulose carbamate solution, i.e. spinning solution；
D, spinning
Spinning solution in step C is made into cellulose carbamate fibre long filament by wet spinning.
Embodiment 4
A kind of production method of cellulose carbamate fibre long filament, comprises the following steps that：
The activation of A, cellulose
First cellulose is dried, then dried cellulose is added to into immersion in liquefied ammonia so as to after activation, obtain activated cellulose；
The preparation of B, cellulose carbamate
The mixture of carbamide and thiourea is added in activated cellulose, the mixture of activated cellulose, carbamide and thiourea is obtained after immersion, then which is heated, carried out esterification, obtain cellulose carbamate；
The preparation of C, cellulose carbamate solution
Cellulose carbamate is added in solution of the sodium hydroxide with aluminium oxide, at -2 DEG C, freezing reaction 3.5h, after the completion of reaction, rises to room temperature and obtain cellulose carbamate solution, i.e. spinning solution；
D, spinning
Spinning solution in step C is made into cellulose carbamate fibre long filament by wet spinning.
Embodiment 5
On the basis of embodiment 1-4：
Preferably, in step, wood pulp of the described cellulose for the degree of polymerization 400.
Preferably, in step, the temperature of described drying is 50 DEG C, and drying time is 1h, and the moisture content that cellulose is caused after being dried is 2%.
Preferably, in step, the temperature of described immersion is -70 DEG C, and soak time is 30min.
Embodiment 6
On the basis of embodiment 1-4：
Preferably, in step, wood pulp of the described cellulose for the degree of polymerization 600.
Preferably, in step, the temperature of described drying is 70 DEG C, and drying time is 3h, and the moisture content that cellulose is caused after being dried is 10%.
Preferably, in step, the temperature of described immersion is -50 DEG C, and soak time is 60min.
Embodiment 7
On the basis of embodiment 1-4：
Preferably, in step, wood pulp of the described cellulose for the degree of polymerization 500.
Preferably, in step, the temperature of described drying is 60 DEG C, and drying time is 2h, and the moisture content 6% of cellulose is caused after being dried.
Preferably, in step, the temperature of described immersion is -60 DEG C, and soak time is 45min.
Embodiment 8
On the basis of embodiment 1-4：
Preferably, in step, wood pulp of the described cellulose for the degree of polymerization 550.
Preferably, in step, the temperature of described drying is 65 DEG C, and drying time is 1.5h, and the moisture content that cellulose is caused after being dried is 8%.
Preferably, in step, the temperature of described immersion is -65 DEG C, and soak time is 35min.
Embodiment 9
On the basis of embodiment 1-4：
Preferably, in stepb, described thiourea is the thiourea solution of 5% concentration, and the thiourea is 0.5 with the mass ratio of activated cellulose:1.
Preferably, in stepb, the temperature of described heating is 140 DEG C, and the reacting by heating time is 2h.
Embodiment 10
On the basis of embodiment 1-4：
Preferably, in stepb, described thiourea is the thiourea solution of 10% concentration, and the thiourea is 1 with the mass ratio of activated cellulose:1.
Preferably, in stepb, the temperature of described heating is 160 DEG C, and the reacting by heating time is 4h.
Embodiment 11
On the basis of embodiment 1-4：
Preferably, in stepb, described thiourea is the thiourea solution of 7.5% concentration, and the thiourea is 0.75 with the mass ratio of activated cellulose:1.
Preferably, in stepb, the temperature of described heating is 150 DEG C, and the reacting by heating time is 3h.
Embodiment 12
On the basis of embodiment 1-4：
Preferably, in stepb, described thiourea is the thiourea solution of 8% concentration, and the thiourea is 0.7 with the mass ratio of activated cellulose:1.
Preferably, in stepb, the temperature of described heating is 159 DEG C, and the reacting by heating time is 2.5h.
Embodiment 13
On the basis of embodiment 1-4：
Preferably, in step C, in the solution of described sodium hydroxide and aluminium oxide, the mass concentration of sodium hydroxide is 8%, and the mass concentration of aluminium oxide is 1%, and dissolving obtains the cellulose carbamate solution that mass concentration is 6%.
Preferably, in step D, in described spinning process, the composition and proportioning of coagulating bath are H2SO4 120g/L, ZnSO4 9g/L, Na2SO4
220g/L, Al2(SO4)3 6g/L。
Embodiment 14
On the basis of embodiment 1-4：
Preferably, in step C, in the solution of described sodium hydroxide and aluminium oxide, the mass concentration of sodium hydroxide is 12%, and the mass concentration of aluminium oxide is 2%, and dissolving obtains the cellulose carbamate solution that mass concentration is 10%.
Preferably, in step D, in described spinning process, the composition and proportioning of coagulating bath are H2SO4 140g/L, ZnSO4 12g/L, Na2SO4
240g/L, Al2(SO4)3 8g/L。
Embodiment 15
On the basis of embodiment 1-4：
Preferably, in step C, in the solution of described sodium hydroxide and aluminium oxide, the mass concentration of sodium hydroxide is 10%, and the mass concentration of aluminium oxide is 1.5%, and dissolving obtains the cellulose carbamate solution that mass concentration is 8%.
Preferably, in step D, in described spinning process, the composition and proportioning of coagulating bath are H2SO4 130g/L, ZnSO4 10.5g/L, Na2SO4
230g/L, Al2(SO4)3 7g/L。
Embodiment 16
On the basis of embodiment 1-4：
Preferably, in step C, in the solution of described sodium hydroxide and aluminium oxide, the mass concentration of sodium hydroxide is 11%, and the mass concentration of aluminium oxide is 1.3%, and dissolving obtains the cellulose carbamate solution that mass concentration is 7%.
Preferably, in step D, in described spinning process, the composition and proportioning of coagulating bath are H2SO4 125g/L, ZnSO4 10g/L, Na2SO4
222g/L, Al2(SO4)3 6.5g/L。
Claims (9)
1. a kind of production method of cellulose carbamate fibre long filament, it is characterised in that：Comprise the following steps that：
The activation of A, cellulose
First cellulose is dried, then dried cellulose is added to into immersion in liquefied ammonia so as to after activation, obtain activated cellulose；
The preparation of B, cellulose carbamate
The mixture of carbamide and thiourea is added in activated cellulose, the mixture of activated cellulose, carbamide and thiourea is obtained after immersion, then which is heated, carried out esterification, obtain cellulose carbamate；
The preparation of C, cellulose carbamate solution
Cellulose carbamate is added in solution of the sodium hydroxide with aluminium oxide, at -10～0 DEG C, 2～4h of freezing reaction, after the completion of reaction, rises to room temperature and obtain cellulose carbamate solution, i.e. spinning solution；
D, spinning
Spinning solution in step C is made into cellulose carbamate fibre long filament by wet spinning.
2. the production method of a kind of cellulose carbamate fibre long filament according to claim 1, it is characterised in that：In step, wood pulp of the described cellulose for the degree of polymerization 400～600.
3. the production method of a kind of cellulose carbamate fibre long filament according to claim 1, it is characterised in that：In step, the temperature of described drying is 50～70 DEG C, and drying time is 1～3h, and moisture content≤10% of cellulose is caused after being dried.
4. the production method of a kind of cellulose carbamate fibre long filament according to claim 1, it is characterised in that：In step, the temperature of described immersion is -70～-50 DEG C, and soak time is 30～60min.
5. the production method of a kind of cellulose carbamate fibre long filament according to claim 1, it is characterised in that：In stepb, described carbamide is the urea liquid of 20～40% concentration, and the carbamide is (2～4) with the mass ratio of activated cellulose:1.
6. a kind of production method of cellulose carbamate fibre long filament according to claim 1 or 5, it is characterised in that：In stepb, described thiourea is the thiourea solution of 5～10% concentration, and the thiourea is (0.5～1) with the mass ratio of activated cellulose:1.
7. the production method of a kind of cellulose carbamate fibre long filament according to claim 1, it is characterised in that：In stepb, the temperature of described heating is 140～160 DEG C, and the reacting by heating time is 2～4h.
8. the production method of a kind of cellulose carbamate fibre long filament according to claim 1, it is characterised in that：In step C, in the solution of described sodium hydroxide and aluminium oxide, the mass concentration of sodium hydroxide is 8～12%, and the mass concentration of aluminium oxide is 1～2%, and dissolving obtains the cellulose carbamate solution that mass concentration is 6～10%.
9. the production method of a kind of cellulose carbamate fibre long filament according to claim 1, it is characterised in that：In step D, in described spinning process, the composition and proportioning of coagulating bath are H2SO4 120～140g/L, ZnSO4 9～12g/L, Na2SO4 220～240g/L, Al2(SO4)3 6～8g/L.
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| CN107044065A (en) * | 2017-04-12 | 2017-08-15 | 周燕 | A kind of paper-making pulping process |
| CN107501415A (en) * | 2017-08-25 | 2017-12-22 | 孙飞勇 | The preparation method of cellulose carbamate |
| CN116162176A (en) * | 2023-02-28 | 2023-05-26 | 赣南师范大学 | Preparation method of cellulose carbamate |
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