CN106702515A - Production technology of cellulose carbamate fiber filaments - Google Patents
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Abstract
The invention relates to a production technology of cellulose carbamate fiber filaments, and belongs to the technical field of production of cellulose carbamate fibers. A complete cellulose carbamate fiber filament production process with high completeness is formed through specific cellulose activation, cellulose carbamate preparation, cellulose carbamate solution preparation and spinning steps, a prepared spinning stock solution has good spinnability, and the final product has good performances, so the technology is very suitable for industrial large-scale production, and considers the production cost, the production efficiency and the product quality.
Description
Technical field
The present invention relates to a kind of production technology of regenerated celulose fibre, it is more particularly related to a kind of production technology of cellulose carbamate fibre long filament, belongs to cellulose carbamate fibre production technical field.
Background technology
Cellulose fibre is the chemical fibre that constantly regenerating natural fiber with nature is made as raw material.The production of cellulose fibre now is mainly viscose process, and the product produced is viscose rayon.
Viscose rayon is one kind of 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 clothes and decorative textile product.The high tenacity staple fibre prepared using different raw material and spinning technique, can be used for the industrial goods such as tire cord, conveyer belt.Current China is the big producer of viscose rayon first, but the current state cellulose fibres overwhelming majority is also according to traditional old technique productions, operation is made viscose glue including dipping, squeezing, crushing, aging, yellow, dissolving, maturation, filtering, deaeration etc., then is made viscose rayon by wet spinning.
In viscose rayon traditional handicraft, the yellowing processes of cellulose will expend substantial amounts of carbon disulfide, and also give off the hydrogen sulfide and irretrievable carbon disulfide of suitable share in spinning phase, and sizable pollution can be caused 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, the research of viscose rayon technique is increasingly turned in recent years it is environmentally friendly and can improve production efficiency, reducing come on the novel process of production cost, and generates some new forming techniques.Because cellulose elementary cell has three hydroxyls, it is readily formed intramolecular and intermolecular hydrogen bonding, crystallinity is very high, so cellulose is difficult to be dissolved in general inorganic and organic solvent, it is necessary to just be easy to processing and utilize using special solvent or by its derivatization is modified.Cellulose derivatization is mainly including esterification, etherificate and graft copolymerization etc..Wherein, cellulose generates cellulose carbamate with urea reaction, process is relatively simple, good spinning property, environmental pollution is small, the fabric function admirable of gained, and urea abundance and nontoxic, price is also relatively cheap, and product cellulose carbamate is stable in properties, can be stored under ambient temperature and moisture environment for a long time.
State Intellectual Property Office discloses a 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 sodium hydroxide solution, stir and soak, then cellulose is taken out and is washed to neutrality, obtain alkalinized celluloses, add urea, stir, it is put into heating in baking oven, react and dry, obtain cellulose carbamate, cellulose carbamate is ground into powder to be added in mixing kettle, and add NaOH, thiocarbamide, the double solvents of deionized water, it is uniformly mixed；Raw material in mixing kettle is sprayed after extrusion, deaeration, filtering by the spinneret orifice of spinneret, sequentially enter and be frozen into the first coagulating tank and the second gelation groove solid, then by after tank washing by filament spinning component stretching, be wound in cellulose carbamate fibre.
Cellulose carbamate is prepared as raw material above invention discloses cellulose and urea, cellulose carbamate solution, all processes of last spinning are then prepared again.But, the process is simultaneously suitably applied industrialization large-scale production, and the spinning solution spinnability of preparation is poor, and spinning technique by corresponding optimization, does not also cause final products performance not good.
State Intellectual Property Office discloses a 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 it fully adsorb urea first, and filters, is dried to obtain the homogeneous mixture of cellulose/urea.Then cellulose/urea admixture is placed in heating response in micro-wave 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, reaction 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 solution, can prepare stabilization, concentrated solution that is transparent and being suitable for industrial spinning and masking.
State Intellectual Property Office discloses a 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 that regenerated celulose fibre is prepared by cellulose carbamate, the method is that cellulose carbamate is dissolved with a kind of solvent compositions, and solvent compositions are the NaOH containing 6~10wt%, the aqueous solution of 0.1~3wt% zinc oxide.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 thawed under conditions of not higher than 50 DEG C, carry out wet spinning, strand obtains regenerated celulose fibre after supersolidification, washing, drying.Cellulose carbamate dissolving difficulty and unstable this two hang-up of solution in conventional technique are this method solve, is worth with industrial applications very high.
State Intellectual Property Office discloses a 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 is raw material using cellulose pulp or by the cellulose pulp and urea of activation process, the higher boiling such as dimethylformamide (DMF) or dimethylacetylamide (DMAc), dimethyl sulfoxide (DMSO) (DMSO), 1-METHYLPYRROLIDONE (NMP) is non-proton and intensive polar solvent in carry out esterification synthesis method of fiber carbamate.Liquid and solid phase reaction method is prepared during cellulose carbamate, from solvent toxicity is small, 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 technology of cellulose carbamate fibre long filament is provided, the technique is adapted to industrialization large-scale production, the spinning solution good spinnability of preparation, final products performance is good.
In order to realize foregoing invention purpose, its specific technical scheme is as follows：
A kind of production technology of cellulose carbamate fibre long filament, it is characterised in that：Comprise the following steps that：
The activation of A, cellulose
First cellulose is added in sodium hydroxide solution and is soaked, carry out basification, after being disposed, filtration washing, then alkalinized celluloses are vacuum dried, obtain activated cellulose；
The preparation of B, cellulose carbamate
Take out to be placed in vacuum drying chamber to the liquid ammonia solution for adding urea in activated cellulose, after immersion and dry, then using heating using microwave, carry out esterification, obtain cellulose carbamate；
The preparation of C, cellulose carbamate solution
Cellulose carbamate is added in sodium hydroxide solution, first time mixed dissolution is carried out；Again to sodium hydroxide solution is added in mixture, second mixed dissolution is carried out；Third time carries out third time mixed dissolution to sodium hydroxide solution is added in mixture, and cellulose carbamate solution, i.e. spinning solution are obtained after rising to normal temperature；
D, spinning
Spinning solution in step C is made cellulose carbamate fibre long filament by wet spinning.
In step, described cellulose is the linter pulp of the degree of polymerization 400~600 to the present invention.
The present invention in step, the mass concentration 15~20% of described sodium hydroxide solution, described NaOH and the volume ratio of cellulose consumption is (4~6):1.
In step, the time of described immersion is 1~2h to the present invention, and temperature is 5~15 DEG C.
In step, the described vacuum drying time is 1~3h to the present invention, and temperature is 40~60 DEG C.
In stepb, described activated cellulose is 1 with urea to the present invention in mass ratio:(2~4), the concentration of the liquid ammonia solution of urea is 20~40%.
In stepb, the heating power of described heating using microwave is 500~800W to the present invention, and the heating response time is 1~3h.
In step C, the preparation of described cellulose carbamate solution is specially the present invention：
Cellulose carbamate is added in the sodium hydroxide solution that concentration is 6~8% at -5~0 DEG C, first time mixed dissolution is carried out；At -10~-5 DEG C to mixture in add concentration be 8~10% sodium hydroxide solution, carry out second mixed dissolution；At -15~-10 DEG C to mixture in add concentration be 10~12% sodium hydroxide solutions, carry out third time mixed dissolution, obtain cellulose carbamate solution, i.e. spinning solution after rising to normal temperature.
In step C, in described first time mixed dissolution, the sodium hydroxide solution of addition is (10~12) with the liquid-solid ratio of cellulose carbamate to the present invention:1, in second described mixed dissolution, the sodium hydroxide solution of addition is (12~14) with the liquid-solid ratio of cellulose carbamate:1, in described third time mixed dissolution, the sodium hydroxide solution of addition is (14~16) with the liquid-solid ratio of cellulose carbamate:1.
In step D, in described spinning process, the composition and proportioning of coagulating bath are Na to the present invention2SO4 230~245g/L, ZnSO48~12g/L, H2SO4
110~140g/L.
The Advantageous Effects that the present invention brings：
1st, the present invention solves the problems, such as that the technique of existing production cellulose carbamate fibre cannot adapt to industrialization large-scale production.The present invention provides a kind of production technology of cellulose carbamate fibre long filament, by specific processing step and technological parameter, form a completeness intact fibre element carbamate fibre long filament production process higher, 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, currently preferred, cellulose in step is the linter pulp of the degree of polymerization 400~600.The methylcellulose content of linter pulp is high, and selects above-mentioned polymerization scope, is more favorable for the dissolving of cellulose, enables to the quality of final products to improve.
3rd, it is currently preferred, the mass concentration 15~20% of sodium hydroxide solution in step, described NaOH and the volume ratio of cellulose consumption is (4~6):1.The selection of above-mentioned special process parameter area causes that cellulose activation degree is high, it is ensured that enough alkali concns.
4th, currently preferred, the time of immersion in step is 1~2h, and temperature is 5~15 DEG C.The selection of above-mentioned special process parameter area makes the hemicellulose preferably dissolution in cellulose pulp, it is ensured that the uniformity of alkali cellulose.
5th, currently preferred, the vacuum drying time in step is 1~3h, and temperature is 40~60 DEG C.The selection of above-mentioned specific process parameters range is so that the moisture content after drying in alkali cellulose is effectively reduced the oxidative degradation of alkali cellulose less than 10%.
6th, currently preferred, activated cellulose in stepb is 1 with urea in mass ratio:(2~4), the concentration of the liquid ammonia solution of urea is 20~40%.The selection of above-mentioned specific process parameters range cause cellulose carbamate in nitrogen content 3% or so, the dissolubility of cellulose carbamate is good, and the spinnability of stoste is also more preferable.
7th, currently preferred, the heating power of heating using microwave in stepb is 500~800W, and the heating response time is 1~3h.Reactant is heated rapidly to 140~160 DEG C of range of reaction temperature by being selected to of above-mentioned specific process parameters range, and carries out esterification, the nitrogen content of product cellulose carbamate is controlled 2~4%.
8th, currently preferred, in step C, the preparation of described cellulose carbamate solution is specially：Cellulose carbamate is added in the sodium hydroxide solution that concentration is 6-8% at -5~0 DEG C, first time mixed dissolution is carried out；At -10~-5 DEG C to mixture in add concentration be 8~10% sodium hydroxide solution, carry out second mixed dissolution；At -15~-10 DEG C to mixture in add concentration be 10~12% sodium hydroxide solutions, carry out third time mixed dissolution, obtain cellulose carbamate solution, i.e. spinning solution after rising to normal temperature.With the dissolving of cellulose carbamate, naoh concentration is gradually reduced in mixed liquor, and NaOH is added by being segmented, and makes the concentration of NaOH evenly, and course of dissolution viscosity gradually increases, the dissolving that temperature is more favorable for cellulose carbamate is gradually reduced.
9th, currently preferred, in the first time mixed dissolution in step C, the sodium hydroxide solution of addition is (10~12) with the liquid-solid ratio of cellulose carbamate:1；In second described mixed dissolution, the sodium hydroxide solution of addition is (12~14) with the liquid-solid ratio of cellulose carbamate:1；In described third time mixed dissolution, the sodium hydroxide solution of addition is (14~16) with the liquid-solid ratio of cellulose carbamate:1；With the dissolving of raw material, the viscosity of mixed liquor is gradually risen, and the amount of NaOH is increased with above-mentioned special parameter, and beneficial to the dissolving of cellulose carbamate, segmentation adds the dissolution velocity that can accelerate cellulose carbamate.
10th, in step D, in described spinning process, the composition and proportioning of coagulating bath are Na to the present invention2SO4 230~245g/L, ZnSO48~12g/L, H2SO4
110~140g/L.The selection of above-mentioned specific process parameters range is directed to cellulose carbamate solution（Spinning solution）Optimize, cellulose carbamate can rapid shaping, the performance of final continuous yarn product is more preferable.
Specific embodiment
Embodiment
1
A kind of production technology of cellulose carbamate fibre long filament, comprises the following steps that：
The activation of A, cellulose
First cellulose is added in sodium hydroxide solution and is soaked, carry out basification, after being disposed, filtration washing, then alkalinized celluloses are vacuum dried, obtain activated cellulose；
The preparation of B, cellulose carbamate
Take out to be placed in vacuum drying chamber to the liquid ammonia solution for adding urea in activated cellulose, after immersion and dry, then using heating using microwave, carry out esterification, obtain cellulose carbamate；
The preparation of C, cellulose carbamate solution
Cellulose carbamate is added in sodium hydroxide solution, first time mixed dissolution is carried out；Again to sodium hydroxide solution is added in mixture, second mixed dissolution is carried out；Third time carries out third time mixed dissolution to sodium hydroxide solution is added in mixture, and cellulose carbamate solution, i.e. spinning solution are obtained after rising to normal temperature；
D, spinning
Spinning solution in step C is made cellulose carbamate fibre long filament by wet spinning.
The cellulose carbamate fibre long filament similar nature prepared through above-mentioned technique can meet the use requirement of viscose fiber filament in viscose fiber filament, and without residual sulphur, 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
On the basis of embodiment 1：
Preferably, in step, described cellulose is the linter pulp of the degree of polymerization 400.
Preferably, in step, the mass concentration 15% of described sodium hydroxide solution, described NaOH and the volume ratio of cellulose consumption is 4:1.
Preferably, in step, the time of described immersion is 1h, and temperature is 5 DEG C.
Preferably, in step, the described vacuum drying time is 1h, and temperature is 40 DEG C.
Embodiment
3
On the basis of embodiment 1：
Preferably, in step, described cellulose is the linter pulp of the degree of polymerization 600.
Preferably, in step, the mass concentration 20% of described sodium hydroxide solution, described NaOH and the volume ratio of cellulose consumption is 6:1.
Preferably, in step, the time of described immersion is 2h, and temperature is 15 DEG C.
Preferably, in step, the described vacuum drying time is 3h, and temperature is 60 DEG C.
Embodiment
4
On the basis of embodiment 1：
Preferably, in step, described cellulose is the linter pulp of the degree of polymerization 500.
Preferably, in step, the mass concentration 17.5% of described sodium hydroxide solution, described NaOH and the volume ratio of cellulose consumption is 5:1.
Preferably, in step, the time of described immersion is 1.5h, and temperature is 10 DEG C.
Preferably, in step, the described vacuum drying time is 2h, and temperature is 50 DEG C.
Embodiment
5
On the basis of embodiment 1：
Preferably, in step, described cellulose is the linter pulp of the degree of polymerization 450.
Preferably, in step, the mass concentration 19% of described sodium hydroxide solution, described NaOH and the volume ratio of cellulose consumption is 4.2:1.
Preferably, in step, the time of described immersion is 1.3h, and temperature is 12 DEG C.
Preferably, in step, the described vacuum drying time is 1.6h, and temperature is 56 DEG C.
Embodiment
6
On the basis of embodiment 1：
Preferably, in stepb, described activated cellulose is 1 with urea in mass ratio:2, the concentration of the liquid ammonia solution of urea is 20%.
Preferably, in stepb, the heating power of described heating using microwave is 500W, and the heating response time is 1h.
Embodiment
7
On the basis of embodiment 1：
Preferably, in stepb, described activated cellulose is 1 with urea in mass ratio:4, the concentration of the liquid ammonia solution of urea is 40%.
Preferably, in stepb, the heating power of described heating using microwave is 800W, and the heating response time is 3h.
Embodiment
8
On the basis of embodiment 1：
Preferably, in stepb, described activated cellulose is 1 with urea in mass ratio:3, the concentration of the liquid ammonia solution of urea is 30%.
Preferably, in stepb, the heating power of described heating using microwave is 650W, and the heating response time is 2h.
Embodiment
9
On the basis of embodiment 1：
Preferably, in stepb, described activated cellulose is 1 with urea in mass ratio:3.5, the concentration of the liquid ammonia solution of urea is 21%.
Preferably, in stepb, the heating power of described heating using microwave is 600W, and the heating response time is 2.5h.
Embodiment
9
On the basis of embodiment 1：
Preferably, in step C, the preparation of described cellulose carbamate solution is specially：
Cellulose carbamate is added in the sodium hydroxide solution that concentration is 6% at -5 DEG C, first time mixed dissolution is carried out；At -10 DEG C to mixture in add concentration be 8% sodium hydroxide solution, carry out second mixed dissolution；At -15 DEG C to mixture in add concentration be 10% sodium hydroxide solution, carry out third time mixed dissolution, obtain cellulose carbamate solution, i.e. spinning solution after rising to normal temperature.
Preferably, in step C, in described first time mixed dissolution, the sodium hydroxide solution of addition is 10 with the liquid-solid ratio of cellulose carbamate:1；In second described mixed dissolution, the sodium hydroxide solution of addition is 12 with the liquid-solid ratio of cellulose carbamate:1；In described third time mixed dissolution, the sodium hydroxide solution of addition is 14 with the liquid-solid ratio of cellulose carbamate:1.
Embodiment
10
On the basis of embodiment 1：
Preferably, in step C, the preparation of described cellulose carbamate solution is specially：
Cellulose carbamate is added in the sodium hydroxide solution that concentration is 8% at 0 DEG C, first time mixed dissolution is carried out；At -5 DEG C to mixture in add concentration be 10% sodium hydroxide solution, carry out second mixed dissolution；At -10 DEG C to mixture in add concentration be 12% sodium hydroxide solution, carry out third time mixed dissolution, obtain cellulose carbamate solution, i.e. spinning solution after rising to normal temperature.
Preferably, in step C, in described first time mixed dissolution, the sodium hydroxide solution of addition is 12 with the liquid-solid ratio of cellulose carbamate:1；In second described mixed dissolution, the sodium hydroxide solution of addition is 14 with the liquid-solid ratio of cellulose carbamate:1；In described third time mixed dissolution, the sodium hydroxide solution of addition is 16 with the liquid-solid ratio of cellulose carbamate:1.
Embodiment
11
On the basis of embodiment 1：
Preferably, in step C, the preparation of described cellulose carbamate solution is specially：
Cellulose carbamate is added in the sodium hydroxide solution that concentration is 7% at -2.5 DEG C, first time mixed dissolution is carried out；At -7.5 DEG C to mixture in add concentration be 9% sodium hydroxide solution, carry out second mixed dissolution；At -12.5 DEG C to mixture in add concentration be 11% sodium hydroxide solution, carry out third time mixed dissolution, obtain cellulose carbamate solution, i.e. spinning solution after rising to normal temperature.
Preferably, in step C, in described first time mixed dissolution, the sodium hydroxide solution of addition is 11 with the liquid-solid ratio of cellulose carbamate:1；In second described mixed dissolution, the sodium hydroxide solution of addition is 13 with the liquid-solid ratio of cellulose carbamate:1；In described third time mixed dissolution, the sodium hydroxide solution of addition is 15 with the liquid-solid ratio of cellulose carbamate:1.
Embodiment
12
On the basis of embodiment 1：
Preferably, in step C, the preparation of described cellulose carbamate solution is specially：
Cellulose carbamate is added in the sodium hydroxide solution that concentration is 7.6% at -2 DEG C, first time mixed dissolution is carried out；At -8 DEG C to mixture in add concentration be 9.5% sodium hydroxide solution, carry out second mixed dissolution；At -14 DEG C to mixture in add concentration be 11.5% sodium hydroxide solution, carry out third time mixed dissolution, obtain cellulose carbamate solution, i.e. spinning solution after rising to normal temperature.
Preferably, in step C, in described first time mixed dissolution, the sodium hydroxide solution of addition is 10.5 with the liquid-solid ratio of cellulose carbamate:1；In second described mixed dissolution, the sodium hydroxide solution of addition is 13.5 with the liquid-solid ratio of cellulose carbamate:1；In described third time mixed dissolution, the sodium hydroxide solution of addition is 14.5 with the liquid-solid ratio of cellulose carbamate:1.
Embodiment
13
On the basis of embodiment 1：
Preferably, in step D, in described spinning process, the composition and proportioning of coagulating bath are Na2SO4 230g/L, ZnSO48g/L, H2SO4
110g/L。
Embodiment
14
On the basis of embodiment 1：
Preferably, in step D, in described spinning process, the composition and proportioning of coagulating bath are Na2SO4 245g/L, ZnSO412g/L, H2SO4
140g/L。
Embodiment
15
On the basis of embodiment 1：
Preferably, in step D, in described spinning process, the composition and proportioning of coagulating bath are Na2SO4 237.5g/L, ZnSO410g/L, H2SO4
125g/L。
Embodiment
16
On the basis of embodiment 1：
Preferably, in step D, in described spinning process, the composition and proportioning of coagulating bath are Na2SO4 240g/L, ZnSO411g/L, H2SO4
130g/L。
Claims (10)
1. a kind of production technology of cellulose carbamate fibre long filament, it is characterised in that：Comprise the following steps that：
The activation of A, cellulose
First cellulose is added in sodium hydroxide solution and is soaked, carry out basification, after being disposed, filtration washing, then alkalinized celluloses are vacuum dried, obtain activated cellulose；
The preparation of B, cellulose carbamate
Take out to be placed in vacuum drying chamber to the liquid ammonia solution for adding urea in activated cellulose, after immersion and dry, then using heating using microwave, carry out esterification, obtain cellulose carbamate；
The preparation of C, cellulose carbamate solution
Cellulose carbamate is added in sodium hydroxide solution, first time mixed dissolution is carried out；Again to sodium hydroxide solution is added in mixture, second mixed dissolution is carried out；Third time carries out third time mixed dissolution to sodium hydroxide solution is added in mixture, and cellulose carbamate solution, i.e. spinning solution are obtained after rising to normal temperature；
D, spinning
Spinning solution in step C is made cellulose carbamate fibre long filament by wet spinning.
2. the production technology of a kind of cellulose carbamate fibre long filament according to claim 1, it is characterised in that：In step, described cellulose is the linter pulp of the degree of polymerization 400~600.
3. the production technology of a kind of cellulose carbamate fibre long filament according to claim 1, it is characterised in that：In step, the mass concentration 15~20% of described sodium hydroxide solution, described NaOH and the volume ratio of cellulose consumption is (4~6):1.
4. the production technology of a kind of cellulose carbamate fibre long filament according to claim 1, it is characterised in that：In step, the time of described immersion is 1~2h, and temperature is 5~15 DEG C.
5. the production technology of a kind of cellulose carbamate fibre long filament according to claim 1, it is characterised in that：In step, the described vacuum drying time is 1~3h, and temperature is 40~60 DEG C.
6. the production technology of a kind of cellulose carbamate fibre long filament according to claim 1, it is characterised in that：In stepb, described activated cellulose is 1 with urea in mass ratio:(2~4), the concentration of the liquid ammonia solution of urea is 20~40%.
7. the production technology of a kind of cellulose carbamate fibre long filament according to claim 1, it is characterised in that：In stepb, the heating power of described heating using microwave is 500~800W, and the heating response time is 1~3h.
8. the production technology of a kind of cellulose carbamate fibre long filament according to claim 1, it is characterised in that：In step C, the preparation of described cellulose carbamate solution is specially：
Cellulose carbamate is added in the sodium hydroxide solution that concentration is 6~8% at -5~0 DEG C, first time mixed dissolution is carried out；At -10~-5 DEG C to mixture in add concentration be 8~10% sodium hydroxide solution, carry out second mixed dissolution；At -15~-10 DEG C to mixture in add concentration be 10~12% sodium hydroxide solutions, carry out third time mixed dissolution, obtain cellulose carbamate solution, i.e. spinning solution after rising to normal temperature.
9. the production technology of a kind of cellulose carbamate fibre long filament according to claim 1 or 8, it is characterised in that：In step C, in described first time mixed dissolution, the sodium hydroxide solution of addition is (10~12) with the liquid-solid ratio of cellulose carbamate:1；In second described mixed dissolution, the sodium hydroxide solution of addition is (12~14) with the liquid-solid ratio of cellulose carbamate:1；In described third time mixed dissolution, the sodium hydroxide solution of addition is (14~16) with the liquid-solid ratio of cellulose carbamate:1.
10. the production technology 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 Na2SO4 230~245g/L, ZnSO48~12g/L, H2SO4110~140g/L.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108930071A (en) * | 2018-08-10 | 2018-12-04 | 高密云鹰新材料科技有限公司 | A kind of carbamate method prepares the production technology of regenerated cellulose staple fiber |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101104957A (en) * | 2007-08-20 | 2008-01-16 | 中国科学院新疆理化技术研究所 | Process for preparing cellulose carbamate fibre |
| CN102691125A (en) * | 2012-06-19 | 2012-09-26 | 武汉大学 | Method for preparing regenerated cellulose fibers with cellulose carbamate |
-
2015
- 2015-09-17 CN CN201510598807.4A patent/CN106702515B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101104957A (en) * | 2007-08-20 | 2008-01-16 | 中国科学院新疆理化技术研究所 | Process for preparing cellulose carbamate fibre |
| CN102691125A (en) * | 2012-06-19 | 2012-09-26 | 武汉大学 | Method for preparing regenerated cellulose fibers with cellulose carbamate |
Non-Patent Citations (1)
| Title |
|---|
| 哈丽丹•买买提等: ""尿素嵌入法生产纤维素氨基甲酸酯新工艺"", 《纤维素科学与技术》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108930071A (en) * | 2018-08-10 | 2018-12-04 | 高密云鹰新材料科技有限公司 | A kind of carbamate method prepares the production technology of regenerated cellulose staple fiber |
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| CN106702515B (en) | 2018-12-14 |
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