CN1041540C - Manufacture of regenerated cellulosic fibre by zinc free viscose process - Google Patents

Manufacture of regenerated cellulosic fibre by zinc free viscose process Download PDF

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CN1041540C
CN1041540C CN 93106008 CN93106008A CN1041540C CN 1041540 C CN1041540 C CN 1041540C CN 93106008 CN93106008 CN 93106008 CN 93106008 A CN93106008 A CN 93106008A CN 1041540 C CN1041540 C CN 1041540C
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viscose
spinning
zinc
spinning bath
cellulose
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CN1095431A (en
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伊达布海·赫姆钱德·佩尔凯
苏南达·库马·罗伊穆利克
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BIRLA RESEARCH INST FOR APPLIE
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Abstract

The present invention discloses a preparation technology for viscose fiber. In the present invention, viscose is spun into filaments in an acidic spinning bath; the differences between the spinning bath and traditional spinning baths lie in that the former does not contain zinc salts, the spinning bath contains sulfuric acid, aluminium sulfate and sodium sulfate, and temperature for spinning is controlled to be 35 DEG C to 60 DEG C. Furthermore, common stretching and subsequent spinning procedures are not changed. Produced regenerated cellulose fiber has a novel sectional plane, namely that an original sectional plane in the shape of the character C, and the fiber has the characteristics of high glossiness and good flexibility.

Description

The zinc free viscose process of the cellulose fibre of preparation regeneration
The present invention relates to a kind of adhering process that carries out the production of short rayon fiber, viscose filament yarn or viscose film.Be particularly related to and make viscose in the acid spinning bath that does not contain zinc salt, carry out spinning.
Adopt viscose process to produce the regenerated cellulose product, such as, viscose staple fibre, viscose film and viscose filament yarn, the first step is to handle by soda bath, and cellulosic material is changed into alkali cellulose.Then, alkali cellulose through pulverizing, experienced, further change into the cellulose xanthate after handling with carbon disulfide.The cellulose xanthate dissolves in the sodium hydroxide solution of dilution again, obtains the content of desirable cellulose and alkali with this.The solution that obtains thus is called viscose glue (Viscose), the also further filtration of this viscose glue, maturation, deaeration, extrudes from spinnerets and enters the spinning bath that mainly contains sulfuric acid, zinc sulfate and sodium sulphate then.
The spinning bath of traditional handicraft mainly contains zinc sulfate or some other soluble zinc salt as the regeneration inhibitor.No matter in viscose or in spinning bath, all can form the yellow acid zinc salt in viscose filament yarn as long as contain zinc salt, this yellow acid zinc salt is much more stable than sodium cellulose xanthate, so long filament is stood stretching.As everyone knows, zinc is a kind of hypertoxic chemical substance, also is extremely harmful even there is the content of PPm in waste water, especially the water source that zinc can polluted drinking water and aquatile produced adverse influence.Except the problem of pollution aspect, in viscose process, use zinc sulfate to also have other disadvantage too much; Such as costing an arm and a leg and being easy in spinning equipment, form deposit to a certain extent.
Except containing zinc sulfate, also contain other viscose modifier in the spinning bath,, be particularly useful for the production of polynosic fibre such as polyethylene glycol, poly(ethylene oxide), amine and formaldehydes etc. as complementary regeneration inhibitor.All these viscose organic modifiers not only bring difficulty to processing, but also contaminated air and water source produce adverse influence to natural environment.
Therefore, in some gyp application, for example when carrying out the production of common viscose fiber, wish to develop a kind of technology of not having zinc fully at least.
Main purpose of the present invention is to develop complete zinc free viscose method and carries out the production of regenerated celulose fibre.
Another object of the present invention is to provide a kind of technology and spinning bath to alleviate to air and contaminated water source.
The 3rd purpose of the present invention is to provide a kind of new technology, and this process using does not contain the viscose solution and the spinning bath of zinc or zinc salt, still brings into play gratifying regeneration interception, makes that the fiber of extrusion molding has necessary strength in spinning bath.
The 4th purpose of the present invention is to provide a kind of technology, and this technology can be used in existing compound in the spinning bath, thereby reduces the technology cost and can also guarantee the reliability of technology.
The 5th purpose of the present invention is to provide a kind of preparation technology of viscose and wherein employed spinning bath, it helps the aquation of viscose filament yarn and the stability of xanthate, play the effect of instead of zinc, can to air and the water source pollute and can fouling in spinnerets or spinning bath pipeline.
The 6th purpose of the present invention is to provide the production technology of the fiber that a kind of glossiness, flexibility and feel be improved.
The 7th purpose of the present invention is to remove the zinc salt that exists in the viscose glue production, and can not produce adverse influence to production process.
The 8th purpose of the present invention is to adopt no zinc salt viscose process to produce various common viscose fiber, comprises the viscose of different dawn numbers, length, solution dyeing (coloured) and other conventional variety.
The 9th purpose of the present invention is to provide a kind of production to have the technology of the fiber of improved dyestuff adsorptivity.
The of the present invention ten purpose is to provide a kind of improved technology, do not have additive in the employed viscose goods in this technology.
Therefore, the 11 purpose of the present invention is to provide a kind of improving one's methods of viscose of producing, and do not contain additive in the employed viscose goods in this method, in spinning bath fully without zinc or zinc salt as the regeneration inhibitor.
Other purpose of the present invention and advantage can be clear that from following description very much.
In order to achieve the above object, we tried out various divalence and trivalent metal ion, for example magnesium sulfate, ferric sulfate and aluminum sulfate etc., and some organic compounds, and urea for example, and the decomposition rate constant of cellulose xanthate studied.Substitute in a large amount of research that zinc carries out in the spinning bath for seeking out a kind of non-toxic compound, we find aluminum sulfate comparison zinc sulfate, and not only economy but also suitable environment are optimal chemical substances.Use aluminum sulfate that the pollution of waste water is obviously reduced.
Common viscose cross section indentation and inhomogeneous.The shape in viscose cross section has very big influence to some important characteristics, and these characteristics comprise glossiness, fullness and feel.As everyone knows, uniform non-zigzag " C " shape or the gloss of tee section increase fiber partially.
We notice that we can realize purpose of the present invention at the technology of exploitation, and deeply convince that aluminum sulfate can replace the zinc sulfate in the spinning bath easily and can not produce any problem.Its way is that in process of production, spinning bath does not add zinc salt, and progressively adds aluminum sulfate.
We notice that further we can the production cross section be the filament of uniform " C " shape, and the characteristic of silk is improved.
We are also noted that the soft property of dyestuff of fiber is better than adding the fiber that zinc technology is made in the present invention, and the few effect of dye dosage is then identical.
In the traditional handicraft of producing viscose, viscose and spinning bath must contain zinc salt, and this is because the formation of zinc cellulose exanthate is depended in the shaping of viscose epidermal area structure.It is believed that zinc compound is the plasticity of the plain yellow acid gel of zinc of fortifying fibre greatly, thereby draw speed is greatly faster than sodium cellulose xanthate.Although a lot of theoretical important function that all zinc and zinc cellulose exanthate play for the moulding of viscose in emphasizing viscose process,, zinc cellulose exanthate does not also have conclusion in this problem that whether can play a key effect aspect the viscose moulding.
Someone proposes, acid spinning bath does not contain zinc salt under the certain situation, but in order to remedy the effect of zinc, use multiple three grades of monoamines, such as methylol, dimethyl amine, methylol methyl amine (methylol metha methyl amine), methylol diethylamide, other amine such as diethylamide or aldehydes, such as formaldehyde etc. as regeneration inhibitor or additive in viscose or the spinning bath.All these modifier all make cost increase or contaminated air and water source in a different manner.Also do not have what practical ways can reclaim this class additive at present from spinning bath, therefore this class additive or their product are cumulative in spinning bath.Therefore, the waste water of discharge must be handled, and this is very undesirable, because they have increased biological aerobic value (B.O.D) greatly, this value must be reduced to the required standard that meets country.
The somebody proposes, and suggestion is used in zinc sulfate to aluminium compound or does not have in the spinning bath of zinc sulfate, but does not have a kind of feasible method to make it to reach business-like scale up till now.
In brief, our invention provides a kind of technology of improved production regenerated fiber silk, and the regenerated celulose fibre that is gone out by explained hereafter of the present invention increases gloss and flexibility; The cross section of viscose is " C " shape, and has good epidermal structure; Comprise the viscose grade slurry is made the cellulose that contains 33%-34% and the NaOH alkali cellulose of 15.55%-16.00% in concentration is the soda bath of 17.5%-18.5%; Alkali cellulose through pulverizing, experienced be the 35-75 viscose of second to obtain viscosity (falling ball method); After the carbon disulfide of adding 28%-33% reacts, alkali cellulose transforms into the cellulose xanthate, be prepared into viscose after this cellulose xanthate dissolved in rare soda bath, wherein contain the cellulose of 6%-11% and the caustic soda of 52%-60%, through spinning in spinning bath after the maturation; It is characterized in that spinning bath does not contain zinc, imitative silk contains sulfuric acid 6.5%-12%, aluminum sulfate [Al in bathing 2(SO 4) 3] 0.3%-2.0%, sodium sulphate 18%-26% is subsequently with viscose drawn, regeneration, desulfurization, bleaching, modification (finishing) and drying.
The preferred technology of the present invention may further comprise the steps:
The viscose grade slurry in containing 17.5%~18.5% soda bath, is removed unnecessary alkali reaching suitable content through extruding, thereby made alkali cellulose contain the cellulose of 33%-34% and the NaOH of 15.5%-16%.Alkali cellulose is the 35-75 falling sphere viscose of second through pulverizing and the experienced viscosity (falling ball method) that obtains, and alkali cellulose is handled with the carbon disulfide of 28%-33% then.The cellulose xanthate that generates is dissolved in rare caustic lye of soda, prepares the viscose that contains 6%-11% cellulose and 52%-60% NaOH, passes through filtration, deaeration and maturation again, and the Huo Dunluoshi index of viscose is 7-12.With its spinning in spinning bath, spinning bath contains the sulfuric acid of 6.5%-12%, the aluminum sulfate [Al of 0.3%-2.0% 2(SO 4) 3] and the sodium sulphate of 18%-26%.Other slaine such as magnesium sulfate, ferric sulfate, also can use.This spinning technique has been removed zinc salt fully.Spinning bath temperature and spinning speed are controlled at respectively in the scope of 35 ℃-' 60 ℃ and 30 meters/minute-75 meters/minute.The viscose that obtains thus stretches in air, and extensibility is 35%-70%.Then, viscose is through thoroughly finishing desulfurization, bleaching, modification and drying according to routine after the regeneration.
The cross section of adopting the viscose that technology of the present invention (that is: aluminum sulfate technology) makes and compares with the common viscose that adopts zinc sulfate technology to make and the sectional view (as shown in Figure 3) of high-wet-modulus fibre (HWM) as shown in Figure 1.Can be clear that very that from figure the fiber that adopts technology of the present invention to make has " C " tee section uniformly, skin forming is good and the spill wrinkle are arranged.The gloss and the soft feeling of fiber also improved in this cross section.
Also once proposed in papers more of the prior art to attempt with aluminium salt instead of zinc or zinc salt.
This type of paper of the prior art of first example proposes to adopt high-concentration sulfuric acid aluminium, and its consumption in spinning bath can be half of sulfuric acid or suitable with it.Also further propose with the additive of aluminium hydroxide in this article as viscose.But the combination of this aluminium salt does not have to form the feasible technology of commercialization.In addition, compare with technology of the present invention, the performance of the viscose that is obtained by this method improves not quite.
This type of paper of the prior art of second example proposes to adopt a kind of special method for preparing viscose glue alkali lye, comprises with sodium carbonate and NaOH and carries out special neutralization, and propose to adopt the aluminum sulfate spinning bath.Because viscose glue alkali needs special preparation, and takes method for distinguishing can not make fiber deposit (precipitation) again in spinning bath, this technology does not reach commercialization yet.Moreover, because preparation viscose glue alkali lye needs special centrifugal device and compound, cause technology cost costliness.
This type of paper of the prior art of the 3rd example proposes to adopt water-bath, and sulfuric acid is identical with addition of aluminum sulfate in the bath.The latter also can be Duoed one times than the former, in addition, this organic compound of a certain amount of naphthalene sulfonic acids of this technological requirement, the result has increased the complexity of technology and has improved cost.
The 4th this type of paper of the prior art (C.A-99-1983-54949d) of example research be in coagulating bath polyvalent metal ion to the influence of cellulose xanthate decomposition rate.This paper proposes to use in spinning bath the aluminum sulfate of same amount to replace zinc salt.Therefore the ratio of aluminum sulfate reaches very high degree, accounts for 20% of sulfuric acid consumption.The research work demonstrates the reduction of xanthate hydrolysis, clearly can not improve fiber properties and obtain " C " tee section.
Contain sulfuric acid, sodium sulphate, zinc sulfate in the spinning bath that this type of paper of the prior art suggestion of the 5th example is adopted and Duo three times aluminum sulfate than zinc sulfate.This technology is not eradicated zinc salt, thereby the characteristic of fiber is subjected to the influence of zinc salt.
The no zinc coagulating bath that contains polyvalent metal ion is adopted in this type of paper suggestion of the prior art of the 6th example, and this polyvalent metal ion of aluminium content in bath is very big.Yet because the content of polyvalent metal ion is big, the characteristic of fiber is unsatisfactory far away, and this fiber does not also have all characteristics of the fiber that the present invention obtains.
This type of paper of the prior art of the 7th example proposes to replace zinc sulfate with aluminum sulfate in spinning bath.At present relevant details is not still understood.Yet if aluminum sulfate replaces zinc sulfate and uses, its consumption should be suitable.
By various experiments, we find that above-mentioned technology all can not make fiber obtain and improve " C " tee section of glossiness, nor can have other good characteristic concurrently, and for example, intensity is big, curl, regenerate that prevention speed is low, extensibility is high and the dyestuff compatibility is good.
By number of research projects, we have been surprised to find that a kind of technology of uniqueness can make the fiber that makes possess aforesaid all good characteristics especially, and the cross section of fiber is " C " shape.In addition, if the consumption that the component in the spinning bath is adjusted and reduced aluminum sulfate as much as possible will reduce the pollution of environment.
We also find, the consumption that only reaches optimized aluminum sulfate is also not all right, its consumption should be interrelated with the consumption of other component, make spinning bath reach a kind of balance, the assurance fiberizing is rapid, and viscose regeneration prevention property is good, solidifies easily and forming, spinnability and draftability are big, and glossiness height, fiber smooth in appearance, soft, compound amount is few and advantage such as repeatability.
As far as our knowledge goes, where do not adopt or where do not deliver even advised also having concurrently the technology of above-mentioned complete characteristic except making " C " tee section fiber, this is confirmed by above-mentioned example.
The content of aluminum sulfate is lower than 0.3% and does not guarantee gratifying regeneration interception, is higher than 2% and can hinders the production of cross section for the fiber of " C " shape, thereby influence glossiness.The content range of aluminum sulfate should be 1/10 to 1/90 of sodium sulphate, 1/5 to 1/50 of sulfuric acid.
So low aluminum sulfate content can only help to make technology to obtain business-like feasibility, the reliability and the repeatability of height.
Aspect the compound of seeking non-toxic inexpensive, we find that aluminum sulfate is the most desirable substitute of zinc in spinning bath, aluminium compound with alkali-soluble, such as aluminum sulfate, aluminium hydroxide or sodium aluminate, add on a small quantity in the viscose and can and play assistant carrier, in spinning technique, play the effect that reduces the sulfonate decomposition rate as dispersant.
In experimentation, we have found and have a kind ofly added aluminum sulfate and thoroughly eradicate the method for the common viscose fiber commercially produced of zinc compound in spinning bath.Viscose can contain also can not contain additive.
The present invention is spun into silk with viscose in no zinc spinning bath, the aluminum sulfate that spinning bath contains can guarantee that a large amount of epidermal area of viscose forms its amount and is same as or is higher than the result that spinning bath contains zinc sulfate.During spinning bath sulfur acid aluminium, the new tow that is shaped is not suppressed aspect stretching.The acid spinning bath of spinning viscose contains sulfuric acid, sodium sulphate and aluminum sulfate.The aerial extensibility of viscose is between 35% and 70%.Then, conventional operations such as desulfurization, bleaching, modification are carried out in the holomorphosis in the rare acid bath of temperature between 80 ℃ and 100% of viscose glue length silk again.
Application the present invention carries out spinning and can adopt any suitable well-known sizing composition aspect the viscose moulding.Preferably use degree of polymerization distribution uniform fibers element when the preparation viscose, scope is made by kraft pulp, sulphite, cotton linter or low temperature caustic soda refining slurry between 300 to 1000.This technology can be selected viscose composition traditional or modification for use, wherein contains the cellulose of the 6%-11% that has an appointment and the caustic soda of 52%-60%.The preparation of viscose can be carried out according to convention, uses a certain amount of carbon disulfide, and for example 28%-33% makes the alkali cellulose sulfonation, to produce the viscose solution that ripening index is 7-12 ° of H.
When in no zinc spinning bath, spinning viscose, contain the sulfuric acid of 6.5%-12%, the sodium sulphate of 18%-28% and the aluminum sulfate of 0.3%-2.0% in further preferably bathing, bathe temperature between 35 ℃ and 60 ℃.The viscose that is generated is stretched in air to a certain degree, and for example, extensibility is 35%-70%.
Aluminum sulfate in the spinning bath of this technology is to CS 2Or the recovery of salt has no effect, and increases CS on the contrary 2And H 2The burst size of S gas.Al in the spinning bath 2(SO 4) 3Relatively zinc sulfate has more economy and is of value to environment.As a result, contaminated wastewater is reduced significantly.
To further be illustrated the present invention in conjunction with following embodiment, but and unrestricted the present invention.
Fig. 1 is the enlarged drawing (about 1000x) that the present invention is spun into (containing aluminium technology) the fibre section microphotograph of fiber.
Fig. 2 contains zinc spinning bath technology (ZnSO for example for adopting 4) be spun into the fibre section enlarged drawing (about 1000x) of general fibre.
Fig. 3 is the fibre section microphotograph enlarged drawing of business-like high-wet-modulus fibre.
Embodiment 1
Common viscose glue slurry is immersed in and contains in 17.5% the sodium hydroxide solution, and unnecessary alkali is got rid of by extruding.The alkali cellulose of so making is through pulverizing and wearing out.Alkali cellulose after aging is handled containing on the basis of alpha fibers the carbon disulfide with 30%.So the sodium cellulose xanthate that forms dissolves in rare caustic lye of soda to form viscose again.Viscose contains 10% cellulose and 5.8% NaOH, and falling ball method viscosity is 55 seconds.Viscose is through after filtration, deaeration and reaching the ripening index of 10 ° of H, squeezes into to contain in the spinning bath that 8% sulfuric acid, 23% sodium sulphate, 0.46% aluminum sulfate and temperature be 50 ℃.Spinning bath does not contain zinc salt.Viscose extensibility in air is 40% to 60%, after viscose is stretched, cuts into short silk.Fiber is finished regeneration in temperature is 95 ℃ acid bath then, and desulfurization, bleaching, modification and drying are carried out routinely.The fiber of producing also has following properties except that its cross section is " C " shape: the dawn number: 1.51 do strong (gram/dawn): 2.63 wet strong (gram/dawn): 1.35 wet doing by force than (%): 51.4 dried degree of stretching (%): 20.8 wet degree of stretching (%): 23.6 embodiment 2
The preparation of viscose removes NaOH and CS 2The content difference outside, all the other are identical in embodiment 1.Content of cellulose in the viscose is 9.5%, and alkali is 54%.Viscosity during the viscose spinning is 48 seconds (falling ball method) at 20 ℃.Spinning bath contains sulfuric acid, the 6 grams per liter aluminum sulfate of 95 grams per liters, the sodium sulphate of 290 grams per liters, and the temperature of spinning bath is 48 ℃.The aerial extensibility of 1.2 dawn viscoses of new moulding is 48%, and refining and back arrangement are carried out routinely.The fibre section of producing is " C " shape, gloss height, good hand touch.Its physical characteristic is as follows: the dawn number: 1.17 do strong (gram/dawn): 2.50 wet strong (gram/dawn): 1.24 wet doing by force than (%): 49.7 dried degree of stretching (%): 17.5 wet degree of stretching (%): 22.0 embodiment 3
The viscose preparation is same as embodiment 1.The slurry of selecting for use natural material to make, ripening index are 9.6 ° of H, are used at the molten spinning 3 dawn viscoses of extruding of spinning.Spinning bath contains 8.5% sulfuric acid, 0.46% Al 2(SO 4) 3, 23% sodium sulphate, the temperature of spinning bath is 50 ℃.Spinning speed is 45 meters/minute.The aerial extensibility of viscose is 47%, cuts into short silk.Refining and arrangement are carried out routinely.
The fiber smooth in appearance of producing does not almost have zigzag.The cross section is " C " shape.Its physical characteristic is as follows: the dawn number: 3.30 do strong (gram/dawn): 2.35 wet strong (gram/dawn): 1.22 Wen Ganqiang are than (%): 51.9 dried degree of stretching (%): 20.0 degree of stretching (%) that wet: 23.3 embodiment 4
The viscose that contains 10.3% cellulose and 5.7% alkali is prepared from 30% 2 sulfo-carbon, and viscosity is 57 seconds (falling ball method).This viscose is through after filtration, deaeration and reaching the ripening index of 10.3 ° of H, squeezes into to contain in the spinning bath that 7.7% sulfuric acid, 1.1% aluminum sulfate, 22.5% sodium sulphate and temperature be 47 ℃.The aerial extensibility of viscose is 52%.The refining arrangement is undertaken by the explanation among the embodiment 1.
The viscose of producing also has following properties except that its cross section is " C " shape: the dawn number: 1.53 do strong (gram/dawn): 2.60 wet strong (gram/dawn): 1.31 wet doing by force than (%): 50.5 dried degree of stretching (%): 20.0 wet degree of stretching (%): 23.5 embodiment 5
The preparation of A, B kind viscose is undertaken by the explanation among the embodiment 1, carries out spinning in the sodium sulphate acid bath of the aluminum sulfate of the sulfuric acid that contains the 95-100 grams per liter, 6 grams per liters and 290 grams per liters.The spinnerets hole count is 19,000, and each bore dia is 70 microns.A, B viscose dawn number are respectively 1.15 and 1.5, and extensibility is 50% and to be cut to length be 44 millimeters short silk.Holomorphosis of short silk and desulfurization routinely, bleaching, arrangement and drying.Fiber carries out dyestuff compatibility and yarn strength test.
A kind fiber B kind fiberoptic fiber specification: millimeter 1.5 dawn * 44,1.15 dawn * 44 millimeter dawn number: 1.13 1.41 do by force, (gram/dawn): 2.67 2.38 is wet strong, (gram/dawn): 1.32 1.18 wet do by force than, (gram %): 49.3 49.4 dried degree of stretching, (%) 19.0 18.8 wet degree of stretching, (%): 23.8 22.0 yarn strengths: spinning count: 40 40 thread tests, (pound): 57.6 53.4C.S.P., 2,304 2136 dyestuff compatibilities: be higher than and contain zinc and be higher than and contain zinc
The general technology of technology general
The logical viscose of logical viscose
The good COLOR FASTNESS of COLOR FASTNESS is good
Glossy feel: good hand touch good hand touch
The effect of hydrochlorate is to reduce regeneration speed, yet the most important thing is to be to dewater and saltout, and is common to various solutions.The coagulation force of ammonium salt is than sodium salt height, and the coagulation force of magnesium ion is identical with sodium ion.Heavy metal ion is more more effective than sodium ion or magnesium ion such as zinc ion, iron ion.The regeneration interception of this cationoid is identical with its coagulation force, along this thinking, has just found the most fruitful aluminium salt, especially aluminum sulfate.
Technology of the present invention has been successfully used to commercially produce, can produce the fiber of all size of dawn number from 0.8 to 12.Embodiment 6
The preparation of viscose is by the carrying out of explanation among the embodiment 1, and ripening index is 10 ° of H, and viscose is spun into silk in two kinds of different spinning baths.
A kind viscose is to make silk in 49 ℃ the spinning bath containing 8.5% sulfuric acid, 0.5% magnesium sulfate, 23% sodium sulphate dawn temperature, and extensibility is 42%.
B kind viscose is to be spun into silk in 49 ℃ the spinning bath containing 8.5% sulfuric acid, 0.5% ferric sulfate, 22.5% sodium sulphate and temperature, and extensibility is 45%.
The extensibility of tow contains MgSO in acid bath 4Situation under be reduced to a certain degree, and the brightness of fiber also reduces.Spinning bath is containing FeSO 4Situation under, the cross section of two kinds of fibers is irregular shape, on one side or both sides have pleated.Fiber properties is as follows:
A kind fiber B kind fiber Denier: 1.57 1.45 do strong (gram/dawn): 2.54 2.52 wet doing by force than (%): 48.0 49.2 dried degree of stretching (%): 19.5 18.7 wet degree of stretching (%): 22.6 23.8 embodiment 7
The commercialization test of present embodiment has obtained success.The preparation of viscose is undertaken by the explanation of embodiment 1.Spinning bath contains the aluminum sulfate of 7.8%-10% sulfuric acid, 0.4%-0.6% and the sodium sulphate of 22%-24%, and temperature is controlled between 46 ℃ and 49 ℃.The desulfurization bleaching and the various arrangement of fiber are carried out routinely.
The fiber of producing is being significantly improved aspect glossiness and the flexibility; Be better than adopting and contain the fiber that zinc technology is produced.Fiber properties is as follows:
A B C D fiber dimensious: dawn * 12, dawn * 0.8,1.5 dawn * 1.2 dawn *
57 millimeters 51 millimeters 51 millimeters 51 millimeters dawn numbers: 1.51 1.61 0.9 11.7 do strong (gram/dawn): 2.54 2.57 2.59 1.75 wet strong (gram/dawn): 1.31 1.37 1.32 0.71 wet doing by force than (%): 51.7 53.0 51.0 40.6 dried degree of stretching (%): 19.1 18.1 18.4 28.5 wet degree of stretching (%) 23.2 19.3 18.9 34.6 crimp percents (%): 12 12 16 12 yarn strength C.S.P. (40): the various fibers of 1,836 2076 2100-all are " C " tee section
Replace zinc salt although we have only gone through with aluminum sulfate, the metal ion of other divalence and trivalent also can replace aluminum sulfate and use, as magnesium sulfate and ferric sulfate.Also have other similar compounds that is suitable for also can be used alone or as a mixture under certain conditions.

Claims (1)

1, good, the fibre section of a kind of producd fibers glossiness height and flexibility is the technology of " C " shape, regenerated celulose fibre that skin forming is good, comprise: viscose glue slurry is immersed in the soda bath that concentration is 17.5%-18.5%, generates the alkali cellulose fiber of the NaOH of the cellulose that contains 33%-34% and 15.55%-16.00%; Alkali cellulose is the 35-75 viscose solution of second through pulverizing and experienced back formation falling ball method viscosity; Carbon disulfide with 28%-33% makes alkali cellulose change into the cellulose xanthate; Xanthate is dissolved in rare caustic soda prepares viscose, this viscose contains the cellulose of 6%-11% and the caustic soda of 52%-60%; Viscose is spun into silk through after the maturation in spinning bath, stretch routinely again after viscose spins out, regeneration, desulfurization, bleaching, modification and drying, it is characterized in that not having zinc in this spinning bath, wherein contain the sulfuric acid of 6.5%-12%, the aluminum sulfate [Al of 0.3%-2.0% 2(SO 4) 3] and the sodium sulphate of 18%-26%; The scope of the spinning bath temperature of spinning between 35 ℃-60 ℃, the scope of spinning speed from 35 meters/assign to 75 meters/minute, the viscose of moulding extensibility scope in air is 35%-70%.
CN 93106008 1993-05-22 1993-05-22 Manufacture of regenerated cellulosic fibre by zinc free viscose process Expired - Lifetime CN1041540C (en)

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CN100359050C (en) * 2004-11-16 2008-01-02 唐山三友集团化纤有限公司 High whiteness and strength adhesive short fiber and process for making same
CN100335689C (en) * 2005-12-29 2007-09-05 山东海龙股份有限公司 Method for producing viscose fiber by using zinc-free coagulating bath
CN103562277A (en) * 2011-05-20 2014-02-05 伊诺维亚薄膜有限公司 Process for processing cellulose films or shaped articles
CN107254718A (en) * 2017-05-05 2017-10-17 东至县鸿棉工贸有限责任公司 A kind of short flannel pulping process
CN112708962B (en) * 2020-12-05 2022-08-05 潍坊欣龙生物材料有限公司 Red yeast rice extract modified protein/cellulose composite fiber and preparation method thereof

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CN100417764C (en) * 2006-09-08 2008-09-10 唐山三友集团化纤有限公司 Ultrashort viscose fiber in paper making, and manufacturing method
CN105714389A (en) * 2016-03-29 2016-06-29 恒天海龙(潍坊)新材料有限责任公司 Special-shaped cross section viscose filament yarn and preparation method thereof
CN105714389B (en) * 2016-03-29 2019-04-26 恒天海龙(潍坊)新材料有限责任公司 Special-shaped cross section viscose filament yarn and preparation method thereof

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