CN101628986B - Production method of natural cellulose membrane - Google Patents
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- CN101628986B CN101628986B CN2009100978672A CN200910097867A CN101628986B CN 101628986 B CN101628986 B CN 101628986B CN 2009100978672 A CN2009100978672 A CN 2009100978672A CN 200910097867 A CN200910097867 A CN 200910097867A CN 101628986 B CN101628986 B CN 101628986B
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Abstract
The invention discloses a production method of natural cellulose membranes, comprising the following steps: (a) immersion; (b) squeezing; (c) grinding; (d) maturing; (e) etiolation; (f) solution; (g) film formation; (h) desulfuration; (i) bleaching; (j) plastification; and (k) drying. The production method has the advantages of mild reaction condition, short spacings among the prepared natural cellulose membranes, stable expansion rate and tensile strength, proper stiffness and flexibility, better colour and luster, good transparence, high hygiene property, and the like, improves the surface property of paper through the plastification, in particular enhances the smoothness of paper surfaces, improves the printability, reduces the deformability of paper and the moisture absorption, thereby reaching the new requirement of modern printing and packaging.
Description
Technical field
The present invention relates to chemical material field, relate in particular to a kind of production method of natural cellulose membrane.
Background technology
Natural cellulose membrane has environmental protection, excellent performance such as nontoxic, and for example Chinese invention patent 90109250.9 discloses and a kind ofly adopted cotton stalk Pericarppium arachidis hypogaeae to prepare the novel method of regenerated cellulose film.With 4.5～5% salpeter solutions to cotton stalk, Pericarppium arachidis hypogaeae hydrolysis after, handle through NaOH, obtaining the cotton stalk fiber cellulose content is 90%, Mn=1.56 * 10
5With the Pericarppium arachidis hypogaeae content of cellulose be 91%, Mn=1.52 * 10
5, and then configuration Mierocrystalline cellulose copper ammon solution, after filtration behind the knifing, coagulation forming in diluted alkaline and diluted acid.
But it is all undesirable to utilize method of the prior art to prepare indexs such as natural cellulose membrane slippery, intensity.
Summary of the invention
The production method of the natural cellulose membrane that the invention provides a kind of reaction conditions gentleness, be easy to control, final product quality is high.
A kind of production method of natural cellulose membrane comprises the steps:
(a) dipping
It is in 16～19% the aqueous sodium hydroxide solution that the cotton pulp dregs of rice are inserted mass percent concentration, soaks 15～30 minutes at 50～70 ℃, obtains the steeping fluid of soda cellulose.
As preferably, the cotton pulp dregs of rice can be inserted mass percent concentration and be in 18% the aqueous sodium hydroxide solution, soaked 20 minutes at 60 ℃, obtain the steeping fluid of soda cellulose.
Natural cellulose generally speaking can not with other material generation chemical reaction, must be made into soda cellulose earlier and just can carry out the reaction of back, the purpose of dipping is exactly to allow the cellulose conversion be the soda cellulose (sodium cellulosate) that can carry out chemical reaction.
The cotton pulp dregs of rice can adopt the existing general various cotton pulp dregs of rice.
(b) squeezing
Alkali lye unnecessary in the steeping fluid is squeezed the soda cellulose that separates after obtaining squeezing.
Squeezing can be adopted general squeezing machine, and squeeze pressure is 0.095 ± 0.015Mpa.
Generally squeeze first fibre (alpha-cellulose) content 32% (mass percent) in soda cellulose, alkali (sodium hydroxide) content 17% (mass percent) is for well.
As preferably, add squeezing auxiliary agent fatty alcohol-polyoxyethylene ether in the squeezing forward direction steeping fluid, the adding of fatty alcohol-polyoxyethylene ether can improve dipping effect, improves the squeeze and filter effect.
The squeezing auxiliary agent can be selected the Visco 44 of BASF AG's production for use and have similar structures and the peregal of function.
The mass ratio of squeezing auxiliary agent and step (a) middle cotton pulp is 1: 3000～4000, preferred 1: 3400～3600.
Behind the cotton pulp dregs of rice dipping, must be separated the alkali lye of surplus, because excessive alkali can hinder CS in the soda cellulose
2To the fine internal divergence of alkali, can make soda cellulose yellow acid fat caking, yellow is inhomogeneous, so that the dissolving difficulty.
(c) pulverize
Soda cellulose after the squeezing is pulverized, become the tiny granular attitude of loose bits.
Pulverizing can be adopted general-purpose equipment, and the particle size after pulverizing theoretically is the smaller the better, but the particle size after considering that easy to process and cost is general and pulverizing is below 0.5mm.
(d) experienced
Soda cellulose after pulverizing at 55～80 ℃, is placed and carried out experienced in 2～4 hours.
Preferably, place and carried out experienced in 2.5 hours at 60 ± 2 ℃.
Experienced be soda cellulose at a certain temperature, place the regular hour, by means of the oxygenizement of air, the macromolecular chain of soda cellulose is ruptured, polymerization degree decline is to reach the suitable viscosity of spinning the paper viscose glue.
(e) yellow
It is that 8～12% aqueous sodium hydroxide solution soaks and alkalizes in advance that soda cellulose after experienced is added earlier mass percent concentration, feeds CS again
2Carry out the yellow reaction and obtain Mierocrystalline cellulose yellow acid fat.
During pre-the alkalization:
Aqueous sodium hydroxide solution concentration preferred 10%;
Aqueous sodium hydroxide solution and experienced after the mass ratio of soda cellulose be 1: 6～8;
Pre-alkalization time is 30～60 minutes, the product oxygen-permeable is improved in preferred 40～60 minutes;
CS
2With the mass ratio of soda cellulose after experienced be 1: 8～12;
In 30～100 minutes yellow reaction times, the yellow temperature of reaction is 18～35 degree.
Soda cellulose is by the CS of phase
2Reaction makes undissolved soda cellulose generate the Mierocrystalline cellulose yellow acid fat of solubility.
(f) dissolving
Mierocrystalline cellulose yellow acid fat is dissolved in diluted alkaline or the water to form spins the paper viscose glue.
Described diluted alkaline is that mass percent concentration is 0.3～0.6% aqueous sodium hydroxide solution, and the preferred mass percentage concentration is 0.5%.
Mierocrystalline cellulose yellow acid fat contacts with diluted alkaline or water, and at first yellow acid fat gene the intensive solvation can take place begins swelling, and the distance between the macromole increases, and so a large amount of lyosorption molecules and constantly disperseing spin the paper viscose solution uniformly until forming.The dissolving of Mierocrystalline cellulose yellow acid fat is exactly a swollen process.
As preferably, can adopt two-part, promptly be divided into and just dissolve and the back dissolving, just dissolve the main swelling action that takes place, the back dissolving is to make Mierocrystalline cellulose yellow acid fat gamma value dissolve formation more uniformly to spin the paper viscose glue.
Dissolving just and back dissolving are generally all carried out in room temperature, and first dissolution time 20～40 minutes is added diluted alkaline or water after just dissolving is finished, back dissolving dissolution time 180～240 minutes.
Diluted alkaline or water consumption are 1.8～2.2 times of Mierocrystalline cellulose yellow acid lipid amount during dissolving just.
Diluted alkaline of adding when dissolve the back or water consumption are 7～8 times of Mierocrystalline cellulose yellow acid lipid amount.
This step obtains spins the paper viscose glue:
Viscosity is 48 ± 2s; The viscosity at this place is the required time representation of 20cm with the small ball of certainweight by the viscosity tube distance.
Instrument: ((pipe range 320mm is carved with the scale of 20cm up and down to stopwatch 2mm steel ball to weigh 0.13 ± 0.01g) round bottom viscosity tube.
Measuring method: viscose glue is filled in viscosity tube (internal diameter 2.5cm, high 20cm), little steel ball (2mm) is aimed at viscosity tube central authorities put down, little steel ball is viscosity by 20cm required time (reading is accurate to 0.1 second).
(g) film forming
The viscose glue that utilizes film-forming apparatus that step (f) is obtained is sprayed onto and obtains the natural cellulose membrane crude product in the precipitation bath.
The spray seam of shower nozzle can be adjusted according to the thickness needs of film.
45～55 ℃ of described coagulation bath temperatures, preferred 48～49 ℃.
For containing the aqueous solution of sulfuric acid and sodium sulfate, wherein sulfuric acid concentration is 140～143g/l in the precipitation bath; Sodium sulfate concentration is 210～230g/l.
But containing a lot of impurity, the natural cellulose membrane crude product inside that obtains of this moment just can produce water white natural cellulose membrane by further processing.
(h) desulfurization
It is to soak in 0.1～0.5% the aqueous sodium hydroxide solution to carry out desulfurization in 20～50 seconds and handle that the natural cellulose membrane crude product is put into mass percent concentration, obtains the natural cellulose membrane crude product after the desulfurization.
90 ℃～110 ℃ of soaking temperatures; Preferred 30 seconds of soak time;
The mass percent concentration of aqueous sodium hydroxide solution preferred 0.2%;
Participate in a large amount of sulphur of chemical reaction generation owing to spin the by product that contains in the paper viscose glue, the sulphur of generation, greatly part enters precipitation bath, is tiny colloidal suspended substance.The sulphur of staying in the paper film accounts for cellulosic 1%.Owing to contain more sulphur in the paper film, make paper be faint yellow or oyster white, transparency is very low, frowziness, wiriness is handled so must carry out desulfurization, and the sulphur content of finished film is dropped to below 0.004.
(i) bleaching
Natural cellulose membrane crude product after the desulfurization is inserted natural cellulose membrane crude product after soak at room temperature obtained bleaching in 20～50 seconds in the aqueous sodium hypochlorite solution.
The preferred immersion 30 seconds.
The mass percent concentration of aqueous sodium hypochlorite solution is 0.05～0.2%, preferred 0.1%.
Natural cellulose membrane crude product after the desulfurization is gloss developing not still, because remaining sulphur is arranged in the paper, leaves inorganic pigment on the paper, be to improve whiteness, and transparency, glossiness must be bleached processing.
(j) plasticising
Natural cellulose membrane crude product after the bleaching is placed in the fluidizer 45～65 ℃ soaked 20～50 seconds, obtain the natural cellulose membrane crude product after the plasticising.
Natural cellulose membrane crude product after preferably will bleaching is placed in the fluidizer 50 ℃ and soaked 30 seconds.
Described fluidizer is at least a among glycerine, PEG (polyoxyethylene glycol), TEG (triglycol), DEG (glycol ether), the KWO (distearyl acid amides alkyl dimethyl ammonium chloride), can be arbitrary proportion when adopting multiple mixing to use.
As preferably, adopt TEG and KWO mixture, the quality of TEG is 2～3 times of KWO quality, adopts TEG and KWO mixture plasticization effect good, product strength is higher.
As preferably, adopt PEG (polyoxyethylene glycol) can improve the slippery of product.
Plasticising is an important chemical treating process of natural cellulose membrane production moulding aftertreatment, and it is related to the quality of finished product nearly, particularly sticking crisp problem.By the fluidizer infiltration, make that the hydrogen bond quantity between cellulosic molecule is effectively controlled, thereby improved the elongation and the tensile strength of cellulose membrane that use properties is improved.By the different plasticizing process material different, can give different performance of cellulose membrane and purposes simultaneously with use.
(k) drying
Natural cellulose membrane crude product after the plasticising is carried out drying obtain the natural cellulose membrane finished product.
Drying temperature 60～100 degree, 1.5～5 minutes time, preferred 3 minutes.
Moisture content in the natural cellulose membrane finished product: 8.2～9.6%.
Cellulose membrane is wet cellulose membrane after plasticising is handled, contain a large amount of moisture, must be through drying treatment, surface and intrinsic processing evaporation of water are fallen, and reasonably shunk, make it to become level and smooth, transparent natural cellulose membrane with certain moisture.
Referring to Fig. 1,2, drying temperature has very big certain influence to product performance as can be known, and the performance of taking all factors into consideration product i.e. point of inflexion on a curve among the figure, and general dry preferred temperature is 80～100 ℃.
Relate to the many places immersion treatment in the inventive method, soaking does not have strict restriction to the soak solution consumption, guarantees good infiltration process object at least, although the soak solution consumption upper limit does not have strict restriction, can determine according to volume of equipment and throughput.
The inventive method reaction conditions gentleness, characteristics such as difference is little between the natural cellulose film web of preparation, and extension rate, tensile strength are stable, have suitable deflection and flexibility, and color and luster is preferably arranged again, and transparency is good, and wholesomeness is strong.Make the surface property of paper be improved by plasticising, particularly the paper slippery improves, and printing is improved, and the deformability of paper reduces, and moisture absorption reduces, and meets the new demand of modern printing packaging.
Description of drawings
Fig. 1 prepares the deformability of natural cellulose membrane and the graph of a relation of drying temperature for the inventive method.
Fig. 2 prepares the rate of moisture absorption of natural cellulose membrane and the graph of a relation of drying temperature for the inventive method, and upper and lower two curves are represented the relation of moisture absorption and desorption rate and drying temperature respectively among the figure.
Embodiment
It is in 18% the aqueous sodium hydroxide solution that 350 kilograms of cotton pulp dregs of rice are inserted mass percent concentration, soaks 20 minutes at 60 ℃, obtains the steeping fluid of soda cellulose.
Add squeezing auxiliary agent (Visco 44) 10 gram backs and utilize the squeezing machine in steeping fluid, squeeze pressure is 0.095Mpa, and the squeezing steeping fluid is removed unnecessary alkali lye, the fine quality percentage composition 32% of squeezing first in soda cellulose.
Soda cellulose after the squeezing is pulverized, become the tiny granular attitude 1150KG of loose bits.Soda cellulose after pulverizing at 60 ℃, is placed and carried out experienced in 2.5 hours.
It is that 10% aqueous sodium hydroxide solution soaks and alkalized in advance in 30 minutes that soda cellulose after experienced is added earlier mass percent concentration, feeds CS again
2Carry out the yellow reaction and obtained Mierocrystalline cellulose yellow acid fat in 60 minutes.The yellow temperature of reaction is 25 degree, aqueous sodium hydroxide solution and experienced after the mass ratio of soda cellulose be 1: 6; CS
2With the mass ratio of soda cellulose after experienced be 1: 10.
Mierocrystalline cellulose yellow acid fat is dissolved in form in the water of 10 times of quality and spins the paper viscose glue.
Utilize film-forming apparatus that the viscose glue that obtains is sprayed onto and obtain the natural cellulose membrane crude product in the precipitation bath, 180 microns of the spray seams of shower nozzle.
48～49 ℃ of coagulation bath temperatures.For containing the aqueous solution of sulfuric acid and sodium sulfate, wherein sulfuric acid concentration is 140g/l in the precipitation bath, and sodium sulfate concentration is 210g/l.
It is to soak in 0.2% the aqueous sodium hydroxide solution to carry out desulfurization in 30 seconds and handle that the natural cellulose membrane crude product is put into mass percent concentration, obtains the natural cellulose membrane crude product after the desulfurization, 100 ℃ of soaking temperatures.
Natural cellulose membrane crude product after the desulfurization is inserted natural cellulose membrane crude product after soak at room temperature obtained bleaching in 30 seconds in the aqueous sodium hypochlorite solution.
The mass percent concentration of aqueous sodium hypochlorite solution is 0.1%.
Natural cellulose membrane crude product after the bleaching is placed in the glycerine 50 ℃ soaked 30 seconds, obtain the natural cellulose membrane crude product after the plasticising.
Natural cellulose membrane crude product after the plasticising is carried out drying obtain the natural cellulose membrane finished product, 100 ℃ of drying temperatures, 3 minutes time.
After testing:
Moisture content in the natural cellulose membrane finished product: 8.5%;
Machine direction tensile strength: 35N/15mm;
Cross direction tensile strength: 18N/15mm;
Longitudinal tensile strain rate: 15%;
Cross direction elongation: 30%;
Average tear degree: 2N.m in length and breadth
2/ g;
Slippery: frictional coefficient static state 0.19, dynamic 0.18 (detection method: ASTMD 1894), resistance to bond 70%RH (GB);
Oxygen-permeable 2.0cc/m
2.24hrs (detection method: ASTMD 1927 testing conditions: 23 ℃ of 0%RH);
In the middle of the physical environment of humidity 6 months just can natural degradation, generate water and carbonic acid gas.
It is in 18% the aqueous sodium hydroxide solution that 350 kilograms of cotton pulp dregs of rice are inserted mass percent concentration, soaks 20 minutes at 60 ℃, obtains the steeping fluid of soda cellulose.
Add squeezing auxiliary agent (Visco 44) 10 gram backs and utilize squeezing machine squeezing steeping fluid to remove unnecessary alkali lye in steeping fluid, squeeze pressure is 0.095mpa, the fine quality percentage composition 32% of squeezing first in soda cellulose.
Soda cellulose after the squeezing is pulverized, become the tiny granular attitude 1140KG of loose bits.Soda cellulose after pulverizing at 70 ℃, is placed and carried out experienced in 2 hours.
It is that 10% aqueous sodium hydroxide solution soaks and alkalized in advance in 35 minutes that soda cellulose after experienced is added earlier mass percent concentration, feeds CS again
2Carry out the yellow reaction and obtained Mierocrystalline cellulose yellow acid fat in 90 minutes.The yellow temperature of reaction is 35 degree, CS
2With the mass ratio of soda cellulose after experienced be 1: 12.
Mierocrystalline cellulose yellow acid fat is dissolved in the water to form spins the paper viscose glue.Adopt two-part, promptly be divided into dissolving just and back dissolving.
Dissolving just and after be dissolved in room temperature and carry out, first dissolution time 30 minutes, back dissolving dissolution time 210 minutes, water consumption is 2 times of Mierocrystalline cellulose yellow acid lipid amount when just dissolving, the water yield of adding during the dissolving of back is 8 times of Mierocrystalline cellulose yellow acid lipid amount.
Utilize film-forming apparatus that the viscose glue that obtains is sprayed onto and obtain the natural cellulose membrane crude product in the precipitation bath, 220 microns of the spray seams of shower nozzle.48～49 ℃ of coagulation bath temperatures.For containing the aqueous solution of sulfuric acid and sodium sulfate, wherein sulfuric acid concentration is 140g/l in the precipitation bath, and sodium sulfate concentration is 230g/1.
It is to soak in 0.15% the aqueous sodium hydroxide solution to carry out desulfurization in 45 seconds and handle that the natural cellulose membrane crude product is put into mass percent concentration, obtains the natural cellulose membrane crude product after the desulfurization, 1050 ℃ of soaking temperatures.
Natural cellulose membrane crude product after the desulfurization is inserted natural cellulose membrane crude product after soak at room temperature obtained bleaching in 30 seconds in the aqueous sodium hypochlorite solution, and the mass percent concentration of aqueous sodium hypochlorite solution is 0.075%.
Natural cellulose membrane crude product after the bleaching is placed in TEG and the KWO mixture 50 ℃ soaked 30 seconds, obtain the natural cellulose membrane crude product after the plasticising, the quality of TEG is 2 times of KWO quality
Natural cellulose membrane crude product after the plasticising is carried out drying obtain the natural cellulose membrane finished product, 90 ℃ of drying temperatures, 3 minutes time.
After testing:
Moisture content in the natural cellulose membrane finished product: 8.2%;
Machine direction tensile strength: 40N/15mm;
Cross direction tensile strength: 20N/15mm;
Longitudinal tensile strain rate: 16%;
Cross direction elongation: 40%;
Average tear degree: 3N.m in length and breadth
2/ g;
Slippery: frictional coefficient static state 0.20, dynamic 0.18 (detection method: ASTMD 1894), resistance to bond 72%RH (GB);
Oxygen-permeable 1.8cc/m
2.24hrs (detection method: ASTMD 1927 testing conditions: 23 ℃ of 0%RH);
In the middle of the physical environment of humidity 6 months just can natural degradation, generate water and carbonic acid gas.
Adopt the technology of embodiment 1, difference is not add the squeezing auxiliary agent before the squeezing,
The finished product are after testing:
Moisture content in the natural cellulose membrane finished product: 10.5%;
Machine direction tensile strength: 33N/15mm;
Cross direction tensile strength: 17N/15mm;
Longitudinal tensile strain rate: 15%;
Cross direction elongation: 36%;
Average tear degree: 1.5N.m in length and breadth
2/ g;
Slippery: frictional coefficient static state 0.21, dynamic 0.19 (detection method: ASTMD 1894), resistance to bond 71%RH (GB);
Oxygen-permeable 1.9cc/m
2.24hrs (detection method: ASTMD 1927 testing conditions: 23 ℃ of 0%RH);
In the middle of the physical environment of humidity 6 months just can natural degradation, generate water and carbonic acid gas.
Adopt the technology of embodiment 2, adopting PEG (polyoxyethylene glycol) when difference is plasticising is fluidizer, and the slippery of the finished product has reached very big improvement, frictional coefficient static state 0.26, dynamic 0.22 (detection method: ASTMD 1894), resistance to bond 73%RH (GB)
The finished product are after testing:
Moisture content in the natural cellulose membrane finished product: 8%;
Machine direction tensile strength: 36N/15mm;
Cross direction tensile strength: 19N/15mm;
Longitudinal tensile strain rate: 14.5%;
Cross direction elongation: 30%;
Average tear degree: 2.6N.m in length and breadth
2/ g;
Oxygen-permeable 1.8cc/m
2.24hrs (detection method: ASTMD 1927 testing conditions: 23 ℃ of 0%RH);
In the middle of the physical environment of humidity 6 months just can natural degradation, generate water and carbonic acid gas.
Adopt the technology of embodiment 2, difference is that the pre-alkalization time before the yellow is 55 minutes, and the finished product oxygen-permeable improves a lot and reaches 3cc/m
2.24hrs (detection method: ASTMD 1927 testing conditions: 23 ℃ of 0%RH)
Moisture content in the natural cellulose membrane finished product: 8.3%;
Machine direction tensile strength: 39N/15mm;
Cross direction tensile strength: 20N/15mm;
Longitudinal tensile strain rate: 15.5%;
Cross direction elongation: 39%;
Average tear degree: 2.9N.m in length and breadth
2/ g;
Slippery: frictional coefficient static state 0.21, dynamic 0.19 (detection method: ASTMD 1894), resistance to bond 72%RH (GB).
Claims (9)
1. the production method of a natural cellulose membrane is characterized in that, comprises the steps:
(a) dipping
It is in 16～19% the aqueous sodium hydroxide solution that the cotton pulp dregs of rice are inserted mass percent concentration, soaks 15～30 minutes at 50～70 ℃, obtains the steeping fluid of soda cellulose;
(b) squeezing
Alkali lye unnecessary in the steeping fluid is squeezed the soda cellulose that separates after obtaining squeezing;
Add squeezing auxiliary agent fatty alcohol-polyoxyethylene ether in the squeezing forward direction steeping fluid, the mass ratio of fatty alcohol-polyoxyethylene ether and step (a) middle cotton pulp is 1: 3000～4000;
(c) pulverize
Soda cellulose after the squeezing is pulverized;
(d) experienced
Soda cellulose after pulverizing at 55～80 ℃, is placed and carried out experienced in 2～4 hours;
(e) yellow
It is that 8～12% aqueous sodium hydroxide solution soaks and alkalizes in advance that soda cellulose after experienced is added earlier mass percent concentration, feeds CS again
2Carry out the yellow reaction and obtain Mierocrystalline cellulose yellow acid fat;
(f) dissolving
Mierocrystalline cellulose yellow acid fat is dissolved in diluted alkaline or the water to form spins the paper viscose glue;
(g) film forming
The viscose glue that utilizes film-forming apparatus that step (f) is obtained is sprayed onto and obtains the natural cellulose membrane crude product in the precipitation bath;
(h) desulfurization
It is to soak in 0.1～0.5% the aqueous sodium hydroxide solution to carry out desulfurization in 20～50 seconds and handle that the natural cellulose membrane crude product is put into mass percent concentration, obtains the natural cellulose membrane crude product after the desulfurization;
(i) bleaching
Natural cellulose membrane crude product after the desulfurization is inserted natural cellulose membrane crude product after soak at room temperature obtained bleaching in 20～50 seconds in the aqueous sodium hypochlorite solution;
(j) plasticising
Natural cellulose membrane crude product after the bleaching is placed in the fluidizer 45～65 ℃ soaked 20～50 seconds, obtain the natural cellulose membrane crude product after the plasticising; Described fluidizer is at least a in glycerine, polyoxyethylene glycol, triglycol, the glycol ether;
(k) drying
Natural cellulose membrane crude product after the plasticising is carried out drying obtain the natural cellulose membrane finished product.
2. production method as claimed in claim 1 is characterized in that, in the step (e) aqueous sodium hydroxide solution with experienced after the mass ratio of soda cellulose be 1: 6～8, alkalization time is 30～40 minutes in advance.
3. production method as claimed in claim 1 is characterized in that, CS in the step (e)
2With the mass ratio of soda cellulose after experienced be 1: 8～12, in 30～100 minutes yellow reaction times, the yellow temperature of reaction is 18～35 degree.
4. production method as claimed in claim 1 is characterized in that, the diluted alkaline described in the step (f) is that mass percent concentration is 0.3～0.6% aqueous sodium hydroxide solution.
5. production method as claimed in claim 1 is characterized in that, 45～55 ℃ of the coagulation bath temperatures described in the step (g).
6. production method as claimed in claim 5 is characterized in that, the precipitation bath described in the step (g) is the aqueous solution that contains sulfuric acid and sodium sulfate, and wherein sulfuric acid concentration is 140～143g/l; Sodium sulfate concentration is 210～230g/l.
7. production method as claimed in claim 1 is characterized in that, in the step (h), and 90 ℃～100 ℃ of the temperature that desulfurization is handled.
8. production method as claimed in claim 1 is characterized in that, in the step (i), the mass percent concentration of aqueous sodium hypochlorite solution is 0.05～0.2%.
9. production method as claimed in claim 1 is characterized in that, in the step (k), and drying temperature 80-100 degree, 1.5～5 minutes time.
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| CN1088225A (en) * | 1992-12-18 | 1994-06-22 | 中国国际科技促进会 | Vegetable fibre film product and technology thereof |
| CN101153207A (en) * | 2007-09-17 | 2008-04-02 | 潍坊恒联玻璃纸有限公司 | Method for manufacturing film special for rubber belt |
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