CN101649059A - Preparing method of antibacterial cellulose membrane - Google Patents
Preparing method of antibacterial cellulose membrane Download PDFInfo
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- CN101649059A CN101649059A CN200910016777A CN200910016777A CN101649059A CN 101649059 A CN101649059 A CN 101649059A CN 200910016777 A CN200910016777 A CN 200910016777A CN 200910016777 A CN200910016777 A CN 200910016777A CN 101649059 A CN101649059 A CN 101649059A
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Abstract
The invention relates to a cellulose membrane and a preparing method thereof, in particular to an antibacterial cellulose membrane and a preparing method thereof. The method comprises the following steps: selecting raw material, preparing viscose glue, injecting antibacterial agent, preparing films, desulphurizing, blenching, plasticizing, drying and humidifying; then, a finished product is obtained; the finished product adopts cotton pulp and wood pulp as raw materials and has the characteristics of energy saving, capability of degrading, no toxin, anti-static electricity, no pollution to objects and antibacterial property in practical application.
Description
Technical field
The present invention relates to a kind of preparation method of cellulose membrane, relate in particular to a kind of preparation method of antibacterial cellulose membrane.
Background technology
Along with the concern of people to healthy and health care of body, require to reduce chemical additive in the food-processing as far as possible, but current extensive development along with processing, transportation, storage integrated technique, the circulation of commodity expands to all over the world, therefore the preservation of food not only needs to keep certain quality guarantee period, but also needs the fresh and easy storage of nutrition.For using film packaging food, if in film, add antiseptic-germicide, can suppress the microorganism growth of food surfaces effectively, and not need the deepfreeze technology, both can save the energy, also can reduce the cost of goods sold of food.
At present, the germ resistance film mainly is antiseptic-germicide to be sneaked into polymkeric substance such as polyethylene or polyvinylidene dichloride to make on the market.Owing to adopt the petrochemical complex material, be used for the food product pack industry and directly affect food quality, affect HUMAN HEALTH simultaneously, also has non-degradable simultaneously, environment is polluted, the cost height, the shortcoming of harm person health can't adapt to the demand of current market to health, environmental protection, ecological film.
Summary of the invention
Technical problem to be solved by this invention has provided a kind of preparation method of antibacterial cellulose membrane, it is raw material that present method adopts cotton pulp, wood pulp natural cellulose, produce a kind of antibacterial cellulose membrane, have save energy, degradable, nontoxic, antistatic, the characteristics of not polluting content, germ resistance.
In order to reach above purpose, the technical solution adopted in the present invention is:
A kind of preparation method of antibacterial cellulose membrane may further comprise the steps: raw material makes finished product after choosing operation, viscose glue preparation section, antiseptic-germicide injection process, film preparation operation, desulfurization process, bleaching process, plasticizing operation, dry damping operation.
Described raw material is chosen operation: choosing weight ratio is 30%～50% cotton pulp and 70%～50% wood pulp.
Described viscose glue preparation section:
A, with the cotton pulp wood pulp chosen after alkalization, squeezing, aging, yellow, make cellulose xanthate;
B, with the cellulose xanthate after the yellow, adding concentration is the NaOH solution of 13～20g/L, dissolves, the volume of every batch of cellulose xanthate is 11～14m
3, NaOH solution add-on 95～135kg/ ton paper, temperature is controlled at 16～19 ℃, makes viscose glue after the dissolving, the composition of its viscose glue: α-cell 8.3～8.7%, NaOH5.0～5.6%, viscosity 50～60sec, ammonium value 5.6～7.0ml, all the other are water;
C, the viscose glue after will dissolving carry out maturation, and temperature is controlled between 36～40 ℃, and the time is controlled at 7.5～9.5h, the index of viscose glue: α-cell8.4～8.8% after the maturation, NaOH5.15～5.6%, viscosity 48～58sec, ammonium value 5.3～6.5ml;
D, with the viscose glue after the maturation, after filtering, enter the deaeration tower, temperature of cooling water is controlled between 16～19 ℃, deaeration tower temperature in is controlled at 36～40 ℃, 27～33 ℃ of deaeration tower temperature out controls, the time is controlled at 1.5～2.5min, makes the spinning viscose glue after the deaeration, spinning viscose glue index: α-cell8.85～9.15%, NaOH5.2～5.5%, viscosity 38～48sec, ammonium value 5.0～5.6ml.
Described antiseptic-germicide injection process: silver zeolite antiseptic-germicide and de-salted water is even by 0.9～1.2: 9.1～8.8 mixed, change in the hold-up vessel after mixing, open pressurized air, open volume pump, adjusting the volume pump flow scale is 500～1000ml/min, be expelled in the viscose glue, mix.
Described film preparation operation: the viscose glue that will inject behind the antiseptic-germicide is delivered in the coagulating tank, and adding concentration is the sulphuric acid soln of 138～148g/L, and the acid bath temperature is controlled between 49～55 ℃, reacts 4～10 seconds, makes film.
Described desulfurization process: with the film of making, change in the desulfurizer, adding concentration is the sodium hydroxide solution of 1.5～3.0g/L, add-on 1.8～3.5kg/ ton paper, desulfurization temperature is 85～90 ℃, desulfurization is after 6～12 seconds, change in the washing bath, washed 10～20 seconds.
Described bleaching process: the film after the desulfurization is changed in the bleaching tank, and adding concentration is 0.6～2.0g/L clorox, add-on 2.0～4.0kg/ ton paper, and 4-10 is after second in bleaching, changes in the washing bath, washes 40～60 seconds.
Described plasticizing operation: the film after will bleaching, washing, change in the plasticizing pond, add the glycerine that concentration is 20～40g/L respectively, add-on is 60～90kg/ ton paper, and concentration is the sorbyl alcohol of 15～30g/L, and add-on is 40～60kg/ ton paper, temperature is controlled at 50～60 ℃, pH value is controlled at 9～12, and fusion time 5～10 seconds is promptly finished plasticizing.
Described dry damping operation: the film after will plastifying changes drying room over to, carry out heat-wind circulate drying, temperature is 129～131 ℃, after dry 80～100 seconds, change between damping, temperature is controlled at 40～48 ℃, relative humidity is controlled at 60～80%RH, damping 5～10 seconds, the moisture controlled of film makes finished product between 6～10%.
Among the present invention, the silver zeolite antiseptic-germicide of adding selects for use the prosperous health inorganic materials company limited that reaches in Xiamen to produce XDK-101 model silver zeolite antiseptic-germicide.
Among the present invention, the glycerine of adding selects for use Shandong Ge Run new forms of energy company limited to produce, and purity is 98% glycerine.
Among the present invention, the sorbyl alcohol of adding selects for use the prosperous China in Wuhan development in science and technology far away company limited to produce M286366 model sorbyl alcohol.
It is raw material that the present invention adopts with cotton pulp, wood pulp natural cellulose, the preparation antibacterial cellulose membrane has reduced the dependence to petrochemicals, degradable, can effectively avoid environmental pollution, nontoxic, the anlistatig performance that has common plastic film simultaneously and do not had.
Utilize the present invention to prepare antibacterial cellulose membrane and pack, can play and regulate moisture in the packing material, and suppress the effect of microbial bacterial growth and breeding, can not pollute content, security is high, and can reach environmental protection to connection with wrapping of piece, performance such as attractive in appearance.
Table one: antibacterial cellulose membrane and traditional antibiotic plastic film contrast table that the present invention produces:
| Project relatively | Antibacterial cellulose membrane of the present invention | Tradition antibiotic plastic film |
| Raw material | Cotton pulp, wood pulp | The petrochemical complex material |
| Degradation property | Degraded fully | Non-degradable or part degraded |
| Security | Safety | Contain toxicant |
Shown in last table: antibacterial cellulose membrane of the present invention, adopting regeneration, eco-friendly power source is raw material, compares with traditional antibiotic plastic film, has not to be detrimental to health, can also save energy, degradable, the advantage of protection environment.
The antibacterial cellulose membrane that preparation method of the present invention produces, technical indicator is as follows after testing:
| Quantitatively | ??a±0.5g/m 2 | Moisture | ??6.0-10.0％ |
| Tensile strength | ??≥20N/15mm | Elongation (indulging) | ??≥10％ |
| The thickness banner is poor | ??≤1.5μm | Bacteriostasis rate | ??≥99％ |
Embodiment
The invention will be further described below in conjunction with embodiment, but embodiments of the present invention are not limited thereto.
Embodiment 1
(1) raw material is chosen operation: choose weight ratio and be 30% cotton pulp and 70% wood pulp, and standby;
(2) viscose glue preparation section:
A, with the cotton pulp wood pulp chosen after alkalization, squeezing, aging, yellow, make cellulose xanthate;
B, with the cellulose xanthate after the yellow, adding concentration is the NaOH solution of 13g/L, dissolves, the volume of every batch of cellulose xanthate is 12m
3, NaOH solution add-on 105kg/ ton paper, temperature is controlled at 16 ℃, makes viscose glue after the dissolving, the composition of its viscose glue: α-cell 8.3%, NaOH5.0%, viscosity 50sec, ammonium value 5.6ml, all the other are water;
C, the viscose glue after will dissolving carry out maturation, and temperature is controlled between 36 ℃, and the time is controlled at 7.5h, the index of viscose glue: α-cell8.40% after the maturation, NaOH5.15%, viscosity 48sec, ammonium value 5.3ml;
D, with the viscose glue after the maturation, after filtering, enter the deaeration tower, temperature of cooling water is controlled between 16 ℃, deaeration tower temperature in is controlled at 36 ℃, 27 ℃ of deaeration tower temperature out controls, the time is controlled at 1.5min, makes the spinning viscose glue after the deaeration, spinning viscose glue index: α-cell8.85%, NaOH5.2%, viscosity 38sec, ammonium value 5.0ml;
(3) antiseptic-germicide injection process: with silver zeolite antiseptic-germicide and de-salted water, be that 0.9: 9.1 mixed is even by weight ratio, change in the hold-up vessel after mixing, open pressurized air, open volume pump, adjusting the volume pump flow scale is 500ml/min, be expelled in the viscose glue, mix;
(4) film preparation operation: the viscose glue that will inject behind the antiseptic-germicide is delivered in the coagulating tank, and adding concentration is the sulphuric acid soln of 138g/L, and the acid bath temperature is controlled at 49 ℃, reacts 4 seconds, makes film;
(5) desulfurization process: with the film of making, change in the desulfurizer, adding concentration is the sodium hydroxide solution of 1.5g/L, and add-on 1.8kg/ ton paper, desulfurization temperature are 85 ℃, and desulfurization changed in the washing bath after 6 seconds, washed 10 seconds;
(6) bleaching process: the film after the desulfurization is changed in the bleaching tank, and adding concentration is the 0.6g/L clorox, and add-on 2.0kg/ ton paper was bleached after 4 seconds, changed in the washing bath, washed 40 seconds;
(7) plasticizing operation: the film after will bleaching, washing, change in the plasticizing pond, add the glycerine that concentration is 20g/L respectively, add-on is a 60kg/ ton paper, concentration is the sorbyl alcohol of 15g/L, and add-on is a 40kg/ ton paper, and temperature is controlled at 50 ℃, pH value is controlled at 9, and fusion time 5 seconds is finished plasticizing;
(8) dry damping operation: the film after will plastifying changes drying room over to, carries out heat-wind circulate drying, and temperature is 131 ℃, after dry 80 seconds, changes between damping, and temperature is controlled at 40 ℃, and relative humidity is controlled at 60%RH, and damping 5 seconds makes finished product.
The antibacterial cellulose membrane of present embodiment preparation, technical indicator is as follows after testing:
| Quantitatively | ??30.2g/m 2 | Moisture | ??8.2％ |
| Tensile strength | ??29.68N/15mm | Elongation (indulging) | ??15.62％ |
| The thickness banner is poor | ??1.2μm | Bacteriostasis rate | ??99.86％ |
The antibacterial cellulose membrane of present embodiment preparation, degradable can effectively be avoided environmental pollution, has nontoxic, anlistatig performance simultaneously.
Embodiment 2
(1) raw material is chosen operation: choose weight ratio and be 35% cotton pulp and 65% wood pulp, and standby;
(2) viscose glue preparation section:
A, with the cotton pulp wood pulp chosen after alkalization, squeezing, aging, yellow, make cellulose xanthate;
B, with the cellulose xanthate after the yellow, adding concentration is the NaOH solution of 14g/L, dissolves, the volume of every batch of cellulose xanthate is 12m
3, NaOH solution add-on 95kg/ ton paper, temperature is controlled at 16 ℃, makes viscose glue after the dissolving, the composition of its viscose glue: α-cell 8.38%, NaOH5.1%, viscosity 52sec, ammonium value 5.8ml, all the other are water;
C, the viscose glue after will dissolving advance maturation, and temperature is controlled between 37 ℃, and the time is controlled at 7.7h, the index of viscose glue: α-cell8.42% after the maturation, NaOH5.3%, viscosity 50sec, ammonium value 5.6ml;
D, with the viscose glue after the maturation, after filtering, enter the deaeration tower, temperature of cooling water is controlled between 17 ℃, deaeration tower temperature in is controlled at 37 ℃, 29 ℃ of deaeration tower temperature out controls, the time is controlled at 1.7min, makes the spinning viscose glue after the deaeration, spinning viscose glue index: α-cell8.90%, NaOH5.3%, viscosity 40sec, ammonium value 5.2ml;
(3) antiseptic-germicide injection process: with silver zeolite antiseptic-germicide and de-salted water, be that 0.95: 9.05 mixed is even by weight ratio, change in the hold-up vessel after mixing, open pressurized air, open volume pump, adjusting the volume pump flow scale is 550ml/min, be expelled in the viscose glue, mix;
(4) film preparation operation: the viscose glue that will inject behind the antiseptic-germicide is delivered in the coagulating tank, and adding concentration is the sulphuric acid soln of 140g/L, and the acid bath temperature is controlled at 50 ℃, reacts 5 seconds, makes film;
(5) desulfurization process: with the film of making, change in the desulfurizer, adding concentration is the sodium hydroxide solution of 1.75g/L, and add-on 2.1kg/ ton paper, desulfurization temperature are 86 ℃, and desulfurization changed in the washing bath after 7 seconds, washed 12 seconds;
(6) bleaching process: the film after the desulfurization is changed in the bleaching tank, and adding concentration is the 0.8g/L clorox, and add-on 2.3kg/ ton paper was bleached after 5 seconds, changed in the washing bath, washed 43 seconds;
(7) plasticizing operation: the film after will bleaching, washing, change in the plasticizing pond, add the glycerine that concentration is 27g/L respectively, add-on is a 68kg/ ton paper, and concentration is the sorbyl alcohol of 20g/L, and add-on is a 45kg/ ton paper, temperature is controlled at 52 ℃, pH value is controlled at 9.5, and fusion time 6 seconds is finished plasticizing;
(8) dry damping operation: the film after will plastifying changes drying room over to, carries out heat-wind circulate drying, and temperature is 130 ℃, after dry 83 seconds, changes between damping, and temperature is controlled at 42 ℃, and relative humidity is controlled at 63%RH, and damping 6 seconds makes finished product.
The antibacterial cellulose membrane of present embodiment preparation, technical indicator is as follows after testing:
| Quantitatively | ??28.6g/m 2 | Moisture | ??8.0％ |
| Tensile strength | ??36.68N/15mm | Elongation (indulging) | ??18.02％ |
| The thickness banner is poor | ??1.2μm | Bacteriostasis rate | ??99.94％ |
The antibacterial cellulose membrane of present embodiment preparation has the advantages that not pollute content, germ resistance.
Embodiment 3
(1) raw material is chosen operation: choose weight ratio and be 37% cotton pulp and 63% wood pulp, and standby;
(2) viscose glue preparation section:
A, with the cotton pulp wood pulp chosen after alkalization, squeezing, aging, yellow, make cellulose xanthate;
B, with the cellulose xanthate after the yellow, adding concentration is the NaOH solution of 15g/L, dissolves, the volume of every batch of cellulose xanthate is 11m
3, NaOH solution add-on 100kg/ ton paper, temperature is controlled at 17 ℃, makes viscose glue after the dissolving, the composition of its viscose glue: α-cell 8.44%, NaOH5.2%, viscosity 53sec, ammonium value 6.1ml, all the other are water;
C, the viscose glue after will dissolving carry out maturation, and temperature is controlled between 37 ℃, and the time is controlled at 8.2h, the index of viscose glue: α-cell8.53% after the maturation, NaOH5.21%, viscosity 51sec, ammonium value 5.7ml;
D, with the viscose glue after the maturation, after filtering, enter the deaeration tower, temperature of cooling water is controlled between 18 ℃, deaeration tower temperature in is controlled at 37 ℃, 28 ℃ of deaeration tower temperature out controls, the time is controlled at 1.9min, makes the spinning viscose glue after the deaeration, spinning viscose glue index: α-cell8.95%, NaOH5.26%, viscosity 42sec, ammonium value 5.1ml;
(3) antiseptic-germicide injection process: with silver zeolite antiseptic-germicide and de-salted water, be that 1.0: 9.0 mixed is even by weight ratio, change in the hold-up vessel after mixing, open pressurized air, open volume pump, adjusting the volume pump flow scale is 600ml/min, be expelled in the viscose glue, mix;
(4) film preparation operation: the viscose glue that will inject behind the antiseptic-germicide is delivered in the coagulating tank, and adding concentration is the sulphuric acid soln of 142g/L, and the acid bath temperature is controlled at 51 ℃, reacts 6 seconds, makes film;
(5) desulfurization process: with the film of making, change in the desulfurizer, adding concentration is the sodium hydroxide solution of 2.0g/L, and add-on 2.4kg/ ton paper, desulfurization temperature are 87 ℃, and desulfurization changed in the washing bath after 8 seconds, washed 13 seconds;
(6) bleaching process: the film after the desulfurization is changed in the bleaching tank, and adding concentration is the 1.1g/L clorox, and add-on 2.7kg/ ton paper was bleached after 6 seconds, changed in the washing bath, washed 47 seconds;
(7) plasticizing operation: the film after will bleaching, washing, change in the plasticizing pond, add the glycerine that concentration is 33g/L respectively, add-on is a 78kg/ ton paper, concentration is the sorbyl alcohol of 25g/L, and add-on is a 51kg/ ton paper, and temperature is controlled at 54 ℃, pH value is controlled at 10, and fusion time 7 seconds is finished plasticizing;
(8) dry damping operation: the film after will plastifying changes drying room over to, carries out heat-wind circulate drying, and temperature is 129 ℃, after dry 87 seconds, changes between damping, and temperature is controlled at 43 ℃, and relative humidity is controlled at 67%RH, and damping 7 seconds makes finished product.
The antibacterial cellulose membrane of present embodiment preparation, technical indicator is as follows after testing:
| Quantitatively | ??30.8g/m 2 | Moisture | ??7.8％ |
| Tensile strength | ??35.56N/15mm | Elongation (indulging) | ??16.88％ |
| The thickness banner is poor | ??1.3μm | Bacteriostasis rate | ??99.88％ |
The antibacterial cellulose membrane of present embodiment preparation, degradable, nontoxic, characteristics that germ resistance is strong are mainly used in the food product pack industry.
Embodiment 4
(1) raw material is chosen operation: choose weight ratio and be 40% cotton pulp and 60% wood pulp, and standby;
(2) viscose glue preparation section:
A, with the cotton pulp wood pulp chosen after alkalization, squeezing, aging, yellow, make cellulose xanthate;
B, with the cellulose xanthate after the yellow, adding concentration is the NaOH solution of 16.5g/L, dissolves, the volume of every batch of cellulose xanthate is 13m
3, NaOH solution add-on 115kg/ ton paper, temperature is controlled at 18 ℃, makes viscose glue after the dissolving, the composition of its viscose glue: α-cell 8.5%, NaOH5.25%, viscosity 55sec, ammonium value 6.3ml, all the other are water;
C, the viscose glue after will dissolving carry out maturation, and temperature is controlled between 38 ℃, and the time is controlled at 8.5h, the index of viscose glue: α-cell8.6% after the maturation, NaOH5.35%, viscosity 53sec, ammonium value 5.9ml;
D, with the viscose glue after the maturation, after filtering, enter the deaeration tower, temperature of cooling water is controlled between 17 ℃, deaeration tower temperature in is controlled at 38 ℃, 30 ℃ of deaeration tower temperature out controls, the time is controlled at 2.0min, makes the spinning viscose glue after the deaeration, spinning viscose glue index: α-cell9.0%, NaOH5.38%, viscosity 43sec, ammonium value 5.3ml;
(3) antiseptic-germicide injection process: with silver zeolite antiseptic-germicide and de-salted water, be that 1.05: 8.95 mixed is even by weight ratio, change in the hold-up vessel after mixing, open pressurized air, open volume pump, adjusting the volume pump flow scale is 750ml/min, be expelled in the viscose glue, mix;
(4) film preparation operation: the viscose glue that will inject behind the antiseptic-germicide is delivered in the coagulating tank, and adding concentration is the sulphuric acid soln of 143g/L, and the acid bath temperature is controlled at 52 ℃, reacts 7 seconds, makes film;
(5) desulfurization process: with the film of making, change in the desulfurizer, adding concentration is the sodium hydroxide solution of 2.25g/L, and add-on 2.65kg/ ton paper, desulfurization temperature are 87.5 ℃, and desulfurization changed in the washing bath after 9 seconds, washed 15 seconds;
(6) bleaching process: the film after the desulfurization is changed in the bleaching tank, and adding concentration is the 1.3g/L clorox, and add-on 3.0kg/ ton paper was bleached after 7 seconds, changed in the washing bath, washed 50 seconds;
(7) plasticizing operation: the film after will bleaching, washing, change in the plasticizing pond, add the glycerine that concentration is 38g/L respectively, add-on is a 86kg/ ton paper, and concentration is the sorbyl alcohol of 29g/L, and add-on is a 58kg/ ton paper, temperature is controlled at 55 ℃, pH value is controlled at 10.5, and fusion time 7.5 seconds is finished plasticizing;
(8) dry damping operation: the film after will plastifying changes drying room over to, carries out heat-wind circulate drying, and temperature is 130 ℃, after dry 90 seconds, changes between damping, and temperature is controlled at 44 ℃, and relative humidity is controlled at 70%RH, and damping 7.5 seconds makes finished product.
The antibacterial cellulose membrane of present embodiment preparation, technical indicator is as follows after testing:
| Quantitatively | ??32.6g/m 2 | Moisture | ??7.6％ |
| Tensile strength | ??36.98N/15mm | Elongation (indulging) | ??16.98％ |
| The thickness banner is poor | ??1.3μm | Bacteriostasis rate | ??99.98％ |
The antibacterial cellulose membrane of present embodiment preparation is mainly used in the food product pack industry, packing material is played the effect that suppresses the microbial bacterial growth and breeding.
Embodiment 5
(1) raw material is chosen operation: choose weight ratio and be 41% cotton pulp and 59% wood pulp, and standby;
(2) viscose glue preparation section:
A, with the cotton pulp wood pulp chosen after alkalization, squeezing, aging, yellow, make cellulose xanthate;
B, with the cellulose xanthate after the yellow, adding concentration is the NaOH solution of 17g/L, dissolves, the volume of every batch of cellulose xanthate is 14m
3, NaOH solution add-on 130kg/ ton paper, temperature is controlled at 17 ℃, makes viscose glue after the dissolving, the composition of its viscose glue: α-cell 8.54%, NaOH5.3%, viscosity 57sec, ammonium value 6.5ml, all the other are water;
C, the viscose glue after will dissolving carry out maturation, and temperature is controlled between 38 ℃, and the time is controlled at 8.8h, the index of viscose glue: α-cell8.62% after the maturation, NaOH5.4%, viscosity 55sec, ammonium value 6.1ml;
D, with the viscose glue after the maturation, after filtering, enter the deaeration tower, temperature of cooling water is controlled between 16 ℃, deaeration tower temperature in is controlled at 38 ℃, 31 ℃ of deaeration tower temperature out controls, the time is controlled at 2.1min, makes the spinning viscose glue after the deaeration, spinning viscose glue index: α-cell9.07%, NaOH5.5%, viscosity 44sec, ammonium value 5.4ml;
(3) antiseptic-germicide injection process: with silver zeolite antiseptic-germicide and de-salted water, be that 1.08: 8.92 mixed is even by weight ratio, change in the hold-up vessel after mixing, open pressurized air, open volume pump, adjusting the volume pump flow scale is 780ml/min, be expelled in the viscose glue, mix;
(4) film preparation operation: the viscose glue that will inject behind the antiseptic-germicide is delivered in the coagulating tank, and adding concentration is the sulphuric acid soln of 144g/L, and the acid bath temperature is controlled at 52 ℃, reacts 8 seconds, makes film;
(5) desulfurization process: with the film of making, change in the desulfurizer, adding concentration is the sodium hydroxide solution of 2.4g/L, and add-on 2.8kg/ ton paper, desulfurization temperature are 88 ℃, and desulfurization changed in the washing bath after 9 seconds, washed 16 seconds;
(6) bleaching process: the film after the desulfurization is changed in the bleaching tank, and adding concentration is the 1.4g/L clorox, and add-on 3.2kg/ ton paper was bleached after 7 seconds, changed in the washing bath, washed 52 seconds;
(7) plasticizing operation: the film after will bleaching, washing, change in the plasticizing pond, add the glycerine that concentration is 30g/L respectively, add-on is a 75kg/ ton paper, and concentration is the sorbyl alcohol of 23g/L, and add-on is a 50kg/ ton paper, temperature is controlled at 56 ℃, pH value is controlled at 10.8, and fusion time 8 seconds is finished plasticizing;
(8) dry damping operation: the film after will plastifying changes drying room over to, carries out heat-wind circulate drying, and temperature is 130 ℃, after dry 92 seconds, changes between damping, and temperature is controlled at 45 ℃, and relative humidity is controlled at 72%RH, and damping 8 seconds makes finished product.
The antibacterial cellulose membrane of present embodiment preparation, technical indicator is as follows after testing:
| Quantitatively | ??40.1g/m 2 | Moisture | ??7.6％ |
| Tensile strength | ??41.86N/15mm | Elongation (indulging) | ??19.78％ |
| The thickness banner is poor | ??1.4μm | Bacteriostasis rate | ??99.91％ |
The antibacterial cellulose membrane of present embodiment preparation is mainly used in the food product pack industry, and germ resistance is strong, can not pollute content, and can reach environmental protection to connection with wrapping of piece, performance such as attractive in appearance.
Embodiment 6
(1) raw material is chosen operation: choose weight ratio and be 43% cotton pulp and 57% wood pulp, and standby;
(2) viscose glue preparation section: a, with the cotton pulp wood pulp chosen after alkalization, squeezing, aging, yellow, make cellulose xanthate;
B, with the cellulose xanthate after the yellow, adding concentration is the NaOH solution of 18g/L, dissolves, the volume of every batch of cellulose xanthate is 13.5m
3, NaOH solution add-on 127kg/ ton paper, temperature is controlled at 18 ℃, makes viscose glue after the dissolving, the composition of its viscose glue: α-cell 8.62%, NaOH5.4%, viscosity 58sec, ammonium value 6.7ml, all the other are water;
C, the viscose glue after will dissolving carry out maturation, and temperature is controlled between 39 ℃, and the time is controlled at 9.1h, the index of viscose glue: α-cell8.75% after the maturation, NaOH5.37%, viscosity 52sec, ammonium value 6.2ml;
D, with the viscose glue after the maturation, after filtering, enter the deaeration tower, temperature of cooling water is controlled between 18 ℃, deaeration tower temperature in is controlled at 39 ℃, 31 ℃ of deaeration tower temperature out controls, the time is controlled at 2.3min, makes the spinning viscose glue after the deaeration, spinning viscose glue index: α-cell9.12%, NaOH5.42%, viscosity 47sec, ammonium value 5.4ml;
(3) antiseptic-germicide injection process: with silver zeolite antiseptic-germicide and de-salted water, be that 1.1: 8.9 mixed is even by weight ratio, change in the hold-up vessel after mixing, open pressurized air, open volume pump, adjusting the volume pump flow scale is 800ml/min, be expelled in the viscose glue, mix;
(4) film preparation operation: the viscose glue that will inject behind the antiseptic-germicide is delivered in the coagulating tank, and adding concentration is the sulphuric acid soln of 146g/L, and the acid bath temperature is controlled at 53 ℃, reacts 8 seconds, makes film;
(5) desulfurization process: with the film of making, change in the desulfurizer, adding concentration is the sodium hydroxide solution of 2.6g/L, and add-on 3.1kg/ ton paper, desulfurization temperature are 88 ℃, and desulfurization changed in the washing bath after 10 seconds, washed 17 seconds;
(6) bleaching process: the film after the desulfurization is changed in the bleaching tank, and adding concentration is the 1.6/L clorox, and add-on 3.5kg/ ton paper was bleached after 8 seconds, changed in the washing bath, washed 55 seconds;
(7) plasticizing operation: the film after will bleaching, washing, change in the plasticizing pond, add the glycerine that concentration is 35g/L respectively, add-on is a 82kg/ ton paper, and concentration is the sorbyl alcohol of 26g/L, and add-on is a 53kg/ ton paper, temperature is controlled at 58 ℃, pH value is controlled at 11, and fusion time 8.5 seconds is finished plasticizing;
(8) dry damping operation: the film after will plastifying changes drying room over to, carries out heat-wind circulate drying, and temperature is 130 ℃, after dry 95 seconds, changes between damping, and temperature is controlled at 46 ℃, and relative humidity is controlled at 75%RH, and damping 8.5 seconds makes finished product.
The antibacterial cellulose membrane of present embodiment preparation, technical indicator is as follows after testing:
| Quantitatively | ??22.5g/m 2 | Moisture | ??7.2％ |
| Tensile strength | ??28.62N/15mm | Elongation (indulging) | ??16.16％ |
| The thickness banner is poor | ??1.5μm | Bacteriostasis rate | ??99.99％ |
The antibacterial cellulose membrane of present embodiment preparation, degradable can effectively be avoided environmental pollution, has the performance antistatic, that germ resistance is strong.
Embodiment 7
(1) raw material is chosen operation: choose weight ratio and be 45% cotton pulp and 55% wood pulp, and standby;
(2) viscose glue preparation section: a, with the cotton pulp wood pulp chosen after alkalization, squeezing, aging, yellow, make cellulose xanthate;
B, with the cellulose xanthate after the yellow, adding concentration is the NaOH solution of 20g/L, dissolves, the volume of every batch of cellulose xanthate is 12.5m
3, NaOH solution add-on 135kg/ ton paper, temperature is controlled at 19 ℃, makes viscose glue after the dissolving, the composition of its viscose glue: α-cell 8.72%, NaOH5.6%, viscosity 60sec, ammonium value 7.0ml, all the other are water;
C, the viscose glue after will dissolving carry out maturation, and temperature is controlled between 40 ℃, and the time is controlled at 9.5h, the index of viscose glue: α-cell8.84% after the maturation, NaOH5.61%, viscosity 58sec, ammonium value 6.5ml;
D, with the viscose glue after the maturation, after filtering, enter the deaeration tower, temperature of cooling water is controlled between 19 ℃, deaeration tower temperature in is controlled at 40 ℃, 33 ℃ of deaeration tower temperature out controls, the time is controlled at 2.5min, makes the spinning viscose glue after the deaeration, spinning viscose glue index: α-cell9.15%, NaOH5.59%, viscosity 48sec, ammonium value 5.6ml;
(3) antiseptic-germicide injection process: with silver zeolite antiseptic-germicide and de-salted water, be that 1.15: 8.85 mixed is even by weight ratio, change in the hold-up vessel after mixing, open pressurized air, open volume pump, adjusting the volume pump flow scale is 850ml/min, be expelled in the viscose glue, mix;
(4) film preparation operation: the viscose glue that will inject behind the antiseptic-germicide is delivered in the coagulating tank, and adding concentration is the sulphuric acid soln of 147g/L, and the acid bath temperature is controlled between 54 ℃, reacts 9 seconds, makes film;
(5) desulfurization process: with the film of making, change in the desulfurizer, adding concentration is the sodium hydroxide solution of 2.8g/L, and add-on 3.3kg/ ton paper, desulfurization temperature are 89 ℃, and desulfurization changed in the washing bath after 11 seconds, washed 19 seconds;
(6) bleaching process: the film after the desulfurization is changed in the bleaching tank, and adding concentration is the 1.8g/L clorox, and add-on 3.8kg/ ton paper was bleached after 9 seconds, changed in the washing bath, washed 58 seconds;
(7) plasticizing operation: the film after will bleaching, washing, change in the plasticizing pond, add the glycerine that concentration is 39g/L respectively, add-on is a 88kg/ ton paper, and concentration is the sorbyl alcohol of 28g/L, and add-on is a 57kg/ ton paper, temperature is controlled at 59 ℃, pH value is controlled at 11.5, and fusion time 9 seconds is finished plasticizing;
(8) dry damping operation: the film after will plastifying changes drying room over to, carries out heat-wind circulate drying, and temperature is 130 ℃, after dry 98 seconds, changes between damping, and temperature is controlled at 47 ℃, and relative humidity is controlled at 78%RH, and damping 9 seconds makes finished product.
The antibacterial cellulose membrane of present embodiment preparation, technical indicator is as follows after testing:
| Quantitatively | ??25.0g/m 2 | Moisture | ??7.0％ |
| Tensile strength | ??29.88N/15mm | Elongation (indulging) | ??16.06％ |
| The thickness banner is poor | ??1.3μm | Bacteriostasis rate | ??99.66％ |
The antibacterial cellulose membrane of present embodiment preparation when carrying out food product pack, can play and regulate moisture in the packing material, and suppress the effect of microbial bacterial growth and breeding, can not pollute content.
Embodiment 8
(1) raw material is chosen operation: choose weight ratio and be 50% cotton pulp and 50% wood pulp, and standby;
(2) viscose glue preparation section: a, with the cotton pulp wood pulp chosen after alkalization, squeezing, aging, yellow, make cellulose xanthate;
B, with the cellulose xanthate after the yellow, adding concentration is the NaOH solution of 19.5g/L, dissolves, the volume of every batch of cellulose xanthate is 11.6m
3, NaOH solution add-on 110kg/ ton paper, temperature is controlled at 19 ℃, makes viscose glue after the dissolving, the composition of its viscose glue: α-cell 8.60%, NaOH5.5%, viscosity 59sec, ammonium value 6.4ml, all the other are water;
C, the viscose glue after will dissolving carry out maturation, and temperature is controlled between 39 ℃, and the time is controlled at 9.3h, the index of viscose glue: α-cell8.71% after the maturation, NaOH5.45%, viscosity 57sec, ammonium value 6.0ml;
D, with the viscose glue after the maturation, after filtering, enter the deaeration tower, temperature of cooling water is controlled between 19 ℃, deaeration tower temperature in is controlled at 39 ℃, 32 ℃ of deaeration tower temperature out controls, the time is controlled at 2.2min, makes the spinning viscose glue after the deaeration, spinning viscose glue index: α-cell9.13%, NaOH5.49%, viscosity 46sec, ammonium value 5.5ml;
(3) antiseptic-germicide injection process: with silver zeolite antiseptic-germicide and de-salted water, be that 1.2: 8.8 mixed is even by weight ratio, change in the hold-up vessel after mixing, open pressurized air, open volume pump, adjusting the volume pump flow scale is 1000ml/min, be expelled in the viscose glue, mix;
(4) film preparation operation: the viscose glue that will inject behind the antiseptic-germicide is delivered in the coagulating tank, and adding concentration is the sulphuric acid soln of 148g/L, and the acid bath temperature is controlled at 55 ℃, reacts 10 seconds, makes film;
(5) desulfurization process: with the film of making, change in the desulfurizer, adding concentration is the sodium hydroxide solution of 3.0g/L, and add-on 3.5kg/ ton paper, desulfurization temperature are 90 ℃, and desulfurization changed in the washing bath after 12 seconds, washed 20 seconds;
(6) bleaching process: the film after the desulfurization is changed in the bleaching tank, and adding concentration is the 2.0g/L clorox, and add-on 4.0kg/ ton paper was bleached after 10 seconds, changed in the washing bath, washed 60 seconds;
(7) plasticizing operation: the film after will bleaching, washing, change in the plasticizing pond, add the glycerine that concentration is 40g/L respectively, add-on is a 90kg/ ton paper, and concentration is the sorbyl alcohol of 30g/L, and add-on is a 60kg/ ton paper, temperature is controlled at 60 ℃, pH value is controlled at 12, and fusion time 10 seconds is finished plasticizing;
(8) dry damping operation: the film after will plastifying changes drying room over to, carries out heat-wind circulate drying, and temperature is 130 ℃, after dry 100 seconds, changes between damping, and temperature is controlled at 48 ℃, and relative humidity is controlled at 80%RH, and damping 10 seconds makes finished product.
The antibacterial cellulose membrane of present embodiment preparation, technical indicator is as follows after testing:
| Quantitatively | ??28.6g/m 2 | Moisture | ??7.0％ |
| Tensile strength | ??32.22N/15mm | Elongation (indulging) | ??17.68％ |
| The thickness banner is poor | ??1.5μm | Bacteriostasis rate | ??99.8％ |
The antibacterial cellulose membrane of present embodiment preparation, when carrying out food product pack, germ resistance is strong, and can not pollute content, is mainly used in the food product pack industry.
Claims (8)
1, a kind of preparation method of antibacterial cellulose membrane, it is characterized in that: may further comprise the steps: raw material makes finished product after choosing operation, viscose glue preparation section, antiseptic-germicide injection process, film preparation operation, desulfurization process, bleaching process, plasticizing operation, dry damping operation, and wherein said raw material is chosen operation: choosing weight ratio is 30%～50% cotton pulp and 70%～50% wood pulp.
2, the preparation method of a kind of antibacterial cellulose membrane according to claim 1 is characterized in that: described viscose glue preparation section:
A, with the cotton pulp wood pulp chosen after alkalization, squeezing, aging, yellow, make cellulose xanthate;
B, with the cellulose xanthate after the yellow, adding concentration is the NaOH solution of 13～20g/L, dissolves, the volume of every batch of cellulose xanthate is 11～14m
3, NaOH solution add-on 95～135kg/ ton paper, temperature is controlled at 16～19 ℃, makes viscose glue after the dissolving, the composition of its viscose glue: α-cell 8.3～8.7%, NaOH5.0～5.6%, viscosity 50～60sec, ammonium value 5.6～7.0ml, all the other are water;
C, the viscose glue after will dissolving carry out maturation, and temperature is controlled between 36～40 ℃, and the time is controlled at 7.5～9.5h, the index of viscose glue: α-cell8.4～8.8% after the maturation, NaOH5.15～5.6%, viscosity 48～58sec, ammonium value 5.3～6.5ml;
D, with the viscose glue after the maturation, after filtering, enter the deaeration tower, temperature of cooling water is controlled between 16～19 ℃, deaeration tower temperature in is controlled at 36～40 ℃, 27～33 ℃ of deaeration tower temperature out controls, the time is controlled at 1.5～2.5min, makes the spinning viscose glue after the deaeration, spinning viscose glue index: α-cell8.85～9.15%, NaOH5.2～5.5%, viscosity 38～48sec, ammonium value 5.0～5.6ml.
3, the preparation method of a kind of antibacterial cellulose membrane according to claim 1, it is characterized in that: described antiseptic-germicide injection process: silver zeolite antiseptic-germicide and de-salted water is even by 0.9～1.2: 9.1～8.8 mixed, change in the hold-up vessel after mixing, open pressurized air, open volume pump, adjusting the volume pump flow scale is 500～1000ml/min, is expelled in the viscose glue, mixes.
4, the preparation method of a kind of antibacterial cellulose membrane according to claim 1, it is characterized in that: described film preparation operation: the viscose glue that will inject behind the antiseptic-germicide is delivered in the coagulating tank, adding concentration is the sulphuric acid soln of 138～148g/L, the acid bath temperature is controlled between 49～55 ℃, reacted 4～10 seconds, and made film.
5, the preparation method of a kind of antibacterial cellulose membrane according to claim 1, it is characterized in that: described desulfurization process: with the film of making, change in the desulfurizer, adding concentration is the sodium hydroxide solution of 1.5～3.0g/L, add-on 1.8～3.5kg/ ton paper, desulfurization temperature is 85～90 ℃, desulfurization is after 6～12 seconds, change in the washing bath, washed 10～20 seconds.
6, the preparation method of a kind of antibacterial cellulose membrane according to claim 1, it is characterized in that: described bleaching process: the film after the desulfurization is changed in the bleaching tank, adding concentration is 0.6～2.0g/L clorox, add-on 2.0～4.0kg/ ton paper, 4-10 is after second in bleaching, change in the washing bath, washed 40～60 seconds.
7, the preparation method of a kind of antibacterial cellulose membrane according to claim 1, it is characterized in that: described plasticizing operation: the film after will bleaching, washing, change in the plasticizing pond, add the glycerine that concentration is 20～40g/L respectively, add-on is 60～90kg/ ton paper, and concentration is the sorbyl alcohol of 15～30g/L, add-on is 40～60kg/ ton paper, temperature is controlled at 50～60 ℃, and the pH value is controlled at 9～12, fusion time 5～10 seconds.
8, the preparation method of a kind of antibacterial cellulose membrane according to claim 1, it is characterized in that: described dry damping operation: the film after will plastifying changes drying room over to, carry out heat-wind circulate drying, temperature is 129～131 ℃, after dry 80～100 seconds, change between damping, temperature is controlled at 40～48 ℃, and relative humidity is controlled at 60～80%RH, damping 5～10 seconds, the moisture controlled of film makes finished product between 6～10%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102212209A (en) * | 2011-04-29 | 2011-10-12 | 钟春燕 | Packaging film for refrigerated foods and preparation method thereof |
| CN102504313A (en) * | 2011-11-07 | 2012-06-20 | 潍坊恒联玻璃纸有限公司 | Method for semi-permeable heat-sealed regenerated cellulose membrane |
| CN102504316A (en) * | 2011-11-07 | 2012-06-20 | 潍坊恒联玻璃纸有限公司 | Method for preparing regenerated cellulose membrane |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102850459B (en) * | 2012-09-24 | 2014-11-26 | 成都丽雅纤维股份有限公司 | Method for producing cellulose membrane by cotton-wood-bamboo composite pulp |
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2009
- 2009-07-13 CN CN2009100167776A patent/CN101649059B/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102212209A (en) * | 2011-04-29 | 2011-10-12 | 钟春燕 | Packaging film for refrigerated foods and preparation method thereof |
| CN102212209B (en) * | 2011-04-29 | 2013-03-20 | 钟春燕 | Packaging film for refrigerated foods and preparation method thereof |
| CN102504313A (en) * | 2011-11-07 | 2012-06-20 | 潍坊恒联玻璃纸有限公司 | Method for semi-permeable heat-sealed regenerated cellulose membrane |
| CN102504316A (en) * | 2011-11-07 | 2012-06-20 | 潍坊恒联玻璃纸有限公司 | Method for preparing regenerated cellulose membrane |
| CN102504316B (en) * | 2011-11-07 | 2013-04-03 | 潍坊恒联玻璃纸有限公司 | Method for preparing regenerated cellulose membrane |
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