CN101649062B - Preparing method of colourful cellulose membrane - Google Patents
Preparing method of colourful cellulose membrane Download PDFInfo
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- CN101649062B CN101649062B CN2009100167808A CN200910016780A CN101649062B CN 101649062 B CN101649062 B CN 101649062B CN 2009100167808 A CN2009100167808 A CN 2009100167808A CN 200910016780 A CN200910016780 A CN 200910016780A CN 101649062 B CN101649062 B CN 101649062B
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Abstract
The invention relates to a cellulose membrane and a preparing method thereof, in particular to a colourful cellulose membrane and a preparing method thereof. The method comprises the following steps: selecting raw material, preparing viscose glue, injecting pigment, preparing films, desulphurizing, blenching, plasticizing, drying and humidifying, and a finished product is obtained. The invention adopts cotton pulp and wood pulp as raw materials. Pigment is directly injected into cellulose glue to produce the colourful cellulose membrane; the cellulose membrane has beautiful color and solves the problems of easy discolourization and color loosing of dying colourful cellulose membrane.
Description
Technical field
The present invention relates to a kind of cellulose membrane and preparation method thereof, relate in particular to a kind of preparation method of colourful cellulose membrane.
Background technology
At present, colourless cellulosefilm can not satisfy people's requirement again on the market, and the color cellulose film becomes a kind of trend gradually.The color cellulose film of producing all is directly to dye with dyestuff after the film forming at present, film after the dyeing fades easily, fades, the packing content thing is polluted, and this also is present color cellulose film market, the big restricted major cause of Application Areas; Dyeing course need carry out heat simultaneously, needs to consume a large amount of steam, has energy dissipation; Full beautiful for the film color and luster after guaranteeing to dye, there is the waste of resource in dye strength control very high, and also taken away a large amount of dyestuffs in the discharge of wastewater after the dyeing; Simultaneously, produce a large amount of sewage after the substantive dyeing, environment has been caused pollution.
Summary of the invention
Technical problem to be solved by this invention has provided a kind of preparation method of colourful cellulose membrane, it is raw material that present method adopts cotton pulp, wood pulp natural cellulose, direct injection pigment in viscose glue, produce colourful cellulose membrane, have beautiful in colour, the problem that solved dyeing colourful cellulose membrane fugitive color, fades.
In order to reach above purpose, the technical solution adopted in the present invention is:
A kind of preparation method of colourful cellulose membrane may further comprise the steps: raw material makes finished product after choosing operation, viscose glue preparation section, pigment 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 12～18g/L, dissolves, the volume of every batch of cellulose xanthate is 10～15m
3, NaOH solution add-on 90～138kg/ ton paper, temperature is controlled at 15～20 ℃, makes viscose glue after the dissolving, the composition of its viscose glue: α-cell 8.2～8.6%, NaOH 4.9～5.6%, viscosity 52～62sec, ammonium value 5.6～7.2ml, all the other are water;
C, the viscose glue after will dissolving carry out maturation, and temperature is controlled between 35～42 ℃, and the time is controlled at 7～10h, the index of viscose glue: α-cell8.5～8.9% after the maturation, NaOH5.1～5.6%, viscosity 49～59sec, ammonium value 5.5～6.6ml;
D, with the viscose glue after the maturation, after filtering, enter the deaeration tower, temperature of cooling water is controlled between 17～20 ℃, deaeration tower temperature in is controlled at 37～41 ℃, 28～34 ℃ of deaeration tower temperature out controls, the time is controlled at 1.0～3.0min, makes the spinning viscose glue after the deaeration, spinning viscose glue index: α-cell8.8～9.3%, NaOH5.2～5.6%, viscosity 42～50sec, ammonium value 5.0～5.5ml.
Described pigment injection process: with pigment dyestuff and de-salted water, be 1: 2～3 ratio by weight ratio, stir, add defoamer again under stirring, the defoamer add-on is 0.5% of a pigment dyestuff amount, squeeze in the hold-up vessel after stirring, open pressurized air, open volume pump, adjust volume pump flow scale to 1200～2000ml/min, be injected in the viscose glue, mix.
Described film preparation operation: the viscose glue that will inject behind the pigment is delivered in the coagulating tank, and adding concentration is the sulphuric acid soln of 140～155g/L, and control acid bath temperature is 50～53 ℃, in 4～9 seconds reaction times, 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 1.6～3.6kg/ ton paper, and desulfurization temperature is 80～90 ℃, desulfurization changed in the washing bath after 6～12 seconds, washed 6～12 seconds.
Described bleaching process: the film after the desulfurization is changed in the bleaching tank, and adding concentration is 0.6～1.6g/L clorox, and add-on 2.5～3.5kg/ ton paper was bleached after 5～9 seconds, changed in the washing bath, washed 40～60 seconds.
Described plasticizing operation: the film after will bleaching, washing, change in the plasticizing pond, add the glycerine that concentration is 25～50g/L respectively, add-on is 70～120kg/ ton paper, and concentration is the sorbyl alcohol of 20～35g/L, and add-on is 45～70kg/ ton paper, temperature is controlled at 52～59 ℃, pH value is controlled at 9～11, and fusion time 4～9 seconds is promptly finished plasticizing.
Described dry damping operation: the film after will plastifying changes drying room over to, carries out heat-wind circulate drying, and temperature is 133 ℃, after dry 70～90 seconds, change between damping, temperature is controlled at 40～50 ℃, relative humidity is controlled at 70～85%RH, and damping 6～12 seconds makes the colourful cellulose membrane finished product.
Among the present invention, the pigment dyestuff of adding selects for use the Hangzhou refined chemical industry company limited that records to produce, and Colanyl 100 serial pigment dyestuffs can be multiple colors such as red, yellow, blue, green.
Among the present invention, the defoamer of adding selects for use Shen, Shijiazhuang human relations development in science and technology company limited to produce SC2 model defoamer.
It is raw material that the present invention adopts with cotton pulp, wood pulp natural cellulose, the preparation colourful cellulose membrane, and in actual applications, degradable has reached environmental protection requirement. and the film that adopts present method to prepare, color is evenly gorgeous, does not fade, and is colour-fast; No static has good elongation and tensile strength, can adapt to automatic high-speed packing, and can reach performances such as the guaranteeing the quality of connection with wrapping of piece, health.
The inventive method at normal temperatures, directly is expelled to pigment in the viscose glue before the film forming, need not to carry out heat, has saved steam consumption greatly, has saved the energy effectively.
The colourful 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 |
The present invention will be further described below in conjunction with embodiment:
Embodiment
Embodiment 1
(1) raw material is chosen operation: choosing weight ratio is that 70% cotton pulp and 30% wood pulp are standby;
(2) 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 13g/L, dissolves, the volume of every batch of cellulose xanthate is 10m
3, NaOH solution add-on 90kg/ ton paper, temperature is controlled at 15 ℃, makes viscose glue after the dissolving, the composition of its viscose glue: α-cell 8.2%, NaOH 4.9%, viscosity 52sec, ammonium value 5.6ml, all the other are water;
C, the viscose glue after will dissolving carry out maturation, and temperature is controlled at 35 ℃, and the time is controlled at 7h, the index of viscose glue: α-cell 8.5% after the maturation, and NaOH 5.1%, viscosity 49sec, ammonium value 5.5ml;
D, with the viscose glue after the maturation, after filtering, enter the deaeration tower, temperature of cooling water is controlled at 17 ℃, deaeration tower temperature in is controlled at 37 ℃, 28 ℃ of deaeration tower temperature out controls, the time is controlled at 1.0min, makes the spinning viscose glue after the deaeration, spinning viscose glue index: α-cell 8.8%, NaOH 5.2%, viscosity 42sec, ammonium value 5.0ml;
(3) pigment injection process: with 50kg red pigment and 150L de-salted water, mixing and stirring adds the 0.25kg defoamer under stirring again, squeeze into after stirring in the hold-up vessel, open pressurized air, open volume pump, adjust the volume pump flow scale to 1200ml/min, be injected in the viscose glue, mix;
(4) film preparation operation: the viscose glue that will inject behind the pigment is delivered in the coagulating tank, and adding concentration is the sulphuric acid soln of 140g/L, and control acid bath temperature is 50 ℃, in 4 seconds reaction times, 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 1.6kg/ ton paper, desulfurization temperature are 80 ℃, and desulfurization changed in the washing bath after 6 seconds, washed 6 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 2.5kg/ ton paper was bleached after 5 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 25g/L respectively, add-on is a 70kg/ ton paper, concentration is the sorbyl alcohol of 35g/L, and add-on is a 70kg/ ton paper, and temperature is controlled at 52 ℃, pH value is controlled at 9, and fusion time 4 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 133 ℃, after dry 82 seconds, changes between damping, and temperature is controlled at 46 ℃, and relative humidity is controlled at 79%RH, and damping 9 seconds makes red cellulose membrane finished product.
The red cellulose membrane of present embodiment preparation, technical indicator is as follows after testing:
| Quantitatively | 25.2g/m 2 | Moisture | 7.6％ |
| Tensile strength | 26.12N/15mm | Elongation (indulging) | 14.66％ |
| The thickness banner is poor | 1.3μm |
Not only color is evenly gorgeous for the red cellulose membrane of present embodiment preparation, and do not fade, colour-fast, avoided pollution effectively to the packing content thing.
Embodiment 2
(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 12g/L, dissolves, the volume of every batch of cellulose xanthate is 11m
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-cell8.28%, NaOH 5.0%, viscosity 53sec, ammonium value 5.8ml, all the other are water;
C, the viscose glue after will dissolving carry out maturation, and temperature is controlled at 36 ℃, and the time is controlled at 7.5h, the index of viscose glue: α-cell 8.58% after the maturation, and NaOH 5.2%, viscosity 51sec, ammonium value 5.6ml;
D, with the viscose glue after the maturation, after filtering, enter the deaeration tower, temperature of cooling water is controlled at 17 ℃, deaeration tower temperature in is controlled at 38 ℃, 30 ℃ of deaeration tower temperature out controls, the time is controlled at 1.3min, makes the spinning viscose glue after the deaeration, spinning viscose glue index: α-cell8.82%, NaOH 5.3%, viscosity 43sec, ammonium value 5.1ml;
(3) pigment injection process: with 80kg orange pigments and 160L de-salted water, mixing and stirring adds the 0.4kg defoamer under stirring again, squeeze into after stirring in the hold-up vessel, open pressurized air, open volume pump, adjust the volume pump flow scale to 1600ml/min, be injected in the viscose glue, mix;
(4) film preparation operation: the viscose glue that will inject behind the pigment is delivered in the coagulating tank, and adding concentration is the sulphuric acid soln of 143g/L, and control acid bath temperature is 52 ℃, in 7 seconds reaction times, makes film;
(5) desulfurization process: with the film of making, change in the desulfurizer, adding concentration is the sodium hydroxide solution of 2.2g/L, and add-on 2.6kg/ ton paper, desulfurization temperature are 85 ℃, and desulfurization changed in the washing bath after 9 seconds, washed 8 seconds;
(6) bleaching process: the film after the desulfurization is changed in the bleaching tank, and adding concentration is the 1.2g/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 30g/L respectively, add-on is a 74kg/ ton paper, concentration is the sorbyl alcohol of 33g/L, and add-on is a 65kg/ ton paper, and temperature is controlled at 55 ℃, the 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 133 ℃, after dry 85 seconds, change between damping, temperature is controlled at 47 ℃, relative humidity is controlled at 81%RH, and damping 10 seconds makes orange cellulose membrane finished product.
The orange cellulose membrane of present embodiment preparation, technical indicator is as follows after testing:
| Quantitatively | 30.1g/m 2 | Moisture | 7.2％ |
| Tensile strength | 29.88N/15mm | Elongation (indulging) | 15.26％ |
| The thickness banner is poor | 1.1μm |
The present invention is at normal temperatures, directly pigment is expelled in the viscose glue before the film forming, need not to carry out heat, has saved steam consumption greatly, has saved the energy effectively.
Embodiment 3
(1) raw material is chosen operation: choosing weight ratio is that 30% cotton pulp and 70% wood pulp are 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 12g/L, dissolves, the volume of every batch of cellulose xanthate is 14m
3, NaOH solution add-on 90kg/ ton paper, temperature is controlled at 17 ℃, makes viscose glue after the dissolving, the composition of its viscose glue: α-cell 8.35%, NaOH 5.2%, viscosity 55sec, ammonium value 5.9ml, all the other are water;
C, the viscose glue after will dissolving carry out maturation, and temperature is controlled at 37 ℃, and the time is controlled at 8h, the index of viscose glue: α-cell8.64% after the maturation, and NaOH 5.2%, viscosity 53sec, ammonium value 5.7ml;
D, with the viscose glue after the maturation, after filtering, enter the deaeration tower, temperature of cooling water is controlled at 18 ℃, 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-cell 8.89%, NaOH 5.3%, viscosity 45sec, ammonium value 5.1ml;
(3) pigment injection process: with 60kg yellow ultramarine and 180L de-salted water, mixing and stirring adds the 0.3kg defoamer under stirring again, squeeze into after stirring in the hold-up vessel, open pressurized air, open volume pump, adjust the volume pump flow scale to 2000ml/min, be injected in the viscose glue, mix;
(4) film preparation operation: the viscose glue that will inject behind the pigment is delivered in the coagulating tank, and adding concentration is the sulphuric acid soln of 145g/L, and control acid bath temperature is 53 ℃, in 6 seconds reaction times, 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 3.5kg/ ton paper, desulfurization temperature are 90 ℃, and desulfurization changed in the washing bath after 10 seconds, washed 11 seconds;
(6) bleaching process: the film after the desulfurization is changed in the bleaching tank, and adding concentration is the 1.5g/L clorox, and add-on 3.4kg/ ton paper was bleached after 9 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 84kg/ ton paper, concentration is the sorbyl alcohol of 31g/L, and add-on is a 62kg/ ton paper, and temperature is controlled at 58 ℃, pH value is controlled at 11, 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 133 ℃, after dry 80 seconds, changes between damping, and temperature is controlled at 45 ℃, and relative humidity is controlled at 77%RH, and damping 9 seconds makes the plain film finished product of yellow fibers.
The plain film of the yellow fibers of present embodiment preparation, technical indicator is as follows after testing:
| Quantitatively | 35.0g/m 2 | Moisture | 7.8％ |
| Tensile strength | 32.22N/15mm | Elongation (indulging) | 16.66％ |
| The thickness banner is poor | 1.2μm |
The plain film of the yellow fibers of present embodiment preparation, no static has good elongation and tensile strength, can adapt to automatic high-speed and pack, and can reach performances such as the guaranteeing the quality of connection with wrapping of piece, health.
Embodiment 4
(1) raw material is chosen operation: choosing weight ratio is that 55% cotton pulp and 45% wood pulp are 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 12.5m
3, NaOH solution add-on 114kg/ ton paper, temperature is controlled at 17.5 ℃, makes viscose glue after the dissolving, the composition of its viscose glue: α-cell 8.4%, NaOH5.1%, viscosity 56sec, ammonium value 6.3ml, all the other are water;
C, the viscose glue after will dissolving carry out maturation, and temperature is controlled at 38 ℃, and the time is controlled at 8.5h, the index of viscose glue: α-cell 8.7% after the maturation, and NaOH 5.3%, viscosity 54sec, ammonium value 6.2ml;
D, with the viscose glue after the maturation, after filtering, enter the deaeration tower, temperature of cooling water is controlled at 18.5 ℃, deaeration tower temperature in is controlled at 39 ℃, 31 ℃ of deaeration tower temperature out controls, the time is controlled at 2min, makes the spinning viscose glue after the deaeration, spinning viscose glue index: α-cell 9.05%, NaOH 5.4%, viscosity 46sec, ammonium value 5.2ml;
(3) pigment injection process: with 80kg blue pigments and 200L de-salted water, mixing and stirring adds the 0.4kg defoamer under stirring again, squeeze into after stirring in the hold-up vessel, open pressurized air, open volume pump, adjust the volume pump flow scale to 1500ml/min, be injected in the viscose glue, mix;
(4) film preparation operation: the viscose glue that will inject behind the pigment is delivered in the coagulating tank, and adding concentration is the sulphuric acid soln of 142g/L, and control acid bath temperature is 51 ℃, in 5 seconds reaction times, makes film;
(5) desulfurization process: with the film of making, change in the desulfurizer, adding concentration is the sodium hydroxide solution of 1.8g/L, and add-on 2.0kg/ ton paper, desulfurization temperature are 86 ℃, and desulfurization changed in the washing bath after 8 seconds, washed 9 seconds;
(6) bleaching process: the film after the desulfurization is changed in the bleaching tank, and adding concentration is the 1.2g/L clorox, and add-on 3.2kg/ ton paper was bleached after 7 seconds, changed in the washing bath, washed 48 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, concentration is the sorbyl alcohol of 27g/L, and add-on is a 58kg/ ton paper, and temperature is controlled at 54 ℃, pH value is controlled at 10, 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 133 ℃, after dry 76 seconds, changes between damping, and temperature is controlled at 43 ℃, and relative humidity is controlled at 74%RH, and damping 8 seconds makes blue cellulose membrane finished product.
The blue cellulose membrane of present embodiment preparation, technical indicator is as follows after testing:
| Quantitatively | 26.2g/m 2 | Moisture | 8.0％ |
| Tensile strength | 25.21N/15mm | Elongation (indulging) | 14.32％ |
| The thickness banner is poor | 1.3μm |
The blue cellulose membrane of present embodiment preparation, in actual applications, degradable has reached environmental protection requirement.
Embodiment 5
(1) raw material is chosen operation: choosing weight ratio is that 55% cotton pulp and 45% wood pulp are standby;
(2) 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 15g/L, dissolves, the volume of every batch of cellulose xanthate is 13m
3, NaOH solution add-on 110kg/ ton paper, temperature is controlled at 18 ℃, makes viscose glue after the dissolving, the composition of its viscose glue: α-cell 8.46%, NaOH 5.3%, viscosity 57sec, ammonium value 6.4ml, all the other are water;
C, the viscose glue after will dissolving carry out maturation, and temperature is controlled at 39 ℃, and the time is controlled at 8.8h, the index of viscose glue: α-cell 8.77% after the maturation, and NaOH 5.5%, 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 at 19 ℃, deaeration tower temperature in is controlled at 40 ℃, 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-cell 9.13%, NaOH 5.4%, viscosity 48sec, ammonium value 5.3ml;
(3) pigment injection process: with 50kg veridian and 120L de-salted water, mixing and stirring adds the 0.25kg defoamer under stirring again, squeeze into after stirring in the hold-up vessel, open pressurized air, open volume pump, adjust the volume pump flow scale to 1600ml/min, be injected in the viscose glue, mix;
(4) film preparation operation: the viscose glue that will inject behind the pigment is delivered in the coagulating tank, and adding concentration is the sulphuric acid soln of 144g/L, and control acid bath temperature is 52 ℃, in 6 seconds reaction times, makes film;
(5) desulfurization process: with the film of making, change in the desulfurizer, adding concentration is the sodium hydroxide solution of 2.5g/L, and add-on 2.6kg/ ton paper, desulfurization temperature are 87 ℃, and desulfurization changed in the washing bath after 8 seconds, washed 8 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 2.9kg/ ton paper was bleached after 6 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 45g/L respectively, add-on is a 96kg/ ton paper, concentration is the sorbyl alcohol of 27g/L, and add-on is a 55kg/ ton paper, and temperature is controlled at 57 ℃, the pH value is controlled at 10.5, 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 133 ℃, after dry 70 seconds, changes between damping, and temperature is controlled at 40 ℃, and relative humidity is controlled at 70%RH, and damping 6 seconds makes the plain film finished product of green fiber.
The plain film of the green fiber of present embodiment preparation, technical indicator is as follows after testing:
| Quantitatively | 31.2g/m 2 | Moisture | 8.2％ |
| Tensile strength | 30.02N/15mm | Elongation (indulging) | 17.11％ |
| The thickness banner is poor | 1.2μm |
The plain film of the green fiber of present embodiment preparation, in actual applications, color is even, does not fade, and is colour-fast.
Embodiment 6
(1) raw material is chosen operation: choosing weight ratio is that 40% cotton pulp and 60% wood pulp are 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 16g/L, dissolves, the volume of every batch of cellulose xanthate is 14m
3, NaOH solution add-on 127kg/ ton paper, temperature is controlled at 19 ℃, makes viscose glue after the dissolving, the composition of its viscose glue: α-cell 8.51%, NaOH 5.4%, viscosity 59sec, ammonium value 6.9ml, all the other are water;
C, the viscose glue after will dissolving carry out maturation, and temperature is controlled at 40 ℃, and the time is controlled at 9.2h, the index of viscose glue: α-cell 8.84% after the maturation, and NaOH 5.5%, viscosity 57sec, ammonium value 6.4ml;
D, with the viscose glue after the maturation, after filtering, enter the deaeration tower, temperature of cooling water is controlled at 19 ℃, deaeration tower temperature in is controlled at 39 ℃, 31 ℃ 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-cell 9.18%, NaOH 5.5%, viscosity 47sec, ammonium value 5.4ml;
(3) pigment injection process: with 60kg violet pigment and 138L de-salted water, mixing and stirring adds the 0.3kg defoamer under stirring again, squeeze into after stirring in the hold-up vessel, open pressurized air, open volume pump, adjust the volume pump flow scale to 1400ml/min, be injected in the viscose glue, mix;
(4) film preparation operation: the viscose glue that will inject behind the pigment is delivered in the coagulating tank, and adding concentration is the sulphuric acid soln of 141g/L, and control acid bath temperature is 49 ℃, in 5 seconds reaction times, 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 2.5kg/ ton paper, desulfurization temperature are 84 ℃, and desulfurization changed in the washing bath after 6 seconds, washed 8 seconds;
(6) bleaching process: the film after the desulfurization is changed in the bleaching tank, and adding concentration is the 1.0g/L clorox, and add-on 3.1kg/ ton paper was bleached after 6 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 48g/L respectively, add-on is a 110kg/ ton paper, concentration is the sorbyl alcohol of 25g/L, and add-on is a 51kg/ ton paper, and temperature is controlled at 55 ℃, pH value is controlled at 10, 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 133 ℃, after dry 90 seconds, change between damping, temperature is controlled at 50 ℃, relative humidity is controlled at 85%RH, and damping 12 seconds makes purple cellulose membrane finished product.
The purple cellulose membrane of present embodiment preparation, technical indicator is as follows after testing:
| Quantitatively | 28.4g/m 2 | Moisture | 6.8％ |
| Tensile strength | 26.68N/15mm | Elongation (indulging) | 15.56％ |
| The thickness banner is poor | 1.1μm |
The purple cellulose membrane of present embodiment preparation, color is evenly gorgeous, does not fade, colour-fast, has avoided the pollution to the packing content thing effectively.
Embodiment 7
(1) raw material is chosen operation: choosing weight ratio is that 60% cotton pulp and 40% wood pulp are 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 13.5m
3, NaOH solution add-on 132kg/ ton paper, temperature is controlled at 17 ℃, makes viscose glue after the dissolving, the composition of its viscose glue: α-cell8.6%, NaOH 5.6%, viscosity 62sec, ammonium value 6.9ml, all the other are water;
C, the viscose glue after will dissolving carry out maturation, and temperature is controlled at 41 ℃, and the time is controlled at 9.7h, the index of viscose glue: α-cell 8.91% after the maturation, and NaOH 5.6%, viscosity 58sec, ammonium value 6.6ml;
D, with the viscose glue after the maturation, after filtering, enter the deaeration tower, temperature of cooling water is controlled at 20 ℃, deaeration tower temperature in is controlled at 41 ℃, 33 ℃ of deaeration tower temperature out controls, the time is controlled at 3.0min, makes the spinning viscose glue after the deaeration, spinning viscose glue index: α-cell 9.3%, NaOH 5.6%, viscosity 50sec, ammonium value 5.5ml;
(3) pigment injection process: with 40kg veridian and 120L de-salted water, mixing and stirring adds the 0.2kg defoamer under stirring again, squeeze into after stirring in the hold-up vessel, open pressurized air, open volume pump, adjust the volume pump flow scale to 1700ml/min, be injected in the viscose glue, mix;
(4) film preparation operation: the viscose glue that will inject behind the pigment is delivered in the coagulating tank, and adding concentration is the sulphuric acid soln of 142g/L, and control acid bath temperature is 51 ℃, in 5 seconds reaction times, makes film;
(5) desulfurization process: with the film of making, change in the desulfurizer, adding concentration is the sodium hydroxide solution of 2.2g/L, and add-on 2.9kg/ ton paper, desulfurization temperature are 88 ℃, and desulfurization changed in the washing bath after 10 seconds, washed 11 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 2.9kg/ ton paper was bleached after 8 seconds, changed in the washing bath, washed 54 seconds;
(7) plasticizing operation: the film after will bleaching, washing, change in the plasticizing pond, add the glycerine that concentration is 49g/L respectively, add-on is a 115kg/ ton paper, concentration is the sorbyl alcohol of 23g/L, and add-on is a 49kg/ ton paper, and temperature is controlled at 56 ℃, pH value is controlled at 11, 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 133 ℃, after dry 88 seconds, change between damping, temperature is controlled at 49 ℃, relative humidity is controlled at 83%RH, and damping 11 seconds makes the plain film finished product of green fiber.
The plain film of the green fiber of present embodiment preparation, technical indicator is as follows after testing:
| Quantitatively | 29.2g/m 2 | Moisture | 7.0％ |
| Tensile strength | 28.54N/15mm | Elongation (indulging) | 16.01％ |
| The thickness banner is poor | 1.3μm |
The plain film of the green fiber of present embodiment preparation, in actual applications, degradable has reached environmental protection requirement.
Embodiment 8
(1) raw material is chosen operation: choosing weight ratio is that 57% cotton pulp and 43% wood pulp are 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 15m
3, NaOH solution add-on 138kg/ ton paper, temperature is controlled at 20 ℃, makes viscose glue after the dissolving, the composition of its viscose glue: α-cell 8.58%, NaOH 5.5%, viscosity 62sec, ammonium value 7.2ml, all the other are water;
C, the viscose glue after will dissolving carry out maturation, and temperature is controlled at 42 ℃, and the time is controlled at 10h, the index of viscose glue: α-cell 9.0% after the maturation, and NaOH 5.4%, viscosity 59sec, ammonium value 6.5ml;
D, with the viscose glue after the maturation, after filtering, enter the deaeration tower, temperature of cooling water is controlled at 20 ℃, deaeration tower temperature in is controlled at 41 ℃, 34 ℃ of deaeration tower temperature out controls, the time is controlled at 2.8min, makes the spinning viscose glue after the deaeration, spinning viscose glue index: α-cell 9.26%, NaOH 5.5%, viscosity 49sec, ammonium value 5.4ml;
(3) pigment injection process: with 60kg veridian and 174L de-salted water, mixing and stirring adds the 0.3kg defoamer under stirring again, squeeze into after stirring in the hold-up vessel, open pressurized air, open volume pump, adjust the volume pump flow scale to 1800ml/min, be injected in the viscose glue, mix;
(4) film preparation operation: the viscose glue that will inject behind the pigment is delivered in the coagulating tank, and adding concentration is the sulphuric acid soln of 144g/L, and control acid bath temperature is 52 ℃, in 7 seconds reaction times, 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 89 ℃, and desulfurization changed in the washing bath after 9 seconds, washed 9 seconds;
(6) bleaching process: the film after the desulfurization is changed in the bleaching tank, and adding concentration is the 1.5g/L clorox, and add-on 3.3kg/ ton paper was bleached after 7 seconds, changes in the washing trough, washes 56 seconds;
(7) plasticizing operation: the film after will bleaching, washing, change in the plasticizing pond, add the glycerine that concentration is 50g/L respectively, add-on is a 120kg/ ton paper, concentration is the sorbyl alcohol of 21g/L, and add-on is a 47kg/ ton paper, and temperature is controlled at 59 ℃, pH value is controlled at 10, 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 133 ℃, after dry 73 seconds, change between damping, temperature is controlled at 41 ℃, relative humidity is controlled at 72%RH, and damping 7 seconds makes green colourful cellulose membrane finished product.
The green colourful cellulose membrane of present embodiment preparation, technical indicator is as follows after testing:
| Quantitatively | 30.0g/m 2 | Moisture | 8.0％ |
| Tensile strength | 29.88N/15mm | Elongation (indulging) | 15.69％ |
| The thickness banner is poor | 1.2μm |
The green colourful cellulose membrane of present embodiment preparation in the preparation process, at normal temperatures, directly is expelled to pigment in the viscose glue before the film forming, need not to carry out heat, has saved steam consumption greatly, has saved the energy effectively.
Claims (1)
1. the preparation method of a colourful cellulose membrane, it is characterized in that: may further comprise the steps: raw material is chosen, make finished product behind the viscose glue preparation section, pigment injection process, film preparation operation, desulfurization process, bleaching process, plasticizing operation, dry damping operation, and concrete steps are as follows:
(1) raw material is chosen: choosing weight ratio is 30%～50% cotton pulp and 70%～50% wood pulp;
(2) viscose glue preparation:
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 12～18g/L, dissolves, the volume of every batch of cellulose xanthate is 10～15m
3, NaOH solution add-on 90～138kg/ ton paper, temperature is controlled at 15～20 ℃, makes viscose glue after the dissolving, the composition of its viscose glue: α-cell 8.2～8.6%, NaOH 4.9～5.6%, viscosity 52～62sec, ammonium value 5.6～7.2ml, all the other are water;
C, the viscose glue after will dissolving carry out maturation, and temperature is controlled between 35～42 ℃, and the time is controlled at 7～10h, the index of viscose glue: α-cell8.5～8.9% after the maturation, NaOH5.1～5.6%, viscosity 49～59sec, ammonium value 5.5～6.6ml;
D, with the viscose glue after the maturation, after filtering, enter the deaeration tower, temperature of cooling water is controlled between 17～20 ℃, deaeration tower temperature in is controlled at 37～41 ℃, 28～34 ℃ of deaeration tower temperature out controls, the time is controlled at 1.0～3.0min, makes the spinning viscose glue after the deaeration, spinning viscose glue index: α-cell8.8～9.3%, NaOH5.2～5.6%, viscosity 42～50sec, ammonium value 5.0～5.5ml;
(3) pigment injection: with pigment dyestuff and de-salted water, be 1: 2～3 ratio by weight ratio, stir, add defoamer again under stirring, the defoamer add-on is 0.5% of a pigment dyestuff amount, squeeze in the hold-up vessel after stirring, open pressurized air, open volume pump, adjust volume pump flow scale to 1200～2000ml/min, be injected in the viscose glue, mix;
(4) film preparation: the viscose glue that will inject behind the pigment is delivered in the coagulating tank, and adding concentration is the sulphuric acid soln of 140～155g/L, and control acid bath temperature is 50～53 ℃, in 4～9 seconds reaction times, makes film;
(5) 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 1.6～3.6kg/ ton paper, and desulfurization temperature is 80～90 ℃, desulfurization changed in the washing bath after 6～12 seconds, washed 6～12 seconds;
(6) bleaching process: the film after the desulfurization is changed in the bleaching tank, and adding concentration is 0.6～1.6g/L clorox, and add-on 2.5～3.5kg/ ton paper was bleached after 5～9 seconds, changed in the washing bath, washed 40～60 seconds;
(7) plasticizing operation: the film after will bleaching, washing, change in the plasticizing pond, add the glycerine that concentration is 25～50g/L respectively, add-on is 70～120kg/ ton paper, concentration is the sorbyl alcohol of 20～35g/L, and add-on is 45～70kg/ ton paper, and temperature is controlled at 52～59 ℃, pH value is controlled at 9～11, plastifies 4～9 seconds;
(8) dry damping operation: the film after will plastifying changes drying room over to, carries out heat-wind circulate drying, and temperature is 133 ℃, after dry 70～90 seconds, change between damping, temperature is controlled at 40～50 ℃, relative humidity is controlled at 70～85%RH, and damping 6～12 seconds makes the colourful cellulose membrane finished product.
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| CN102504313B (en) * | 2011-11-07 | 2013-07-17 | 潍坊恒联玻璃纸有限公司 | Method for semi-permeable heat-sealed 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 |
| CN103012825A (en) * | 2012-11-29 | 2013-04-03 | 安徽徽宁电器仪表集团有限公司 | Preparation method of instrument material |
| CN105696305A (en) * | 2015-09-20 | 2016-06-22 | 绍兴春明天然纤维素膜有限公司 | Production method of colorful natural cellulose membranes |
| CN110004734A (en) * | 2019-02-22 | 2019-07-12 | 山东恒联新材料股份有限公司 | A kind of environmentally friendly high dark coloured technique of regenerated cellulose film thoroughly |
| CN110684228A (en) * | 2019-09-18 | 2020-01-14 | 山东恒联新材料股份有限公司 | Laboratory preparation method of color regenerated cellulose membrane |
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|---|---|---|---|---|
| WO1992019807A1 (en) * | 1991-04-25 | 1992-11-12 | Courtaulds Plc | Dyeing of cellulose |
| 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 |
| CN101265617A (en) * | 2008-04-30 | 2008-09-17 | 宜宾丝丽雅集团有限公司 | Method for producing coloured cut staple by dying viscose glue |
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2009
- 2009-07-13 CN CN2009100167808A patent/CN101649062B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1992019807A1 (en) * | 1991-04-25 | 1992-11-12 | Courtaulds Plc | Dyeing of cellulose |
| 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 |
| CN101265617A (en) * | 2008-04-30 | 2008-09-17 | 宜宾丝丽雅集团有限公司 | Method for producing coloured cut staple by dying viscose glue |
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