CN101718010A - Method for preparing seaweed fiber - Google Patents
Method for preparing seaweed fiber Download PDFInfo
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- CN101718010A CN101718010A CN200910312937A CN200910312937A CN101718010A CN 101718010 A CN101718010 A CN 101718010A CN 200910312937 A CN200910312937 A CN 200910312937A CN 200910312937 A CN200910312937 A CN 200910312937A CN 101718010 A CN101718010 A CN 101718010A
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Abstract
The invention relates to a method for preparing seaweed fiber. The method comprises: adding pretreated seaweed raw material to digestive juice for digestion; filtering digested solution; taking filtrate as spinning solution to spin; and adding cross-linking agents in the digestion or spinning process. The method directly takes the solution obtained from the seaweed raw material through treatment, digestion and filtration to spin. Compared with conventional seaweed fiber spinning process routes, the process route reduces dilution, washing, calcium precipitation, decalcification, precipitation, filtration, drying, grinding, sodium alginate formation, sodium alginate dissolution, defoaming and other processes, greatly reduces cost, and also avoids using chemical reagents causing serious pollution.
Description
Technical field
The present invention relates to field of textiles, relate to the manufacture field of fiber specifically, relate to a kind of preparation method of alginate fibre in particular.
Background technology
Along with petroleum resources are exhausted day by day, traditional chemical fibre industry is faced with the crisis of raw material disappearance; Land resource is in short supply, grain and cotton is striven problems such as ground but the raw material Zhao cotton of viscose and xylon exist.And people constantly increase the demand of fiber, and it is very urgent therefore to develop new fibrous raw material resource.
70% area is covered by seawater on the earth, and marine algae resource is very abundant in the ocean, and is inexhaustible, nexhaustible.In order to address the above problem, in recent years, marine natural compound alginate fibre etc. is subjected to paying close attention to widely, is green renewable resource, utilizes the alginate fibre of preparation such as sodium alginate to can be used as the green fiber material and uses.
At present, the preparation method of alginate fibre is that the water miscible alginate of employing is a raw material mostly, be mixed with the certain density aqueous solution, this solution after handling, deaeration under the vacuum can be obtained spinning solution, utilize measuring pump to extrude it again from spinnerets, enter in the calcium chloride water and solidify, promptly obtain alginate fibre.In early days in patent CN 1068158A and CN1119547A, elaborate the method for preparing alginate fibre with sodium alginate as people such as Sun Yushan.The later stage relevant patent of report is basically on the basis of these two pieces of patents, and alginate fibre is carried out the research of modification aspect, as proposing among the patent CN 1940153A sodium alginate and chitosan graft; Perhaps propose among the patent CN 1986921A with water and lower alcohol as first coagulating bath; Perhaps proposing with sodium alginate and potassium alginate mixture among the patent CN101037814A is the feedstock production alginate fibre.
These research thinkings and mechanism all are that the water miscible alginate of employing is a raw material, and the preparation spinning solution changes water-fast alginate into by methods such as ion-exchanges at last, and research contents comprises concentration of dope, temperature; The set of dispense ratio of coagulating bath, concentration, temperature etc. are to the influence of fibre property; Add other component fiber is carried out modification, increase the functional of fiber.Its main raw material all is water-soluble alginates.
And the process route that extracts alginic acid and salt thereof from marine alga mostly is: immersion → chopping → digestion → dilution → filtration, washing → calcium are analysed → decalcification → precipitation → filtration → oven dry → pulverizing → finished product sodium alginate.Because its technological process of production is long, not high, the required chemical reagent of production efficiency is many, environmental pollution is serious, cause the cost of producing alginate higher, seriously restricted application and the popularization of alginate fibre in civilian garment industry.A kind of method for preparing sodium alginate has been reported in patent application 01115139.0, this method has increased on the basis of above-mentioned traditional handicraft to be handled the early stage of sea-tangle, but a large amount of chemical reagent, especially chloro-containing reagents of using are difficult to satisfy modern environmental protection demand in whole process procedure.
Alginate fibre has been carried out some researchs in the application of civilian dress ornament fermentation both at home and abroad, in the CN200710188153.3 patent, disclose the research of superfine seaweed fiber towel quilt, yet cost has been higher, general public is difficult to buy.Up to the present, yet there are no the research report that directly carries out spinning with marine alga.For the raw material direct fabrics prepare alginate fibre, can significantly reduce the cost of producing alginate fibre with the marine alga, popularize the civilian dress ornament of alginate fibre.
Because traditional handicraft is to prepare alginate by marine alga through complicated chemical method, be raw material again with the alginate, prepare alginate fibre through spinning technique, at last as dress material, complicated step makes alginate fibre dress ornament cost very high, people are difficult to buy, and the penetration and promotion of alginate fibre dress ornament is difficulty very.In order to overcome this difficult problem, the present invention is natural to have, environmental protection, marine alga inexpensive, that be easy to get are raw material, directly obtains spinning solution and carries out spinning and prepare alginate fibre.Direct spinning technology shortens the technological process in the alginate preparation process greatly, and reduced the consumption of chemical raw material, not only alleviate pollution to environment, and greatly reduce production cost, significantly reduce the market price of alginate fibre, lay a good foundation in the application and the large-scale production of garment industry for the expansion alginate fibre, further improve the comfortableness of people's dress ornament, have great importance to alleviating the resource scarcity situation simultaneously.
Summary of the invention
The object of the invention is to provide a kind of preparation method of alginate fibre, and the use that described preparation method is simple to operate, with low cost, avoided the chemical reagent of high pollution can reduce the production cost of alginate fibre goods greatly.
In order to realize the foregoing invention purpose, the present invention takes following technical scheme:
A kind of preparation method of alginate fibre, described method comprises: the marine alga raw material joins in the digestive juice and digests after pre-treatment, and postdigestive solution filters, and filtrate is carried out spinning as spinning solution, and adds crosslinking agent in digestion process or spinning process.
The present invention directly carries out spinning with the marine alga raw material through handling the solution that obtains after digestion and the filtration, compare with traditional alginate fibre spinning technique route, this process route has reduced flow processs such as dilution, washing, calcium are analysed, decalcification, precipitation, filtration, oven dry, pulverizing, finished product sodium alginate, sodium alginate dissolving, deaeration, and cost is significantly reduced.Simultaneously, also avoided the use of with serious pollution chemical reagent.
According to foregoing preparation method, any crosslinking agent that described crosslinking agent can be known for those skilled in the art are common, the present invention preferably adopts is one or several any mixing in chloropropylene oxide, borax, toluene di-isocyanate(TDI) or the twain-aldehyde compound compound, more preferably glutaraldehyde or glyoxal;
Described dosage of crosslinking agent is 1/4～3/4 of a marine alga raw material weight, is preferably 1/2.
The present invention takes the dosage of crosslinking agent of above-mentioned scope, is in order further to improve the fiber quality of preparation on the basis of realizing the object of the invention.If dosage of crosslinking agent is few, the degree of cross linking is not enough, the fiber poor water resistance, and the filament performance is low; If crosslinking agent is too much, degree of cross linking height, silk is hard, and feel is poor, and in addition, too much crosslinking agent is difficult for removing, and causes waste, has improved production cost.
Described crosslinking agent can add in digestion process, for example earlier crosslinking agent is joined in the digestive juice, adds the marine alga raw material of pre-treatment then; Perhaps can behind the marine alga raw material that adds pre-treatment, add digestive juice again; Even can be in the digestion process process, even digestion process joins crosslinking agent in the digestive juice after finishing.
In addition, crosslinking agent can also add in spinning process, for example joins in the employed coagulating bath in the process of setting of spinning; Perhaps when oil agent, join in the used finish.
The present invention preferably adds crosslinking agent in digestion process, especially before the marine alga raw material is joined digestive juice, perhaps the marine alga raw material is joined digestive juice after, add described crosslinking agent, stir evenly and get final product.
In digestion process, add crosslinking agent, add crosslinking agent with other steps and compare, can be so that the crosslinking agent mixing be more even, under the prerequisite that reaches the like products quality, dosage of crosslinking agent is few, and is crosslinked more abundant.
According to foregoing preparation method, described pre-treatment is shredded then for the marine alga raw material is soaked.
Described immersion can be with reference to the marine alga raw material soaking operation of prior art, the present invention is preferably at room temperature and is soaked in water, preferably being the water logging bubble 6～24h of 5～20 times of marine alga raw material weights with weight, more preferably is the water logging bubble 6～15h of 8～12 times of marine alga raw material weights with weight.
The present invention finds that through overtesting after marine alga absorbed a certain amount of moisture, cell tissue was just saturated, no longer absorbs moisture, more also not effect of time expand.The water yield, time are controlled at above-mentioned scope, can using water wisely, raise the efficiency.
The present invention even can also further preferably in immersion process, add formaldehyde, the formaldehyde consumption is preferably and adds that to make concentration of formaldehyde behind the formaldehyde be 0.3～2%, and more preferably 0.7～1.4%.
By adding formaldehyde, can precipitate the pigment in the marine alga raw material, make that the fiber colour that finally processes is better.
In order further to shorten the time that digests later, even can also preferably in immersion process, add carbonate and carry out predigestion, be preferably one or more any mixing in sodium carbonate, potash or the carbonic hydroammonium, more preferably sodium carbonate;
Described carbonate consumption is preferably 0.5～5% of marine alga raw material, is preferably 1～3%, and more preferably 2%.
In addition, if, can obtain fresh marine alga raw material near the marine alga places of origin of raw materials, such as sea-tangle, even soaking-free, can directly use after the washes clean.Therefore, above-mentioned pre-treatment is not the necessary condition that realizes the object of the invention.
After soaking end, the marine alga raw material after preferably will soaking washes with water, and is colourless to cleaning solution.
Chopping of the present invention can be preferably the marine alga raw material that will soak, and to be cut into length and width be 1～10cm.
According to foregoing preparation method, described digestive juice is a carbonate aqueous solution, is preferably one or more any mixing in sodium carbonate, potash or the carbonic hydroammonium, more preferably sodium carbonate;
Described digestive juice concentration is 5%～25%, is preferably 15%～20%; Described digestive juice is 0.5: 1～5: 1 with marine alga raw material weight ratio, is preferably 1: 1～3: 1; More preferably 2: 1.
According to foregoing preparation method, described digestion is stirred for joining in the digestive juice through the marine alga raw material of pre-treatment, heats up, and leaves standstill after the insulation reaction, and vacuumizing and defoaming both got then.
According to foregoing preparation method, described stirring is speed 80～120rpm, is preferably 100rpm; Described intensification is for being warming up to 40～60 ℃, be preferably 50 ℃, described insulation reaction reduces mixing speed to 55～65rpm for heat up finishing after 0.5～1.5h is stirred in the back, reduces mixing speed to 25～35rpm after stirring 1.5～2.5h again, is cooled to 30～40 ℃ after stirring 2.5～3.5h; Being preferably and heat up finishing to reduce mixing speed to 60rpm after 1h is stirred in the back, reducing mixing speed to 30rpm after stirring 2h again, being cooled to 35 ℃ after stirring 3h.
According to foregoing preparation method, described vacuumizing and defoaming is deaeration 1.5～2.5h under pressure 100～1000Pa, is preferably deaeration 2h under 400～700Pa.
The present invention can use the double helix extruder after digestion process finishes, postdigestive solution is sent in the filter filtered.
Perhaps feed nitrogen in reaction vessel, be forced into 0.3～0.7MPa, be preferably 0.5MPa, the bleeder valve of openable container bottom is sent material into filter then.
What preferably adopted in its middle filtrator filter medium aperture is 200～1000 orders, more preferably 300～500 orders.
According to foregoing preparation method, described filter liquor concentration is weight percentage 10～65%, 30～85 ℃ of temperature, and viscosity 800～3000mPaS, preferred concentration are weight percentage 30～50%, 50～65 ℃ of temperature, viscosity 1000～2000mPaS.
According to foregoing preparation method, described spinning for use spinnerets spray silk, solidify after-drawing, oil agent, crosslinked back drying both alginate fibre.
Spray silk of the present invention can be with reference to the processing technology of alginate fibre in the prior art, and what the present invention preferably adopted is that nascent tow is derived with 8～15m/min speed, is preferably 10m/min.
Jet stretch is controlled at 10～30% then, is preferably 18～22%, and drawing-off is 1.5～3 times then, is preferably 1.8～2.5 times
Wherein the The hole diameter of spinneret of spray silk usefulness can be preferably 0.05～0.12mm, more preferably 0.08mm.
Described solidifying can preferably adopt calcium chloride water as coagulating bath.
Calcium chloride water concentration is 1～5%, is preferably 2.5%.
Setting time is preferably 30～180 seconds, more preferably 30 seconds.
In addition, in order further to increase the functional of alginate fibre, can also in coagulating bath, increase metal ions such as silver ion, copper ion, ferrous ion.Its concrete detail operations and consumption can be with reference to the prior art similar operations.
According to foregoing preparation method, described crosslinked be 40～120 ℃ of down dry 5～40min, be preferably 60～100 ℃ of down dry 10～20min, more preferably 80 ℃ of dry 10min down.
Above-mentioned crosslinked operating parameter is a preferred operations of the present invention, can further improve the alginate fibre product quality, if for example the time is too short, temperature is too low, cross-linking reaction is complete inadequately; Temperature is too high, causes the degraded of alginate fibre main chain, has reduced fibre strength.
Marine alga raw material of the present invention includes but not limited to red algae, green alga, brown algae and sargassum.
By alginate fibre line density≤1.5d that said method makes, fracture strength 〉=3.0g/d.
The preparation method of alginate fibre provided by the invention has following advantage:
(1) simple to operate, step is few, is fit to suitability for industrialized production;
(2) avoid the use of a large amount of poisonous chemical reagent, operating personnel have been poisoned little, be beneficial to environmental protection;
(3) product chemical reagent residual quantity is lower, is beneficial to the healthy of user;
(4) processing cost reduces greatly, is convenient to the popularization and application of high-grade alginate fibre goods.
The specific embodiment
Below with embodiment technical scheme of the present invention is further described; to help advantage to technical scheme of the present invention; effect has further to be understood, and embodiment does not limit protection scope of the present invention, and protection scope of the present invention is decided by claim.
Embodiment 1
With 0.5 kilogram in commercial dried sea-tangle, place 5 kilograms of running water, add 10g sodium carbonate, in water, add 50 gram formalins simultaneously, at room temperature soaked 12 hours.
With soaked sea-tangle be washed till washing lotion be colourless after, be cut into the square of 1cm size.In the 5L reactor, add with 1 kilogram of 15% aqueous sodium carbonate of deionized water preparation, add crosslinking agent glyoxal 250 grams simultaneously, simultaneously the sea-tangle that cuts is put into still.
Start stirring, speed is 100r/min, and temperature is raised to 50 ℃, observe and stir moment of torsion, after 1 hour mixing speed is reduced to 60r/min, after 2 hours mixing speed is reduced to 30r/min, stop after being cooled to 35 ℃ after 3 hours stirring, leave standstill, vacuumizing and defoaming 2 hours, vacuum pressure 500Pa.
In still, lead to nitrogen, pressurization 0.5MPa, bleeder valve, booster pump are sent material into filter at the bottom of the unlatching still, and using the aperture is that 400 purpose filter mediums filter, and the filtrate that filtration obtains directly enters spinning pump and carries out spinning.
The filter liquor concentration 40% that obtains, viscosity is 1500mPaS, adjusts 55 ℃ of temperature, and the spinning jet used aperture of spinning is 0.08mm, calcium chloride water is as coagulating bath, concentration is 2.5%, and setting time is 30 seconds, jet stretch 20%, nascent tow is derived 2.2 times of first break draft with 10m/min speed, oil agent, 80 ℃ be crosslinked down, dry 10 minutes, cut off obtaining filament number 1.5d, the alginate fibre of intensity 3.92g/d.
Embodiment 2
With 0.5 kilogram in commercial dried sea-tangle, place 5 kilograms of running water, add 20g sodium carbonate, in water, add 50 gram formalins simultaneously, at room temperature soaked 12 hours.
With soaked sea-tangle be washed till washing lotion be colourless after, be cut into the square of 2cm size.In the 5L reactor, add with 1.5 kilograms of 15% aqueous sodium carbonates of deionized water preparation, add crosslinking agent glyoxal 250 grams simultaneously, simultaneously the sea-tangle that cuts is put into still.
Start stirring, speed is 100r/min, and temperature is raised to 50 ℃, observe and stir moment of torsion, after 1 hour mixing speed is reduced to 60r/min, after 2 hours mixing speed is reduced to 30r/min, stop after being cooled to 35 ℃ after 3 hours stirring, leave standstill, vacuumizing and defoaming 2 hours, vacuum pressure 500Pa.
In still, lead to nitrogen, pressurization 0.5MPa, bleeder valve, booster pump are sent material into filter at the bottom of the unlatching still, and using the aperture is that 400 purpose filter mediums filter, and the filtrate that filtration obtains directly enters spinning pump and carries out spinning.
The filter liquor concentration 40% that obtains, viscosity is 1400mPaS, adjusts 60 ℃ of temperature, and the spinning jet used aperture of spinning is 0.08mm, calcium chloride water is as coagulating bath, concentration is 2.5%, and setting time is 35 seconds, jet stretch 22%, nascent tow is derived 2.3 times of first break draft with 10m/min speed, oil agent, 80 ℃ be crosslinked down, dry 10 minutes, cut off obtaining filament number 1.43d, the alginate fibre of intensity 3.91g/d.
Embodiment 3
With 1.0 kilograms in commercial dried sea-tangle, place 8 kilograms of running water, add 10g sodium carbonate, in water, add 56 gram formalins simultaneously, at room temperature soaked 10 hours.
With soaked sea-tangle be washed till washing lotion be colourless after, be cut into the square of 1cm size.In the 10L reactor, add with 2 kilograms of 17% aqueous sodium carbonates of deionized water preparation, add crosslinking agent glyoxal 600 grams simultaneously, simultaneously the sea-tangle that cuts is put into still.
Start stirring, speed is 100r/min, and temperature is raised to 50 ℃, observe and stir moment of torsion, after 1 hour mixing speed is reduced to 62r/min, after 2 hours mixing speed is reduced to 28r/min, stop after being cooled to 35 ℃ after 3 hours stirring, leave standstill, vacuumizing and defoaming 2 hours, vacuum pressure 500Pa.
In still, lead to nitrogen, pressurization 0.5MPa, bleeder valve, booster pump are sent material into filter at the bottom of the unlatching still, and using the aperture is that 300 purpose filter mediums filter, and the filtrate that filtration obtains directly enters spinning pump and carries out spinning.
The filter liquor concentration 45% that obtains, viscosity is 2000mPaS, adjusts 55 ℃ of temperature, and the spinning jet used aperture of spinning is 0.08mm, calcium chloride water is as coagulating bath, concentration is 2.5%, and setting time is 40 seconds, jet stretch 20%, nascent tow is derived 2.2 times of first break draft with 10m/min speed, oil agent, 80 ℃ be crosslinked down, dry 10 minutes, cut off obtaining filament number 1.49d, the alginate fibre of intensity 3.90g/d.
Embodiment 4
With 1.5 kilograms in commercial dried sea-tangle, place 18 kilograms of running water, add 30g sodium carbonate, at room temperature soaked 15 hours.
With soaked sea-tangle be washed till washing lotion be colourless after, be cut into the square of 1cm size.In the 30L reactor, add with 1.5 kilograms of 18% aqueous sodium carbonates of deionized water preparation, add crosslinking agent glyoxal 600 grams simultaneously, simultaneously the sea-tangle that cuts is put into still.
Start stirring, speed is 90r/min, and temperature is raised to 50 ℃, observe and stir moment of torsion, after 1 hour mixing speed is reduced to 61r/min, after 2.2 hours mixing speed is reduced to 29r/min, stop after being cooled to 35 ℃ after 3 hours stirring, leave standstill, vacuumizing and defoaming 2 hours, vacuum pressure 400Pa.
In still, lead to nitrogen, pressurization 0.5MPa, bleeder valve, booster pump are sent material into filter at the bottom of the unlatching still, and using the aperture is that 500 purpose filter mediums filter, and the filtrate that filtration obtains directly enters spinning pump and carries out spinning.
The filter liquor concentration 30% that obtains, viscosity is 1000mPaS, adjusts 55 ℃ of temperature, and the spinning jet used aperture of spinning is 0.12mm, calcium chloride water is as coagulating bath, concentration is 2.0%, and setting time is 30 seconds, jet stretch 18%, nascent tow is derived 1.9 times of first break draft with 10m/min speed, oil agent, 80 ℃ be crosslinked down, dry 15 minutes, cut off obtaining filament number 1.51d, the alginate fibre of intensity 3.91g/d.
Embodiment 5
With 10 kilograms in commercial dried sea-tangle, place the double centner running water, add 200g sodium carbonate, in water, add 500 gram formalins simultaneously, at room temperature soaked 6 hours.
With soaked sea-tangle be washed till washing lotion be colourless after, be cut into the square of 2cm size.In the 150L reactor, add with 30 kilograms of 20% aqueous sodium carbonates of deionized water preparation, add crosslinking agent glyoxal 5kg simultaneously, simultaneously the sea-tangle that cuts is put into still.
Start stirring, speed is 110r/min, and temperature is raised to 40 ℃, observe and stir moment of torsion, after 0.5 hour mixing speed is reduced to 60r/min, after 1.8 hours mixing speed is reduced to 30r/min, stop after being cooled to 35 ℃ after 3 hours stirring, leave standstill, vacuumizing and defoaming 2 hours, vacuum pressure 600Pa.
In still, lead to nitrogen, pressurization 0.5MPa, bleeder valve, booster pump are sent material into filter at the bottom of the unlatching still, and using the aperture is that 400 purpose filter mediums filter, and the filtrate that filtration obtains directly enters spinning pump and carries out spinning.
The filter liquor concentration 38% that obtains, viscosity is 1300mPaS, adjusts 80 ℃ of temperature, and the spinning jet used aperture of spinning is 0.08mm, calcium chloride water is as coagulating bath, concentration is 2.7%, and setting time is 50 seconds, jet stretch 22%, nascent tow is derived 2.5 times of first break draft with 8m/min speed, oil agent, 80 ℃ be crosslinked down, dry 20 minutes, cut off obtaining filament number 1.25d, the alginate fibre of intensity 3.9g/d.
Embodiment 6
With 2.5 kilograms in commercial dried sea-tangle, place 25 kilograms of running water, add 25g sodium carbonate, at room temperature soaked 12 hours.
With soaked sea-tangle be washed till washing lotion be colourless after, be cut into the square of 1cm size.In the 50L reactor, add with 5 kilograms of 17% aqueous sodium carbonates of deionized water preparation, add crosslinking agent glyoxal 1625 grams simultaneously, simultaneously the sea-tangle that cuts is put into still.
Start stirring, speed is 100r/min, and temperature is raised to 60 ℃, observe and stir moment of torsion, after 0.7 hour mixing speed is reduced to 59r/min, after 2 hours mixing speed is reduced to 30r/min, 3.1 stop after being cooled to 35 ℃ after hour stirring, leave standstill, vacuumizing and defoaming 2 hours vacuum pressure 600Pa.
In still, lead to nitrogen, pressurization 0.5MPa, bleeder valve, booster pump are sent material into filter at the bottom of the unlatching still, and using the aperture is that 300 purpose filter mediums filter, and the filtrate that filtration obtains directly enters spinning pump and carries out spinning.
The filter liquor concentration 38% that obtains, viscosity is 1300mPaS, adjusts 78 ℃ of temperature, and the spinning jet used aperture of spinning is 0.06mm, calcium chloride water is as coagulating bath, concentration is 1.0%, and setting time is 60 seconds, jet stretch 19%, nascent tow is derived 2.4 times of first break draft with 15m/min speed, oil agent, 70 ℃ be crosslinked down, dry 10 minutes, cut off obtaining filament number 1.29d, the alginate fibre of intensity 3.85g/d.
Embodiment 7
With 50 kilograms in commercial dried sea-tangle, place 400 kilograms of running water, add 1.5kg sodium carbonate, in water, add 1200 gram formalins simultaneously, at room temperature soaked 14 hours.
With soaked sea-tangle be washed till washing lotion be colourless after, be cut into the square of 4cm size.In the 600L reactor, add with 50 kilograms of 15% aqueous sodium carbonates of deionized water preparation, add crosslinking agent glyoxal 20kg simultaneously, simultaneously the sea-tangle that cuts is put into still.
Start stirring, speed is 120r/min, temperature is raised to 50 ℃, observe and stir moment of torsion, 1.1 after hour mixing speed is reduced to 58r/min, after 2 hours mixing speed is reduced to 32r/min, stop after being cooled to 35 ℃ after 3.1 hours stirring, leave standstill, vacuumizing and defoaming 2.1 hours, vacuum pressure 700Pa.
In still, lead to nitrogen, pressurization 0.5MPa, bleeder valve, booster pump are sent material into filter at the bottom of the unlatching still, and using the aperture is that 400 purpose filter mediums filter, and the filtrate that filtration obtains directly enters spinning pump and carries out spinning.
The filter liquor concentration 42% that obtains, viscosity is 1700mPaS, adjusts 58 ℃ of temperature, and the spinning jet used aperture of spinning is 0.09mm, calcium chloride water is as coagulating bath, concentration is 2.2%, and setting time is 30 seconds, jet stretch 21%, nascent tow is derived 2.2 times of first break draft with 12m/min speed, oil agent, 60 ℃ be crosslinked down, dry 10 minutes, cut off obtaining filament number 1.50d, the alginate fibre of intensity 3.82g/d.
Embodiment 8
With 25 kilograms in commercial dried sea-tangle, place 225 kilograms of running water, add 500g sodium carbonate, in water, add 2700 gram formalins simultaneously, at room temperature soaked 8 hours.
With soaked sea-tangle be washed till washing lotion be colourless after, be cut into the square of 3cm size.In the 350L reactor, add with 50 kilograms of 19% aqueous sodium carbonates of deionized water preparation, add crosslinking agent glyoxal 7500 grams simultaneously, simultaneously the sea-tangle that cuts is put into still.
Start stirring, speed is 80r/min, and temperature is raised to 50 ℃, observe and stir moment of torsion, after 1 hour mixing speed is reduced to 60r/min, after 2 hours mixing speed is reduced to 31r/min, 3.2 stop after being cooled to 37 ℃ after hour stirring, leave standstill, vacuumizing and defoaming 2.2 hours vacuum pressure 600Pa.
In still, lead to nitrogen, pressurization 0.5MPa, bleeder valve, booster pump are sent material into filter at the bottom of the unlatching still, and using the aperture is that 500 purpose filter mediums filter, and the filtrate that filtration obtains directly enters spinning pump and carries out spinning.
The filter liquor concentration 47% that obtains, viscosity is 2200mPaS, adjusts 50 ℃ of temperature, and the spinning jet used aperture of spinning is 0.11mm, calcium chloride water is as coagulating bath, concentration is 5.0%, and setting time is 70 seconds, jet stretch 15%, nascent tow is derived 2.0 times of first break draft with 9m/min speed, oil agent, 90 ℃ be crosslinked down, dry 10 minutes, cut off obtaining filament number 1.52d, the alginate fibre of intensity 3.90g/d.
Embodiment 9
With 0.5 kilogram in commercial dried sea-tangle, place 5.5 kilograms of running water, add 10g sodium carbonate, at room temperature soaked 11 hours.
With soaked sea-tangle be washed till washing lotion be colourless after, be cut into the square of 2cm size.In the 10L reactor, add with 1 kilogram of 12% aqueous sodium carbonate of deionized water preparation, add crosslinking agent glyoxal 350 grams simultaneously, simultaneously the sea-tangle that cuts is put into still.
Start stirring, speed is 95r/min, and temperature is raised to 55 ℃, observe and stir moment of torsion, after 1 hour mixing speed is reduced to 60r/min, after 2.1 hours mixing speed is reduced to 35r/min, stop after being cooled to 38 ℃ after 3 hours stirring, leave standstill, vacuumizing and defoaming 2 hours, vacuum pressure 700Pa.
In still, lead to nitrogen, pressurization 0.4MPa, bleeder valve, booster pump are sent material into filter at the bottom of the unlatching still, and using the aperture is that 300 purpose filter mediums filter, and the filtrate that filtration obtains directly enters spinning pump and carries out spinning.
The filter liquor concentration 33% that obtains, viscosity is 1100mPaS, adjusts 63 ℃ of temperature, and the spinning jet used aperture of spinning is 0.08mm, calcium chloride water is as coagulating bath, concentration is 2.5%, and setting time is 30 seconds, jet stretch 25%, nascent tow is derived 3.0 times of first break draft with 10m/min speed, oil agent, 100 ℃ be crosslinked down, dry 20 minutes, cut off obtaining filament number 1.1d, the alginate fibre of intensity 3.86g/d.
Embodiment 10
With 35 kilograms in commercial dried sea-tangle, place 350 kilograms of running water, add 700g sodium carbonate, in water, add 4900 gram formalins simultaneously, at room temperature soaked 12 hours.
With soaked sea-tangle be washed till washing lotion be colourless after, be cut into the square of 1cm size.In the 450L reactor, add with 70 kilograms of 10% aqueous sodium carbonates of deionized water preparation, add crosslinking agent glyoxal 8750 grams simultaneously, simultaneously the sea-tangle that cuts is put into still.
Start stirring, speed is 110r/min, temperature is raised to 45 ℃, observe and stir moment of torsion, 1.2 after hour mixing speed is reduced to 58r/min, after 2.3 hours mixing speed is reduced to 30r/min, stop after being cooled to 34 ℃ after 2.9 hours stirring, leave standstill, vacuumizing and defoaming 2 hours, vacuum pressure 500Pa.
In still, lead to nitrogen, pressurization 0.6MPa, bleeder valve, booster pump are sent material into filter at the bottom of the unlatching still, and using the aperture is that 400 purpose filter mediums filter, and the filtrate that filtration obtains directly enters spinning pump and carries out spinning.
The filter liquor concentration 40% that obtains, viscosity is 1600mPaS, adjusts 45 ℃ of temperature, and the spinning jet used aperture of spinning is 0.08mm, calcium chloride water is as coagulating bath, concentration is 2.7%, and setting time is 100 seconds, jet stretch 20%, nascent tow is derived 2.8 times of first break draft with 10m/min speed, oil agent, 80 ℃ be crosslinked down, dry 15 minutes, cut off obtaining filament number 1.25d, the alginate fibre of intensity 3.85g/d.
Embodiment 11
With 50 kilograms in commercial dried sea-tangle, place 550 kilograms of running water, add 500g sodium carbonate, in water, add 2750 gram formalins simultaneously, at room temperature soaked 5 hours.
With soaked sea-tangle be washed till washing lotion be colourless after, be cut into the square of 2cm size.In the 700L reactor, add with 25 kilograms of 25% aqueous sodium carbonates of deionized water preparation, add crosslinking agent glyoxal 25kg simultaneously, simultaneously the sea-tangle that cuts is put into still.
Start stirring, speed is 100r/min, temperature is raised to 60 ℃, observe and stir moment of torsion, 0.9 after hour mixing speed is reduced to 55r/min, after 1.7 hours mixing speed is reduced to 28r/min, stop after being cooled to 33 ℃ after 2.7 hours stirring, leave standstill, vacuumizing and defoaming 1.7 hours, vacuum pressure 600Pa.
In still, lead to nitrogen, pressurization 0.6MPa, bleeder valve, booster pump are sent material into filter at the bottom of the unlatching still, and using the aperture is that 400 purpose filter mediums filter, and the filtrate that filtration obtains directly enters spinning pump and carries out spinning.
The filter liquor concentration 30% that obtains, viscosity is 1000mPaS, adjusts 53 ℃ of temperature, and the spinning jet used aperture of spinning is 0.10mm, calcium chloride water is as coagulating bath, concentration is 3.0%, and setting time is 150 seconds, jet stretch 10%, nascent tow is derived 2.2 times of first break draft with 10m/min speed, oil agent, 80 ℃ be crosslinked down, dry 18 minutes, cut off obtaining filament number 1.45d, the alginate fibre of intensity 3.84g/d.
Embodiment 12
With 40 kilograms in commercial dried sea-tangle, place 320 kilograms of running water, add 200g sodium carbonate, at room temperature soaked 18 hours
With soaked sea-tangle be washed till washing lotion be colourless after, be cut into the square of 1cm size.In the 550L reactor, add with 160 kilograms of 20% aqueous sodium carbonates of deionized water preparation, add crosslinking agent glyoxal 24kg simultaneously, simultaneously the sea-tangle that cuts is put into still.
Start stirring, speed is 100r/min, temperature is raised to 55 ℃, observe and stir moment of torsion, 1.5 after hour mixing speed is reduced to 60r/min, after 2.0 hours mixing speed is reduced to 30r/min, stop after being cooled to 40 ℃ after 3.0 hours stirring, leave standstill, vacuumizing and defoaming 2 hours, vacuum pressure 500Pa.
In still, lead to nitrogen, pressurization 0.7MPa, bleeder valve, booster pump are sent material into filter at the bottom of the unlatching still, and using the aperture is that 300 purpose filter mediums filter, and the filtrate that filtration obtains directly enters spinning pump and carries out spinning.
The filter liquor concentration 46% that obtains, viscosity is 2100mPaS, adjusts 40 ℃ of temperature, and the spinning jet used aperture of spinning is 0.09mm, calcium chloride water is as coagulating bath, concentration is 4.0%, and setting time is 30 seconds, jet stretch 20%, nascent tow is derived 1.6 times of first break draft with 14m/min speed, oil agent, 45 ℃ be crosslinked down, dry 12 minutes, cut off obtaining filament number 2.0d, the alginate fibre of intensity 3.80g/d.
Embodiment 13
With 30 kilograms in commercial dried sea-tangle, place 300 kilograms of running water, add 1.5kg sodium carbonate, at room temperature soaked 20 hours.
With soaked sea-tangle be washed till washing lotion be colourless after, be cut into the square of 4cm size.In the 450L reactor, add with 60 kilograms of 15% aqueous sodium carbonates of deionized water preparation, add crosslinking agent glutaraldehyde 12kg simultaneously, simultaneously the sea-tangle that cuts is put into still.
Start stirring, speed is 105r/min, temperature is raised to 50 ℃, observe and stir moment of torsion, 1.0 after hour mixing speed is reduced to 60r/min, after 2.0 hours mixing speed is reduced to 27r/min, stop after being cooled to 35 ℃ after 2.5 hours stirring, leave standstill, vacuumizing and defoaming 2 hours, vacuum pressure 800Pa.
In still, lead to nitrogen, pressurization 0.3MPa, bleeder valve, booster pump are sent material into filter at the bottom of the unlatching still, and using the aperture is that 200 purpose filter mediums filter, and the filtrate that filtration obtains directly enters spinning pump and carries out spinning.
The filter liquor concentration 50% that obtains, viscosity is 2400mPaS, adjusts 52 ℃ of temperature, and the spinning jet used aperture of spinning is 0.08mm, calcium chloride water is as coagulating bath, concentration is 2.5%, and setting time is 30 seconds, jet stretch 22%, nascent tow is derived 1.5 times of first break draft with 12m/min speed, oil agent, 120 ℃ be crosslinked down, dry 10 minutes, cut off obtaining filament number 2.06d, the alginate fibre of intensity 3.78g/d.
Embodiment 14
With 10 kilograms in commercial dried sea-tangle, place 200 kilograms of running water, in water, add 3400 gram formalins, at room temperature soaked 12 hours.
With soaked sea-tangle be washed till washing lotion be colourless after, be cut into the square of 7cm size.In the 400L reactor, add with 50 kilograms of 5% aqueous sodium carbonates of deionized water preparation, add crosslinking agent borax 4.5kg simultaneously, simultaneously the sea-tangle that cuts is put into still.
Start stirring, speed is 120r/min, temperature is raised to 40 ℃, observe and stir moment of torsion, 1.2 after hour mixing speed is reduced to 57r/min, after 1.5 hours mixing speed is reduced to 33r/min, stop after being cooled to 38 ℃ after 3.5 hours stirring, leave standstill, vacuumizing and defoaming 1.5 hours, vacuum pressure 1000Pa.
In still, lead to nitrogen, pressurization 0.5MPa, bleeder valve, booster pump are sent material into filter at the bottom of the unlatching still, and using the aperture is that 800 purpose filter mediums filter, and the filtrate that filtration obtains directly enters spinning pump and carries out spinning.
The filter liquor concentration 15% that obtains, viscosity is 900mPaS, adjusts 75 ℃ of temperature, and the spinning jet used aperture of spinning is 0.12mm, calcium chloride water is as coagulating bath, concentration is 2.9%, and setting time is 40 seconds, jet stretch 30%, nascent tow is derived 2.2 times of first break draft with 15m/min speed, oil agent, 110 ℃ be crosslinked down, dry 5 minutes, cut off obtaining filament number 1.44d, the alginate fibre of intensity 3.86g/d.
Embodiment 15
With 20 kilograms in commercial dried sea-tangle, place the double centner running water, at room temperature soaked 10 hours.
With soaked sea-tangle be washed till washing lotion be colourless after, be cut into the square of 10cm size.In the 200L reactor, add with 20 kilograms of 12% aqueous sodium carbonates of deionized water preparation, add crosslinking agent glyoxal 10kg simultaneously, simultaneously the sea-tangle that cuts is put into still.
Start stirring, speed is 100r/min, temperature is raised to 50 ℃, observe and stir moment of torsion, 1.1 after hour mixing speed is reduced to 65r/min, after 2.5 hours mixing speed is reduced to 25r/min, stop after being cooled to 30 ℃ after 3.0 hours stirring, leave standstill, vacuumizing and defoaming 2.5 hours, vacuum pressure 100Pa.
In still, lead to nitrogen, pressurization 0.6MPa, bleeder valve, booster pump are sent material into filter at the bottom of the unlatching still, and using the aperture is that 1000 purpose filter mediums filter, and the filtrate that filtration obtains directly enters spinning pump and carries out spinning.
The filter liquor concentration 62% that obtains, viscosity is 2800mPaS, adjusts 32 ℃ of temperature, and the spinning jet used aperture of spinning is 0.05mm, calcium chloride water is as coagulating bath, concentration is 3.5%, and setting time is 180 seconds, jet stretch 25%, nascent tow is derived 2.0 times of first break draft with 10m/min speed, oil agent, 85 ℃ be crosslinked down, dry 40 minutes, cut off obtaining filament number 1.46d, the alginate fibre of intensity 3.83g/d.
Embodiment 16
Other operations of present embodiment are identical with embodiment 13, and just crosslinking agent is a toluene di-isocyanate(TDI), and the filament number of preparation is 2.15d, intensity 3.75g/d.
Embodiment 17
Present embodiment is identical with embodiment 13, and just crosslinking agent changes into and joining in the coagulating bath.The filament number of preparation is 1.93d, intensity 3.76g/d.
The present invention also provides following test example, so that the present invention will be further described:
Test example 1
This test example has been investigated the fiber quality difference of the alginate fibre of the inventive method preparation with the art methods preparation:
Annotate: 5,6 data list of references patents 200710106864.1.
Wherein 1 is embodiment 1 product, and 2 is embodiment 6 products, and 3 is embodiment 15 products, and 4 is embodiment
17 products, 5,6 is prior art products, just according to prior art, such as after the method for patent application 01115139 prepares alginate, becomes alginate fibre with the alginate for the raw material spinning process again.
As can be known from the above table, the properties of product of the present invention preparation basic near in addition reached the performance of prior art products.
Test example 2
This test example has been investigated the influence of dosage of crosslinking agent for product, specifically carries out according to the operation of embodiment 1.
| Dosage of crosslinking agent | Adding opportunity | Fracture strength (g/d) | Ultimate strength CV | Elongation at break | Elongation at break CV | |
| ?1 | ??250g | Digestion | ?3.92 | ??9.1％ | ??1.8％ | ??9.6％ |
| ?2 | ??375g | Digestion | ?3.90 | ??10.8％ | ??2.1％ | ??4.6％ |
| ?3 | ??125g | Digestion | ?3.22 | ??20.1％ | ??2.1％ | ??5.2％ |
| ?4 | ??100g | Digestion | ?2.57 | ??10.6％ | ??4.5％ | ??5.9％ |
| ?5 | ??250g | Coagulating bath | ?2.97 | ??12.7％ | ??3.9％ | ??10.2％ |
| ?6 | ??250g | Oil agent | ?3.01 | ??11.9％ | ??4.7％ | ??9.7％ |
Last table is prepared for the parameter according to embodiment 1, has just adjusted dosage of crosslinking agent and adding opportunity, and this test example illustrates that dosage of crosslinking agent in technical scheme scope of the present invention, can further improve the performance of product.From data such as fracture strength, ultimate strength CV, elongation at break, elongation at break CV all as can be seen, the properties of product of technical solution of the present invention preparation have more advantage, and wherein, institute's optimized technical scheme effect is better.Simultaneously, the crosslinking agent adding also has certain influence for properties of product opportunity, and is fashionable when adding in digestion process, because the digestive juice volume is bigger, and the marine alga raw material soaking wherein, and crosslinking agent can be dispersed in marine alga raw material surface more uniformly.And more deep contact marine alga like this can be so that cross-linking reaction thereafter be more abundant, and for to reach under the product prerequisite of equal quality, dosage of crosslinking agent that is to say that still less when dosage of crosslinking agent was identical, properties of product had further lifting.Yet it should be noted that dosage of crosslinking agent and adding are not the sufficient and necessary condition that the object of the invention realizes opportunity.From last table data, as can be known,, perhaps add and change to some extent opportunity, can prepare the alginate fibre approaching equally with the prior art products performance even if dosage of crosslinking agent is not in the technical solution of the present invention scope.
Claims (10)
1. the preparation method of an alginate fibre is characterized in that, described method comprises: the marine alga raw material is after pre-treatment, join in the digestive juice and digest, postdigestive solution filters, and filtrate is carried out spinning as spinning solution, and adds crosslinking agent in digestion process or spinning process.
2. preparation method according to claim 1 is characterized in that, described crosslinking agent is one or several any mixing in chloropropylene oxide, borax, toluene di-isocyanate(TDI) or the twain-aldehyde compound compound, is preferably glutaraldehyde or glyoxal; Described dosage of crosslinking agent is 1/4～3/4 of a marine alga raw material weight, is preferably 1/2.
3. preparation method according to claim 1 is characterized in that, described pre-treatment is shredded then for the marine alga raw material is soaked.
4. preparation method according to claim 1 is characterized in that described digestive juice is a carbonate aqueous solution, is preferably one or more any mixing in sodium carbonate, potash or the carbonic hydroammonium, more preferably sodium carbonate; Described digestive juice concentration is 5%～25%, is preferably 15%～20%; Described digestive juice is 0.5: 1～5: 1 with marine alga raw material weight ratio, is preferably 1: 1～3: 1; More preferably 2: 1.
5. preparation method according to claim 1 is characterized in that, described digestion is stirred for joining in the digestive juice through the marine alga raw material of pre-treatment, heats up, and leaves standstill after the insulation reaction, and vacuumizing and defoaming both got then.
6. preparation method according to claim 4 is characterized in that described mixing speed is 80～120rpm, is preferably 100rpm; Described intensification is for being warming up to 40～60 ℃, be preferably 50 ℃, described insulation reaction reduces mixing speed to 55～65rpm for heat up finishing after 0.5～1.5h is stirred in the back, reduces mixing speed to 25～35rpm after stirring 1.5～2.5h again, is cooled to 30～40 ℃ after stirring 2.5～3.5h; Being preferably and heat up finishing to reduce mixing speed to 60rpm after 1h is stirred in the back, reducing mixing speed to 30rpm after stirring 2h again, being cooled to 35 ℃ after stirring 3h.
7. preparation method according to claim 4 is characterized in that, described vacuumizing and defoaming is deaeration 1.5～2.5h under pressure 100～1000Pa, is preferably deaeration 2h under 400～700Pa.
8. preparation method according to claim 1 is characterized in that described filter liquor concentration is weight percentage 10～65%, 30～85 ℃ of temperature, viscosity 800～3000mPaS, preferred concentration are weight percentage 30～50%, 50～65 ℃ of temperature, viscosity 1000～2000mPaS.
9. preparation method according to claim 1 is characterized in that, described spinning for use spinnerets spray silk, solidify after-drawing, oil agent, crosslinked back drying both alginate fibre.
10. preparation method according to claim 9 is characterized in that, described crosslinked be 40～120 ℃ of down dry 5～40min, be preferably 60～100 ℃ of down dry 10～20min, more preferably 80 ℃ of dry 10min down.
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Address after: 100025 Beijing city Chaoyang District street, No. 3 Yan Jing Li Patentee after: China Textile Academy Address before: 100025 Beijing city Chaoyang District street, No. 3 Yan Jing Li Patentee before: CHINA TEXTILE ACADEMY |