CN107268095A - A kind of selenium-rich fiber producing processes - Google Patents
A kind of selenium-rich fiber producing processes Download PDFInfo
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- CN107268095A CN107268095A CN201610213337.XA CN201610213337A CN107268095A CN 107268095 A CN107268095 A CN 107268095A CN 201610213337 A CN201610213337 A CN 201610213337A CN 107268095 A CN107268095 A CN 107268095A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
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Abstract
A kind of method for preparing selenium-rich fiber, comprises the following steps：It is included in during plant pulp prepares cellulose fibre and adds organism containing selenium, obtains selenium-rich fiber.Selenium-rich fiber producing processes are simple, it is easily controlled, and the fiber prepared by this method is viscose rayon, its sucting wet air permeability is good, long with personal contact's time available for underwear or bedding, Organic Selenium can be absorbed through personal skin during personal skin metabolism, security is good, and utilization rate is high.
Description
Technical field
The present invention relates to a kind of preparation method of multifunctional fibre, specifically, being related to a kind of preparation method of selenium-rich fiber.
Background technology
Selenium is referred to as " king of anticancer " in body trace element by scientist, and scientific circles' research is found, blood selenium level
Height and the generation of cancer are closely bound up.The height of Se content in substantial amounts of survey data explanation, regional a food and soil
There is direct relation with the incidence of disease of cancer, for example：Se content in this regional food and soil is high, the incidence of disease of cancer
It is just low with the death rate, conversely, this regional cancer morbidity and the death rate are just high, the generation of fact explanation selenium and cancer
Close relation.It is in body trace element " king of anticancer " that scientific circles, which also identify selenium, simultaneously.It can strengthen and exempt from
Epidemic disease power, prevent diabetes, prevent cataract, prevent cardiovascular and cerebrovascular disease, prevent Keshan disease, Kaschin-Beck disease, arthritis,
Removing toxic substances, toxin expelling, prevent and treat hepatopathy, protection liver.
Selenium is divided into two kinds in the existing way of nature:Inorganic selenium and Organic Selenium.Inorganic selenium refers generally to sodium selenite and selenic acid
Sodium, is obtained from the byproduct of metal mineral reserves.The latter is that selenium is combined into by bioconversion with amino acid, typically with selenium
The form presence of methionine, follows Methionine metabolism approach to be metabolized, participates in the synthesis of albumen, easily stored in tissue,
Absorb；It can be rapidly immediately used by the body after being absorbed by the body, be effectively improved blood in human body in selenium situation.Scientific investigations showed that, have
Machine Se accumulation is on amino acid, protein equimolecular, compared with the inorganic seleniums such as sodium selenite, selenium malt have edible safety,
Have no toxic side effect, absorption rate is high, the advantages of be of high nutritive value.The absorption and utilization of inorganic selenium are less desirable, its
Biological effectiveness is low, and toxicity is larger, and scope is small between dosis toxica and requirement, thus is strictly limited its usage amount.
In existing selenium-rich fiber production technology, be nanometer selenium or selenium compound addition fiber production process in, from
And using fiber to contain selenium element, this selenium is inorganic selenium, there is certain bio-toxicity, and utilization rate is low.Such as：It is Chinese special
Profit application discloses CN 102586950A and discloses a kind of method for preparing zinc selenide nanofiber, and invention is using double crucibles
Method, electrostatic spinning technique is combined with selenization technology, is prepared for ZnSe nanofibers.Invention includes three steps：
(1) spinning solution is prepared.By Zn (NO3)2·6H2O and PVP, is added in DMF solvent, forms spinning solution；
(2) ZnO nano fiber is prepared.PVP/Zn (NO are prepared using electrostatic spinning technique3)2Composite nano fiber, then
Progress is thermally treated resulting in ZnO nano fiber；(3) ZnSe nanofibers are prepared.
It is added in the prior art using inorganic selenium powder in spinning solution and carries out spinning, is prepared into the fiber containing selenium.
But this method uses inorganic selenium compound, it is unfavorable for the security of fiber, and the spinning property of fiber is poor.
Therefore, proposing the present invention.
The content of the invention
The purpose of one aspect of the present invention provides a kind of preparation method of selenium-rich fiber, using the preparation method, it is to avoid use
Inorganic methyl seleninic acid, and use through plant or microorganism, the Organic Selenium of mushroom conversion, be conducive to the security of fiber
With the utilization rate of selenium.
The purpose of another aspect of the present invention provides a kind of preparation method of selenium-rich fiber, and prepared by this method is rich in selenium fiber
Spinning property is good, fault is largely reduced.
A kind of preparation method of selenium-rich fiber of the present invention, is included in during plant pulp prepares cellulose fibre and adds
The body of Organic Selenium containing selenium, obtains selenium-rich fiber.
On the one hand, a kind of preparation method of selenium-rich fiber, comprises the following steps：
(1) preparation of Organic Selenium extract solution:Selenium organism will be contained to be added in sodium hydroxide solution, impregnated at normal temperatures,
After dipping, take its extract solution to be filtered, obtain Organic Selenium extract solution；
(2) Organic Selenium extract solution is added during plant pulp prepares cellulose fibre, selenium-rich fiber is obtained.
On the other hand, a kind of preparation method of selenium-rich fiber, comprises the following steps：
(A) processing of the organism containing selenium:The organism containing selenium of solid-state is mixed with water, and is ground to particle diameter less than 10um, warp
Cross screening or filter, obtain the slurry of organism containing selenium；
(B) slurry of organism containing selenium that step (A) is obtained is added during plant pulp prepares cellulose fibre,
Obtain selenium-rich fiber.
Generally, plant pulp is prepared into the process of cellulose fibre and included, plant pulp is first soaked through alkali, yellow, dissolving with
And filter process, the spinning solution after filtering obtains tow after spinning, and tow can obtain cellulose after subsequent treatment
Fiber.
In the embodiment of the application, the described extract solution of organism containing selenium is in the leaching of plant pulp alkali or course of dissolution
Add, can also be added in spinning solution.It is preferred that, the described extract solution of organism containing selenium is in course of dissolution or spinning
Added in stoste.
In another embodiment herein, the described slurry of organism containing selenium is added in plant pulp course of dissolution,
It can also be added in spinning solution.It is preferred that, the described slurry of organism containing selenium is added in spinning solution.
In this application, organism containing selenium is added in cellulose fibre preparation process, after mixing viscose glue made from spinning
Fiber, spinning property is good, and its fibre defect is substantially reduced.
Technical scheme is described in further detail below.
On the one hand, a kind of preparation method of selenium-rich fiber, can use following steps：
(1) preparation of Organic Selenium extract solution:Selenium organism will be contained to be added in sodium hydroxide solution, impregnated at normal temperatures,
After dipping, its extract solution is taken to be filtered, i.e. to obtain Organic Selenium extract solution；
(2) Organic Selenium extract solution is added during plant pulp prepares cellulose fibre, selenium-rich fiber is obtained.
On the other hand, a kind of preparation method of selenium-rich fiber, comprises the following steps：
(A) processing of the organism containing selenium:The organism containing selenium of solid-state is mixed with water, and is ground to particle diameter less than 10um, warp
Cross screening or filter, obtain the slurry of organism containing selenium；
(B) slurry of organism containing selenium that step (A) is obtained during plant pulp prepares cellulose fibre, is obtained
Selenium-rich fiber.
In one embodiment, in organism containing selenium the content containing selenium in more than 1500ppm.
In one embodiment, in step (1), the concentration of sodium hydroxide solution is 1-50g/L, preferably 10-20g/L.
In one embodiment, in step (1), organism containing selenium impregnates 10-90 at normal temperatures in sodium hydroxide solution
Minute.
In some embodiments, in step (1), the amount ratio 1 of organism containing selenium and sodium hydroxide solution：2-40kg/L,
It is preferred that 1：20-40kg/L.
In some embodiments, in step (A), the concentration of the slurry of organism containing selenium grinding is 5-20%.
In some embodiments, described organism containing selenium includes Se-enriched yeast, product containing organic selenium.
In this application, plant pulp is typically to be prepared from by plant material by boiling, and digestion process steams including alkaline process
Boil, kraft cooking and/or sulfite cooking process.
In this application, described alkaline cooking, kraft cooking and/or sulfite cooking process use existing skill
The conventional method of art.
Described plant pulp includes but is not limited to grass kind plant pulp, wood pulps, bamboo pulp, hemp dissolving pulp or Cotton Pulp
Deng one kind or its two or more mixing；It is preferred that, described plant pulp includes wood pulps, bamboo pulp, hemp dissolving pulp
Or one kind of Cotton Pulp or its two or more mixing.
In some embodiments, described organism containing selenium extract solution is added in the leaching of plant pulp alkali or course of dissolution,
It can also be added in spinning solution.
In some embodiments, described organism containing selenium extract solution adds in plant pulp course of dissolution or spinning solution
Enter；It is preferred that, the described extract solution of organism containing selenium is added in spinning solution.
In some embodiments, the slurry of organism containing selenium is added during plant pulp dissolves, can also be former in spinning
Added in liquid.
It is preferred that, the described slurry of organism containing selenium is added in spinning solution.
In one embodiment, the extract solution of organism containing selenium that is added during plant pulp prepares cellulose fibre or
In slurry, the addition of Organic Selenium is the 2-500ppm of alpha cellulose weight in plant pulp；It is preferred that, 5-100ppm
。
In some embodiments, during the extract solution of organism containing selenium or the slurry of organism containing selenium are mixed with spinning solution, keep
The temperature control of mixture when it is mixed is at 17-50 DEG C, and preferable temperature is controlled at 25-30 DEG C.
Organism containing selenium is with the addition of before cellulose fiber spinning, the extract solution of organism containing selenium is especially added so that obtain
Fiber spinnability it is more preferable.Meanwhile, inventor is found surprisingly that, compared to not adding the fibre that the body spinning of Organic Selenium containing selenium is obtained
For dimension, its product fault declines more.Analyzing its reason may be, Organic Selenium extract solution or Organic Selenium carrier (contain selenium
Organism) certain or Cucumber acted on yellow sulfur byproduct species, generate a kind of chelate, this chelate is covered in
Nascent fibre surface, forms one layer of pellicle, and the pellicle is conducive to the solvent in as-spun fibre to deviate to enter coagulating bath, from
And being conducive to the shaping of fiber, fiber is not easy to be pulled off when going out coagulating bath, is difficult to form blob of viscose, so as to reduce fault
。
Vegetable slurries of the present invention refer to dissolving after plant pulp yellow and obtain the spinning original after slurries, or dissolving, filtering
Liquid, or formation slurries during alkali leaching.
The plant pulp performance that the present invention is used meets People's Republic of China (PRC) textile industry standard FZ/T 51001-2009,
FZ/T 51002-2006。
The assay method of selenium-rich fiber Se content of the present invention is National Standard of the People's Republic of China GB/T30157.
The plant pulp of the present invention can be prepared from by all pulping process disclosed in prior art.
Generally, in the preparation process of plant pulp, using plant as raw material, prepared through processes such as boiling, bleaching, acid treatments
Obtain plant pulp.
In this application, during plant pulp prepares cellulose fibre, except adding the extract solution of organism containing selenium or containing
Outside selenium organism slurry, other technical process and technological parameter can use method disclosed in prior art.
In this application, it is preferred that the method that plant pulp prepares cellulose fibre includes following process：Dipping, it is experienced
, yellow, dissolving, spinning, refining, the process such as drying.
Described dipping includes, and plant pulp is impregnated in temperature is 30-50 DEG C of aqueous slkali.
Further, squeezing is also included between impregnating and be experienced, is crushed, is conventionally handled.
The described experienced progress in experienced drum, control temperature is at 15-60 DEG C.
In described yellowing processes, the addition of carbon disulfide is the 25-45wt% of alpha cellulose weight.
Further, in yellowing processes, yellow temperature is 25-35 DEG C.
What the present invention was added is organism containing selenium, is through the inverted Organic Selenium such as plant or microorganism, mushroom.This hair
The selenium-rich fiber producing processes of bright offer are simple, are easily controlled, and the fiber prepared by this method is viscose rayon,
Fiber spinnability, its product fault declines, and its sucting wet air permeability is good, available for underwear or bedding, with personal contact
Time is long, and Organic Selenium can be absorbed through personal pore during personal skin metabolism, and security is good, and utilization rate is high.
Embodiment
A kind of selenium-rich fiber producing processes of the present invention are described in further detail below, the protection model of the present invention is not limited
Enclose, its protection domain is defined with claims.Some disclosed details provide complete to each disclosed embodiment
Foliation solution.However, those skilled in the relevant art know, one or more of these concrete details are not used, and are used
The situation of other materials etc. can also realize embodiment.
Or " another embodiment " throughout the specification mentioned " embodiment ", or " embodiment ",
Or " some embodiments " refers to that the feature that is related to related to the embodiment or structure are included at least one
In individual embodiment." embodiment " occurred in specification, or " embodiment ", or " another embodiment "
Or " some embodiments " is unnecessary refers both to identical embodiment.
Using wood pulps, bamboo pulp or Cotton Pulp it is respectively a batch in all embodiments in following specific embodiments
Production, respective performance parameter is identical.
Definition：
In the application, described organism containing selenium refers to that selenium is combined by the conversion such as plant or microorganism, mushroom with amino acid
Form.For example, organism containing selenium includes " Se-enriched yeast or product containing organic selenium ", typically refers in the incubation of yeast
The inorganic selenium of the forms such as sodium selenite is added, it is converted into Organic Selenium, and enrichment forms one obtained in Se-enriched yeast
Plant microbial fermentation product.Can be from directly commercially Se-enriched yeast, for example Angel Yeast Co., Ltd gives birth to
The Se-enriched yeast of production.Or the published method of prior art prepares Se-enriched yeast, for example, disclose the with reference to Chinese patent
Embodiment 1 or 2 in Se-enriched yeast and preparation method thereof disclosed in CN103911299A prepares Se-enriched yeast.
The type of barms, fermentation culture, zymotechnique etc. in this application, the use on the application do not influence.
As long as the amount containing selenium in Se-enriched yeast reaches to a certain degree.
In this application, term " normal temperature " is to be often referred to temperature at 10-30 DEG C.
" ppm " represents the content of certain in material or some compositions in this application, is expressed as a few millionths.
Further below with specific example in detail technical scheme.
Embodiment 1
1) preparation of the extract solution of organism containing selenium
1000g Se-enriched yeasts (buying in Angel Yeast Co., Ltd) are added to 40L 20g/L sodium hydroxides
In solution, the content of selenium element is 2200ppm in Se-enriched yeast, impregnates 30 minutes at normal temperatures, after dipping, takes it to carry
Take liquid to be filtered, obtain Organic Selenium extract solution；
2) preparation of cellulose fibre
Wood pulps impregnate in sodium hydroxide solution, and the concentration of sodium hydroxide solution is 210g/L；Pulp after impregnation process
Through squeezing, crush, experienced, yellow, in yellowing processes, the addition of carbon disulfide is the 32wt% of alpha cellulose weight
, yellow temperature is 30 DEG C；
Wood pulp after yellow is dissolved, and the Organic Selenium extract solution of step (1) is added in course of dissolution, wherein, contain
The addition of Organic Selenium accounts for the 20ppm of alpha cellulose weight in viscose, Organic Selenium extract solution in selenium organism extract solution
Mixed 30 minutes for 30 DEG C in temperature with viscose progress；Wood pulp after dissolving is by filtering, and the glue after filtering passes through spinning
Tow is obtained, acid bath composition is：Acid bath is constituted：Sulfuric acid 100g/L, sodium sulphate 315g/L, zinc sulfate 10.0g/L, spin
Silk speed is 50m/min, and tow can obtain the cellulose fibre that Se content is 5ppm after subsequent treatment.
Embodiment 2
1) preparation of the extract solution of organism containing selenium
500g product containing organic seleniums are added in 10L 10g/L sodium hydroxide solutions, the content of selenium element is in Se-enriched yeast
2200ppm, impregnates 90 minutes, after dipping, takes its extract solution to be filtered, obtain Organic Selenium extract solution at normal temperatures；
2) preparation of cellulose fibre
Wood pulps impregnate in sodium hydroxide solution, and the concentration of sodium hydroxide solution is 240g/L；Pulp after impregnation process
Through squeezing, crush, experienced, yellow, in yellowing processes, the addition of carbon disulfide is the 32wt% of alpha cellulose weight
, yellow temperature is 25 DEG C, and the wood pulp after yellow is dissolved, and the wood pulp after dissolving is by filtering；
Organic Selenium extract solution is added in spinning solution after filtration, wherein, Organic Selenium adds in the extract solution of organism containing selenium
Enter the 20ppm that amount accounts for alpha cellulose weight in viscose, Organic Selenium extract solution is mixed for 35 DEG C with viscose progress in temperature
, it is sufficiently mixed, glue obtains tow by spinning, acid bath composition is：Sulfuric acid 90.g/L, sodium sulphate 315g/L, zinc sulfate
10.2g/L, spinning speed is 55m/min, and tow can obtain the cellulose fibre that Se content is 5ppm after subsequent treatment
。
Embodiment 3
1) preparation of the extract solution of organism containing selenium
The 20g/L sodium hydroxides that 500g Se-enriched yeasts (buying in Angel Yeast Co., Ltd) are added into 10L are molten
In liquid, the content of selenium element is 2200ppm in Se-enriched yeast, impregnates 50 minutes at normal temperatures, after dipping, takes it to extract
Liquid is filtered, and obtains Organic Selenium extract solution；
2) preparation of cellulose fibre
Wood pulps impregnate in sodium hydroxide solution, and the concentration of sodium hydroxide solution is 240g/L；Pulp after impregnation process
Through squeezing, crush, experienced, yellow, in yellowing processes, the addition of carbon disulfide is the 25wt% of alpha cellulose weight
, yellow temperature is 25 DEG C, and the wood pulp after yellow is dissolved, and the wood pulp after dissolving is by filtering；
Organic Selenium extract solution is added in spinning solution after filtration, wherein, Organic Selenium adds in the extract solution of organism containing selenium
Enter the 10ppm that amount accounts for alpha cellulose weight in viscose, Organic Selenium extract solution is mixed for 35 DEG C with viscose progress in temperature
, it is sufficiently mixed, glue obtains tow by spinning, acid bath composition is：Sulfuric acid 90.g/L, sodium sulphate 307g/L, zinc sulfate
14.2g/L, spinning speed is 55m/min, and tow can obtain the cellulose fibre that Se content is 3ppm after subsequent treatment
。
Embodiment 4
1) preparation of the extract solution of organism containing selenium
The 20g/L sodium hydroxides that 500g Se-enriched yeasts (buying in Angel Yeast Co., Ltd) are added into 10L are molten
In liquid, the content of selenium element is 2200ppm in Se-enriched yeast, impregnates 45 minutes at normal temperatures, after dipping, takes it to extract
Liquid is filtered, and obtains Organic Selenium extract solution；
2) preparation of cellulose fibre
Wood pulps impregnate in the sodium hydroxide solution of 35 DEG C of temperature, and the concentration of sodium hydroxide solution is 240g/L；At dipping
Pulp after reason through squeezing, crush, experienced, yellow, in yellowing processes, the addition of carbon disulfide is alpha cellulose
The 31wt% of weight, yellow temperature is 30 DEG C；
Wood pulp after yellow is dissolved, and the Organic Selenium extract solution of step (1) is added in course of dissolution, wherein, contain
The addition of Organic Selenium accounts for the 100ppm of alpha cellulose weight in viscose, Organic Selenium extract solution in selenium organism extract solution
Mixed 60 minutes for 15 DEG C in temperature with viscose progress；Wood pulp after dissolving is by filtering, and the glue after filtering passes through spinning
Tow is obtained, acid bath composition is：Acid bath is constituted：Sulfuric acid 98g/L, sodium sulphate 320g/L, zinc sulfate 12.5g/L, spinning
Speed is 50m/min, and tow can obtain the cellulose fibre that Se content is 27ppm after subsequent treatment.
Embodiment 5
1) preparation of the extract solution of organism containing selenium
The 20g/L sodium hydroxides that 500g Se-enriched yeasts (buying in Angel Yeast Co., Ltd) are added into 12L are molten
In liquid, the content of selenium element is 2200ppm in Se-enriched yeast, impregnates 30 minutes at normal temperatures, after dipping, takes it to extract
Liquid is filtered, and obtains Organic Selenium extract solution；
2) preparation of cellulose fibre
Wood pulps impregnate in sodium hydroxide solution, and the concentration of sodium hydroxide solution is 240g/L；Pulp after impregnation process
Through squeezing, crush, experienced, yellow, in yellowing processes, the addition of carbon disulfide is the 30wt% of alpha cellulose weight
, yellow temperature is 25 DEG C；
Wood pulp after yellow is dissolved, and the Organic Selenium extract solution of step (1) is added in course of dissolution, wherein, contain
The addition of Organic Selenium accounts for the 100ppm of alpha cellulose weight in viscose in selenium organism extract solution, and organism containing selenium is carried
Liquid is taken to be mixed 30 minutes for 30 DEG C in temperature with viscose progress；Wood pulp after dissolving is by filtering, and the glue after filtering passes through
Spinning obtains tow, and acid bath composition is：Acid bath is constituted：Sulfuric acid 130g/L, sodium sulphate 280g/L, zinc sulfate 13.4g/L
, spinning speed is 50m/min, and tow can obtain the cellulose fibre that Se content is 26ppm after subsequent treatment.
Embodiment 6
1) preparation of the extract solution of organism containing selenium
500g product containing organic seleniums are added in 12L 20g/L sodium hydroxide solutions, the content of selenium element is in Se-enriched yeast
2200ppm, impregnates 20 minutes, after dipping, takes its extract solution to be filtered, obtain Organic Selenium extract solution at normal temperatures；
2) preparation of cellulose fibre
Wood pulps impregnate in temperature is 40 DEG C of sodium hydroxide solution, and the concentration of sodium hydroxide solution is 240g/L, and is added
Enter step 1) Organic Selenium extract solution, wherein, the addition of Organic Selenium accounts for first kind in viscose in the extract solution of organism containing selenium
The 50ppm of cellulose；Pulp after impregnation process through squeezing, crush, experienced, yellow, in yellowing processes, two
The addition of nitric sulfid is the 30wt% of alpha cellulose weight, and yellow temperature is 25 DEG C；Wood pulp after yellow is dissolved
, the wood pulp after dissolving is by filtering, and the glue after filtering obtains tow by spinning, and acid bath composition is：Acid bath is constituted
：Sulfuric acid 125g/L, sodium sulphate 315g/L, zinc sulfate 10.4g/L, spinning speed is 50m/min, and tow is after subsequent treatment
It can obtain the cellulose fibre that Se content is 14ppm.
Embodiment 7
1) preparation of the extract solution of organism containing selenium
The 20g/L sodium hydroxides that 500g Se-enriched yeasts (buying in Angel Yeast Co., Ltd) are added into 15L are molten
In liquid, the content of selenium element is 2200ppm in Se-enriched yeast, impregnates 30 minutes at normal temperatures, after dipping, takes it to extract
Liquid is filtered, and obtains Organic Selenium extract solution；
2) preparation of cellulose fibre
Wood pulps impregnate in sodium hydroxide solution, and the concentration of sodium hydroxide solution is 240g/L；Pulp after impregnation process
Through squeezing, crush, experienced, yellow, in yellowing processes, the addition of carbon disulfide is the 30wt% of alpha cellulose weight
, yellow temperature is 35 DEG C；
Wood pulp after yellow is dissolved, and the Organic Selenium extract solution of step (1) is added in course of dissolution, wherein, contain
The addition of Organic Selenium accounts for the 70ppm of alpha cellulose weight in viscose, Organic Selenium extract solution in selenium organism extract solution
Mixed 30 minutes for 25 DEG C in temperature with viscose progress；Wood pulp after dissolving is by filtering, and the glue after filtering passes through spinning
Tow is obtained, acid bath composition is：Acid bath is constituted：Sulfuric acid 110g/L, sodium sulphate 290g/L, zinc sulfate 10.5g/L, spin
Silk speed is 50m/min, and tow can obtain the cellulose fibre that Se content is 18ppm after subsequent treatment.
Embodiment 8
1) processing of the organism containing selenium
500g Se-enriched yeasts (buying in Angel Yeast Co., Ltd) are added in 9.5L pure water, selenium-rich ferment
The content of selenium element is 2200ppm in mother, is ground to form at normal temperatures using sand mill less than 10um particle diameters, by 10um
Membrane filtration, obtains the slurry of organism containing selenium that content is 5%；
2) preparation of cellulose fibre
Wood pulps impregnate in sodium hydroxide solution, and the concentration of sodium hydroxide solution is 240g/L；Pulp after impregnation process
Through squeezing, crush, experienced, yellow, in yellowing processes, the addition of carbon disulfide is the 30wt% of alpha cellulose weight
, yellow temperature is 35 DEG C；
Wood pulp after yellow is dissolved, and the slurry of organism containing selenium of step (1) is added in course of dissolution, wherein,
The addition of Organic Selenium accounts for the 100ppm of alpha cellulose weight in viscose in the slurry of organism containing selenium, organism containing selenium with
Viscose is carried out in the mixing 30 minutes of 25 DEG C of temperature；Wood pulp after dissolving is by filtering, and the glue after filtering passes through spinning
Tow is obtained, acid bath composition is：Acid bath is constituted：Sulfuric acid 110g/L, sodium sulphate 315g/L, zinc sulfate 11.5g/L,
Spinning speed is 50m/min, and tow can obtain the cellulose fibre that Se content is 40ppm after subsequent treatment.
Comparative example 1
This experimental example is to adding the extract solution of organism containing selenium and the slurry of organism containing selenium, with being not added with obtaining prepared by organism containing selenium
To the performance of cellulose fibre contrasted.
Comparative example 1 is without organism containing selenium is added in preparation process, and its preparation method reference implementation example 1 eliminates implementation
The step of making of the organism containing selenium of example 1, and the step of second step addition body of Organic Selenium containing selenium, other processing steps
And technological parameter reference implementation example 1；Other processing steps and technological parameter reference implementation example 1.
Test sample is the cellulose fibre that embodiment 1-8 is prepared.Its result such as see the table below.
Claims (10)
1. a kind of preparation method of selenium-rich fiber, is included in during plant pulp prepares cellulose fibre and adds organism containing selenium, obtain selenium-rich fiber.
2. preparation method according to claim 1, comprises the following steps：
(1) preparation of Organic Selenium extract solution:Selenium organism will be contained to be added in sodium hydroxide solution, impregnated at normal temperatures, after dipping, take its extract solution to be filtered, obtain Organic Selenium extract solution；
(2) Organic Selenium extract solution is added during plant pulp prepares cellulose fibre, selenium-rich fiber is obtained.
Or, comprise the following steps：
(A) processing of the organism containing selenium:The organism containing selenium of solid-state is mixed with water, and is ground to particle diameter less than 10um, by screening or filtering, obtains the slurry of organism containing selenium；
(B) slurry of organism containing selenium that step (A) is obtained is added during plant pulp prepares cellulose fibre, selenium-rich fiber is obtained.
3. preparation method according to claim 2, it is characterised in that in step (1), the concentration of sodium hydroxide solution is 1-50g/L, preferably 10-20g/L.
4. the preparation method according to claim any one of 2-3, it is characterised in that in step (1), the amount ratio 1 of organism containing selenium and sodium hydroxide solution：2-40kg/L, it is preferable that 1：20-40kg/L；
Or, in step (A), the concentration of the slurry of organism containing selenium grinding is 5-20%.
5. the preparation method according to claim any one of 2-4, it is characterised in that the described extract solution of organism containing selenium is added in the leaching of plant pulp alkali or course of dissolution, or is added in spinning solution；
It is preferred that, the described extract solution of organism containing selenium is added in plant pulp course of dissolution or spinning solution；It is furthermore preferred that the described extract solution of organism containing selenium is added in spinning solution.
6. the preparation method according to claim any one of 2-4, it is characterised in that the slurry of organism containing selenium is added during plant pulp dissolves, or is added in spinning solution；
It is preferred that, the described slurry of organism containing selenium is added in spinning solution.
7. the preparation method according to claim 5 or 6, it is characterised in that in the extract solution of organism containing selenium or slurry added during plant pulp prepares cellulose fibre, the addition of Organic Selenium is the 2-500ppm of alpha cellulose weight in plant pulp；It is preferred that, 5-100ppm.
8. the preparation method according to any one of claim 1 or 6, it is characterised in that when the extract solution of organism containing selenium or the slurry of organism containing selenium are mixed with spinning solution, the temperature control of mixture is at 17-50 DEG C, and preferable temperature is controlled at 25-30 DEG C.
9. preparation method according to claim 1, it is characterised in that described plant pulp includes but is not limited to one kind or its two or more mixing of grass kind plant pulp, wood pulps, bamboo pulp, hemp dissolving pulp or Cotton Pulp etc.；It is preferred that, described plant pulp includes wood pulps, bamboo pulp, hemp dissolving pulp or one kind of Cotton Pulp or its two or more mixing；
Described organism containing selenium includes Se-enriched yeast, product containing organic selenium.
10. the cellulose fibre that a kind of preparation method of any one of claim 1-9 selenium-rich fiber is prepared from, Se content is more than 0.5ppm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610213337.XA CN107268095B (en) | 2016-04-07 | 2016-04-07 | A kind of selenium-rich fiber producing processes |
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|---|---|---|---|
| CN201610213337.XA CN107268095B (en) | 2016-04-07 | 2016-04-07 | A kind of selenium-rich fiber producing processes |
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| CN107268095A true CN107268095A (en) | 2017-10-20 |
| CN107268095B CN107268095B (en) | 2019-10-29 |
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| CN108754655A (en) * | 2018-05-30 | 2018-11-06 | 景洪丽 | The preparation method of nanometer selenium regenerated celulose fibre |
| CN112795992A (en) * | 2020-12-30 | 2021-05-14 | 福建恒益纺织有限公司 | Selenium-containing regenerated fiber skin-care antibacterial multifunctional fabric and preparation method thereof |
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| CN1641079A (en) * | 2003-03-06 | 2005-07-20 | 王开利 | Nano selenium trace element fiber |
| CN101703319A (en) * | 2009-09-25 | 2010-05-12 | 成钢 | Wool fibre fabric sweat shirt (pants) with functions of powerful antibiosis, cancer prevention and life prolonging by utilizing nano silver, selenium and germanium |
| KR20110015319A (en) * | 2009-08-07 | 2011-02-15 | 나노폴리(주) | Method for manufacturing multi-functional fabric with antimicrobial and far-infrared ray radition function |
| CN102550795A (en) * | 2011-12-26 | 2012-07-11 | 苏州硒谷科技有限公司 | Method for extracting selenium-containing protein from selenium-enriched yeast |
| CN105019050A (en) * | 2014-04-30 | 2015-11-04 | 上海水星家用纺织品股份有限公司 | Method for preparing selenium-enriched fiber |
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| CN1641079A (en) * | 2003-03-06 | 2005-07-20 | 王开利 | Nano selenium trace element fiber |
| KR20110015319A (en) * | 2009-08-07 | 2011-02-15 | 나노폴리(주) | Method for manufacturing multi-functional fabric with antimicrobial and far-infrared ray radition function |
| CN101703319A (en) * | 2009-09-25 | 2010-05-12 | 成钢 | Wool fibre fabric sweat shirt (pants) with functions of powerful antibiosis, cancer prevention and life prolonging by utilizing nano silver, selenium and germanium |
| CN102550795A (en) * | 2011-12-26 | 2012-07-11 | 苏州硒谷科技有限公司 | Method for extracting selenium-containing protein from selenium-enriched yeast |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108754655A (en) * | 2018-05-30 | 2018-11-06 | 景洪丽 | The preparation method of nanometer selenium regenerated celulose fibre |
| CN112795992A (en) * | 2020-12-30 | 2021-05-14 | 福建恒益纺织有限公司 | Selenium-containing regenerated fiber skin-care antibacterial multifunctional fabric and preparation method thereof |
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