CN106835328B - A kind of preparation method of flame-retardant anti-bacterial fiber precursor - Google Patents
A kind of preparation method of flame-retardant anti-bacterial fiber precursor Download PDFInfo
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- CN106835328B CN106835328B CN201710105664.8A CN201710105664A CN106835328B CN 106835328 B CN106835328 B CN 106835328B CN 201710105664 A CN201710105664 A CN 201710105664A CN 106835328 B CN106835328 B CN 106835328B
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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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/54—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of unsaturated nitriles
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Artificial Filaments (AREA)
Abstract
The present invention relates to textile fabric manufacturing technology fields.The invention discloses a kind of preparation methods of flame-retardant anti-bacterial fiber precursor, it includes ingredient, polypropylene dissolution, antibacterial agent addition, fire retardant addition and spinning, wherein antibacterial agent is the composition of aluminum phosphate, calcium phosphate and aluminium triphosphate, and fire retardant is the composition of ammonium hydrogen carbonate, sodium bicarbonate, saleratus and diatomite.Preparation preparation method in the present invention is simple, and slightly transformation can carry out in existing production equipment, and the difficulty of upgrading is smaller；The fiber precursor that the present invention is prepared keep original acrylic fiber a little on the basis of also assign that fiber precursor is good fire-retardant and antibacterial functions.
Description
Technical field
The present invention relates to textile fabric manufacturing technology fields, more particularly, to a kind of preparation side of flame-retardant anti-bacterial fiber precursor
Method.
Background technique
Polyacrylonitrile fibre is also referred to as acrylic fibers, is the propylene of the polyacrylonitrile or acrylonitrile by mass percent greater than 85%
Lonitrile copolymer, through synthetic fibers made of dry spinning or wet spinning, the elasticity of polyacrylonitrile fibre is like wool, but warmth retention property
It is also higher than wool, while having many advantages, such as bulk, easy dye, softness, lovely luster, not being afraid of and damage by worms, it can be according to different purposes
It is required that with natural fibre blended or pure spinning, obtained textile can be widely applied to the fields such as decoration, clothes.
But since polyacrylonitrile fibre is that high polymer fiber belongs to combustible, limit oxygen index 17
~18, belong in synthetic fibers it is minimum, using being restricted to a certain extent, therefore the flame-retardant modified meaning of acrylic fibers
It is great；Meanwhile with the raising of the level of consumption, demand of the consumer to fiber functionalization is also increasing, especially resistant fiber
The demand of the functions such as bacterium performance, therefore antibacterial modified meaning is also quite great.
Summary of the invention
To solve the above problems, the present invention provides a kind of fiber precursors easily operated and obtained to have antibacterial flame-retardant function
The preparation method of the flame-retardant anti-bacterial fiber precursor of energy.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of preparation method of flame-retardant anti-bacterial fiber precursor, comprising the following steps:
A) raw material is weighed by following parts by weight: 90 parts of polyacrylonitrile, 1.5~3.5 parts of fire retardant, antibacterial agent 0.25~0.45
Part, 350~500 parts of organic solvent；
B) by polyacrylonitrile and organic solvent mixed dissolution, and strong stirring dissolves at 101~129 DEG C, mixing time
It is 601~719 minutes, spinning solution A is made；
C) antibacterial agent, and strong stirring 30~40 minutes at 96~109 DEG C are added into spinning solution A, spinning is made
Stoste B；
D) fire retardant is added thereto, spinning solution is made after agitated after certain time is cooling by spinning solution B；
E) spinning solution is transported to spinning machine, forms in coagulating bath after spinning head squeezes out, is then drawn through coagulating bath
It stretches, flame-retardant anti-bacterial fiber precursor is made in water-bath and the process that oils.
The antibacterial agent that the present invention selects all is to have inorganic phosphate salt resistant to high temperature, can resist high temperature without
Decompose, therefore, can be added in higher temperature, can either guarantee that it is not destroyed, also can guarantee its preferably with it is organic
Solvent and polyacrylonitrile fusion, do not occur segregation phenomenon；But the fractions in fire retardant, such as ammonium hydrogen carbonate and sodium bicarbonate
Belong to and meet the labile inorganic matter bicarbonate of high temperature, it is therefore desirable to be added again after solution is slightly cooling, need to select
One can either guarantee well to merge with organic principle, not decompose completely after capable of guaranteeing its addition again.
Preferably, fire retardant be 8~11wt% of ammonium hydrogen carbonate, 10~13wt% of sodium bicarbonate, 5~10wt% of saleratus,
Surplus is diatomite.
Ammonium hydrogen carbonate can decompose release carbon dioxide and ammonia after heated, and carbon dioxide and ammonia are all can not combustion gas
Body can inhibit continuing for burning after meeting open fire, play fire-retardant effect, the fire-retardant gas amount discharged after decomposing
Greatly, good flame retardation effect, there is also corresponding disadvantages for it, i.e., the ammonia of its release has irritation, though largely release ammonia
Continuing for burning can be so prevented, but can also generate certain adverse effect to consumer；Also can after sodium bicarbonate is heated
It decomposes, but it decomposes the carbon dioxide for only generating colorless and odorless, will not generate additional irritative gas；Although with bicarbonate
Ammonium is compared, and gas production is smaller, but nonirritant to the person, more friendly；Ammonium hydrogen carbonate compounded with sodium bicarbonate share for
Fire retardant, it can play the function of highly effective flame-retardant, it is also ensured that generated irritative gas can be in tolerance interval
It is interior, serious harm is not generated to the person, the addition of saleratus is mainly played synthesis Nagasaki temperature of allotment fire retardant, made
It is more wide to produce gas temperature range；Diatomite is a kind of porous silicate mineral, and the porosity having can to prepare
Obtained by fiber there is certain heat-proof quality, can more protect user meeting open fire is that will not be burnt, scald；Silicon simultaneously
Diatomaceous earth can also be used as the carrier of sodium bicarbonate and ammonium hydrogen carbonate, keep it more firm, uniform with polyacrylonitrile, Bu Huifa
Phenomena such as raw deposition.
Preferably, antibacterial agent is 20~30wt% of aluminum phosphate, 10~20wt% of calcium phosphate, surplus is aluminium triphosphate.
Preferably, organic solvent is one of dimethyl sulfoxide, n,N-Dimethylformamide, n,N-dimethylacetamide
Or a variety of mixture.
Preferably, diatomite passes through following pretreatment: diatomite in powder being first broken to 1~2 micron, then in dehydrated alcohol
It is ultrasonically treated in solution 10~600 seconds, is then ultrasonically treated 1~60 minute in saturated sodium bicarbonate solution, it is finally clear with water
It washes 4~6 times；Controlled at 50~75 DEG C when ultrasonic treatment.
Diatomite pretreatment can remove remaining organic impurities and inorganic dust in its microchannel, while in saturated carbon
Ion exchange can occur in acid sodium solution, remove heavy metal ion remaining in diatomite surface and duct, it is living simultaneously
Change the surface ion in its surface and duct, makes it have better absorption property, it can be preferably by other in fire retardant
Component is adsorbed in its surface and duct.
Preferably, spinning solution B is cooled down using 50~60 DEG C of water bath with thermostatic control in step d, after water-bath equality of temperature
Fire retardant is added thereto.
50~60 DEG C, being one can either guarantee that fire retardant is well merged with organic principle, can guarantee its addition again
Complete Undec temperature range afterwards, temperature is high may to make the fire retardant decomposed occur, and influence its performance, temperature is low
It can make it difficult to merge with organic principle again；Using the cooling method of water bath with thermostatic control, the time of cooling can be preferably controlled, and
And guarantee that temperature is not less than requirement when cooling.
Preferably, it for amount is 1.6~2.0g/min that spinning condition, which is pump, in step e, spinning head is 80~100 holes.
Therefore, it the invention has the following advantages: the preparation preparation method in the present invention is simple, is set in existing production
Standby upper slightly transformation can carry out, and the difficulty of upgrading is smaller；The fiber precursor that the present invention is prepared is keeping original nitrile
Synthetic fibre fiber a little on the basis of also assign that fiber precursor is good fire-retardant and antibacterial functions.
Specific embodiment
Further description of the technical solution of the present invention With reference to embodiment.
Obviously, the described embodiments are merely a part of the embodiments of the present invention, instead of all the embodiments.Based on this
Embodiment in invention, all other reality obtained by those of ordinary skill in the art without making creative efforts
Example is applied, shall fall within the protection scope of the present invention.
Embodiment 1
A kind of preparation method of flame-retardant anti-bacterial fiber precursor, comprising the following steps:
A) raw material is weighed by following parts by weight: 90 parts of polyacrylonitrile, 1.5 parts of fire retardant, 0.25 part of antibacterial agent, organic solvent
350 parts；Fire retardant is ammonium hydrogen carbonate 8wt%, sodium bicarbonate 10wt%, saleratus 5wt%, diatomite 77wt%；Antibacterial agent is phosphorus
Sour aluminium 20wt%, calcium phosphate 10wt%, aluminium triphosphate 70wt%；Organic solvent is dimethyl sulfoxide；
Diatomite passes through following pretreatment before addition: diatomite in powder being first broken to 1 micron, then in ethanol solution
Middle ultrasonic treatment 10 seconds, is then ultrasonically treated 1 minute in saturated sodium bicarbonate solution, finally washes with water 4 times；Ultrasonic treatment
When controlled at 50 DEG C；
B) by polyacrylonitrile and organic solvent mixed dissolution, and strong stirring dissolves at 101 DEG C, mixing time 601
Minute, spinning solution A is made；
C) antibacterial agent, and strong stirring 30 minutes at 96 DEG C are added into spinning solution A, spinning solution B is made；
D) spinning solution B is cooled down using 50 DEG C of water bath with thermostatic control, and fire retardant is added thereto after water-bath equality of temperature, is passed through
Spinning solution is made after stirring；
E) spinning solution is transported to spinning machine, forms in coagulating bath after spinning head squeezes out, is then drawn through coagulating bath
It stretches, flame-retardant anti-bacterial fiber precursor is made in water-bath and the process that oils；Spinning condition be pump for amount be 1.6g/min, spinning head 80
Hole.
Embodiment 2
A kind of preparation method of flame-retardant anti-bacterial fiber precursor, comprising the following steps:
A) raw material is weighed by following parts by weight: 90 parts of polyacrylonitrile, 2 parts of fire retardant, 0.3 part of antibacterial agent, organic solvent 400
Part；Fire retardant is ammonium hydrogen carbonate 9wt%, sodium bicarbonate 11wt%, saleratus 6wt%, diatomite 74wt%；Antibacterial agent is aluminum phosphate
25wt%, calcium phosphate 15wt%, aluminium triphosphate 60wt%；Organic solvent is N,N-dimethylformamide；
Diatomite passes through following pretreatment before addition: diatomite in powder is first broken to 1.5 microns, it is then molten in dehydrated alcohol
It is ultrasonically treated in liquid 200 seconds, is then ultrasonically treated 20 minutes, finally washes with water 5 times in saturated sodium bicarbonate solution；Ultrasound
Controlled at 60 DEG C when processing；
B) by polyacrylonitrile and organic solvent mixed dissolution, and strong stirring dissolves at 110 DEG C, mixing time 650
Minute, spinning solution A is made；
C) antibacterial agent, and strong stirring 35 minutes at 104 DEG C are added into spinning solution A, spinning solution B is made；
D) spinning solution B is cooled down using 55 DEG C of water bath with thermostatic control, and fire retardant is added thereto after water-bath equality of temperature, is passed through
Spinning solution is made after stirring；
E) spinning solution is transported to spinning machine, forms in coagulating bath after spinning head squeezes out, is then drawn through coagulating bath
It stretches, flame-retardant anti-bacterial fiber precursor is made in water-bath and the process that oils；Spinning condition be pump for amount be 1.7g/min, spinning head 85
Hole.
Embodiment 3
A kind of preparation method of flame-retardant anti-bacterial fiber precursor, comprising the following steps:
A) raw material is weighed by following parts by weight: 90 parts of polyacrylonitrile, 3 parts of fire retardant, 0.4 part of antibacterial agent, organic solvent 450
Part；Fire retardant is ammonium hydrogen carbonate 10wt%, sodium bicarbonate 12wt%, saleratus 8wt%, diatomite 70wt%；Antibacterial agent is phosphoric acid
Aluminium 28wt%, calcium phosphate 18wt%, aluminium triphosphate 54wt%；Organic solvent is dimethyl sulfoxide, N,N-dimethylformamide, N, N-
The mixture of dimethyl acetamide volume ratio 1:1:1；
Diatomite passes through following pretreatment before addition: diatomite in powder is first broken to 1.5 microns, it is then molten in dehydrated alcohol
It is ultrasonically treated in liquid 400 seconds, is then ultrasonically treated 40 minutes, finally washes with water 5 times in saturated sodium bicarbonate solution；Ultrasound
Controlled at 70 DEG C when processing；
B) by polyacrylonitrile and organic solvent mixed dissolution, and strong stirring dissolves at 120 DEG C, mixing time 700
Minute, spinning solution A is made；
C) antibacterial agent, and strong stirring 35 minutes at 105 DEG C are added into spinning solution A, spinning solution B is made；
D) spinning solution B is cooled down using 55 DEG C of water bath with thermostatic control, and fire retardant is added thereto after water-bath equality of temperature, is passed through
Spinning solution is made after stirring；
E) spinning solution is transported to spinning machine, forms in coagulating bath after spinning head squeezes out, is then drawn through coagulating bath
It stretches, flame-retardant anti-bacterial fiber precursor is made in water-bath and the process that oils；Spinning condition be pump for amount be 1.9g/min, spinning head 95
Hole.
Embodiment 4
A kind of preparation method of flame-retardant anti-bacterial fiber precursor, comprising the following steps:
A) raw material is weighed by following parts by weight: 90 parts of polyacrylonitrile, 3.5 parts of fire retardant, 0.45 part of antibacterial agent, organic solvent
500 parts；Fire retardant is ammonium hydrogen carbonate 11wt%, sodium bicarbonate 13wt%, saleratus 10wt%, diatomite 66wt%；Antibacterial agent is
Aluminum phosphate 30wt%, calcium phosphate 20wt%, aluminium triphosphate 50wt%；Organic solvent is DMAC N,N' dimethyl acetamide；
Diatomite passes through following pretreatment before addition: diatomite in powder being first broken to 2 microns, then in ethanol solution
Middle ultrasonic treatment 600 seconds, is then ultrasonically treated 60 minutes in saturated sodium bicarbonate solution, finally washes with water 6 times；At ultrasound
Controlled at 75 DEG C when reason；
B) by polyacrylonitrile and organic solvent mixed dissolution, and strong stirring dissolves at 129 DEG C, mixing time 719
Minute, spinning solution A is made；
C) antibacterial agent, and strong stirring 40 minutes at 109 DEG C are added into spinning solution A, spinning solution B is made；
D) spinning solution B is cooled down using 60 DEG C of water bath with thermostatic control, and fire retardant is added thereto after water-bath equality of temperature, is passed through
Spinning solution is made after stirring；
E) spinning solution is transported to spinning machine, forms in coagulating bath after spinning head squeezes out, is then drawn through coagulating bath
It stretches, flame-retardant anti-bacterial fiber precursor is made in water-bath and the process that oils；Spinning condition be pump for amount be 2.0g/min, spinning head 100
Hole.
Through flame-proof antibiotic polyacrylonitrile fibre fiber number made from above-mentioned technique be 10~14dtex, tensile strength be 800~
900Mpa, fiber surface is more smooth, and limit oxygen index is to have quite reliable flame retardant property between 25~30；Using oscillation
Method (GB/T 20944.3-2008) tests flame-retardant anti-bacterial fiber made from above-described embodiment, and the antibiotic rate to Escherichia coli is 99%
Or more, the antibiotic rate to Staphylococcus aureus is 99.5% or more.
It should be understood that those skilled in the art, can be improved or be become according to the above description
It changes, and all these modifications and variations should all belong to the protection domain of appended claims of the present invention.
Claims (5)
1. a kind of preparation method of flame-retardant anti-bacterial fiber precursor, it is characterised in that the following steps are included:
A) raw material is weighed by following parts by weight: 90 parts of polyacrylonitrile, 1.5~3.5 parts of fire retardant, 0.25~0.45 part of antibacterial agent,
350~500 parts of organic solvent；The fire retardant is 8~11wt% of ammonium hydrogen carbonate, 10~13wt% of sodium bicarbonate, saleratus 5
~10wt%, surplus are diatomite；The antibacterial agent is 20~30wt% of aluminum phosphate, and 10~20wt% of calcium phosphate, surplus is trimerization
Aluminum phosphate；
B) by polyacrylonitrile and organic solvent mixed dissolution, and strong stirring dissolves at 101~129 DEG C, mixing time 601
~719 minutes, spinning solution A is made；
C) antibacterial agent, and strong stirring 30~40 minutes at 96~109 DEG C are added into spinning solution A, spinning solution is made
B；
D) fire retardant is added thereto, spinning solution is made after agitated after certain time is cooling by spinning solution B；
E) spinning solution is transported to spinning machine, is formed in coagulating bath after spinning head squeezes out, then through coagulating bath stretching, water
Flame-retardant anti-bacterial fiber precursor is made in process of bathing and oil.
2. a kind of preparation method of flame-retardant anti-bacterial fiber precursor according to claim 1, it is characterised in that: described is organic
Solvent is one of dimethyl sulfoxide, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide or a variety of mixtures.
3. a kind of preparation method of flame-retardant anti-bacterial fiber precursor according to claim 1, it is characterised in that the diatom
Soil passes through following pretreatment: diatomite in powder being first broken to 1~2 micron, 10~600 are then ultrasonically treated in ethanol solution
Second, it is then ultrasonically treated 1~60 minute, finally washes with water 4~6 times in saturated sodium bicarbonate solution；It is ultrasonically treated time control
Temperature processed is 50~75 DEG C.
4. a kind of preparation method of flame-retardant anti-bacterial fiber precursor according to claim 1, it is characterised in that: the step d
In, spinning solution B is cooled down using 50~60 DEG C of water bath with thermostatic control, and fire retardant is added thereto after water-bath equality of temperature.
5. a kind of preparation method of flame-retardant anti-bacterial fiber precursor according to claim 1, it is characterised in that: the step e
It for amount is 1.6~2.0g/min that middle spinning condition, which is pump, and spinning head is 80~100 holes.
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| CN107604457A (en) * | 2017-10-18 | 2018-01-19 | 温州市赢创新材料技术有限公司 | A kind of flame-retardant polypropylene long filament and preparation method thereof |
| CN108103612A (en) * | 2017-11-30 | 2018-06-01 | 湖州科博信息科技有限公司 | A kind of preparation method of anti-bacterial fibre |
| CN108085777A (en) * | 2017-11-30 | 2018-05-29 | 湖州科博信息科技有限公司 | A kind of anti-bacterial fibre |
| CN110747630A (en) * | 2019-09-29 | 2020-02-04 | 薛采智 | Waterproof flame-retardant textile and preparation method thereof |
| CN112745456B (en) * | 2019-10-30 | 2022-07-12 | 中国石油化工股份有限公司 | Flame-retardant antibacterial agent, preparation method and application thereof, and flame-retardant antibacterial thermoplastic resin composition |
| CN114525697A (en) * | 2022-02-25 | 2022-05-24 | 昆山傲毅包装制品有限公司 | Environment-friendly paper pulp, environment-friendly paper pulp manufacturing process and environment-friendly paper |
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| CN102286800A (en) * | 2011-05-30 | 2011-12-21 | 上海瑞贝卡纤维材料科技有限公司 | Functional modified acrylic fiber for hair and preparation method thereof |
| CN105507011A (en) * | 2016-02-01 | 2016-04-20 | 安安(中国)有限公司 | Production method for novel flame-retardant PU synthetic leather |
| CN106237577A (en) * | 2016-08-01 | 2016-12-21 | 陈潜 | Extinguishment additive agent |
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| CN102029040A (en) * | 2010-11-29 | 2011-04-27 | 北京航空航天大学 | Complex additive used for extinguishment with water mist |
| CN102286800A (en) * | 2011-05-30 | 2011-12-21 | 上海瑞贝卡纤维材料科技有限公司 | Functional modified acrylic fiber for hair and preparation method thereof |
| CN105507011A (en) * | 2016-02-01 | 2016-04-20 | 安安(中国)有限公司 | Production method for novel flame-retardant PU synthetic leather |
| CN106237577A (en) * | 2016-08-01 | 2016-12-21 | 陈潜 | Extinguishment additive agent |
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Effective date of registration: 20191230 Address after: 226400, Jiangsu, Nantong province Rudong County town of Legislative Yuan neighborhood committee, Jianghai North Road No. 8 Patentee after: Nantong City Hong Xin fiber Co., Ltd Address before: 313105, Huzhou, Zhejiang province Changxing County Lu Shan Industrial Park Patentee before: Zhejiang peak Textile Co., Ltd. |