CN1060235C - Antibacterial polypropylene fiber and manufacturing method thereof - Google Patents

Antibacterial polypropylene fiber and manufacturing method thereof Download PDF

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Publication number
CN1060235C
CN1060235C CN 96118358 CN96118358A CN1060235C CN 1060235 C CN1060235 C CN 1060235C CN 96118358 CN96118358 CN 96118358 CN 96118358 A CN96118358 A CN 96118358A CN 1060235 C CN1060235 C CN 1060235C
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bacteriostatic
polypropylene
agent
master batch
weight
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CN1148106A (en
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林宝森
任泽雄
罗学谦
张丽
成惠
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INST OF YUEYANG PETRO-CHEMICAL GENERAL PLANT
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INST OF YUEYANG PETRO-CHEMICAL GENERAL PLANT
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Abstract

The invention discloses an antibacterial polypropylene fiber and a manufacturing method thereof. The method adopts 0.5 to 1.0 weight percent of imidazoline substances as bacteriostatic agents , 0.05 to 0.07 weight percent of alkyl ammonium bromide substances as phase transformation agents (B) and 98.93 to 99.45 weight percent of polypropylene to prepare bacteriostatic master batches, and then 5 to 10 weight percent of bacteriostatic master batches and 90 to 95 weight percent of polypropylene are mixed and spun to prepare the product of the invention, wherein the product contains 500ppm to 1000ppm of bacteriostatic agents, thereby solving the problem of poor bacteriostatic effect and avoiding the post-finishing process. The product has obvious inhibition effect on various bacteria and lasting antibacterial property, and can be used in the health care field and various industries such as clothing, household fabrics and the like.

Description

A kind of bacteriostatic PP fiber and manufacture method thereof
The present invention relates to a kind of bacteriostatic PP fiber and manufacture method thereof.
In the prior art, the report of bacteriostatic fiber is more, but generally all in polymer, add ceramic, fragrant halogen compounds, organosilicon quaternary amines, copper, zinc, silver-colored plasma compound etc., have plenty of and fiber is carried out back arrangement give its bacteriostasis, the shortcoming of said method be all to fiber physical property or the fungistatic effect in using have a negative impact.
Bacteriostatic agent used in the present invention-naphthenic acid imidazoline compounds is a kind of fine chemical product with multiple excellent properties, report as bactericide and corrosion inhibiter is abroad just arranged the end of the sixties, U.S. MillmasterOnyx and Nalco company have developed naphthenic acid imidazoline respectively and have made bactericide, microbicide and high-efficient corrosion inhibitor product, be used for fuel, industry water, lubricating oil, cosmetics to prevent growth of microorganism, also can be used for epoxy curing agent and curing accelerator occasion, but do not see report so far as the chemical fibre bacteriostatic agent.U.S. US3705027 patent report, the growth dilution test method of application standard (Stamdor Groth DintionTest Method) is carried out bactericidal assay, 1-aminoethyl-2-naphthenic acid imidazoline has the good sterilization effect to Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus, hammer mushroom, aspergillus niger, water polo algae, PCs, its minimal inhibitory concentration 10ppm-500ppm.
The object of the present invention is to provide a kind of mattress polypropylene fibre and manufacture method thereof of pressing down, use the imidazolines material to make bacteriostatic agent, and add a spot of agent (also being bactericide) that changes mutually, obtain the good bacteriostatic PP fiber of fungistatic effect, and a kind of fiber process process no change is provided, fiber physical property is not had influence, and do not need the arrangement of any back, promptly give the manufacture method that fiber has the bacteriostatic PP fiber of remarkable fungistatic effect.
The objective of the invention is to realize by the following technical solutions: with imidazolines material (bacteriostatic agent A) with change mutually that agent (B) (also being bactericide) mixes with polypropylene and granulation obtains the antibacterial master batch of polypropylene; then antibacterial master batch is mixed by a certain percentage with fibrous polypropylene; spinning under 230-280 ℃ temperature; again through coiling, boundling, drawing-off, curl, process such as typing; promptly get bacteriostatic PP fiber, contain the bacteriostatic agent of 500ppm-1000ppm (weight) in this novel bacteriostatic fiber.The present invention's technical scheme preferably is that bacteriostatic agent (A) selects for use chemical formula to be
Figure 9611835800031
The imidazolines material, the R in the formula is a cycloalkyl, R ' is H, CH 2CH 2NH 2, (CH 2CH 2NH) nCH 2CH 2NH 2, (n is 1-2 positive integer) is as naphthenic acid imidazoline (A 1), amine ethyl naphthenic acid imidazoline (A 2), triethylene tetramine basic ring alkanoic acid imidazoline (A 3) and tetraethylenepentamine naphthenic acid imidazoline (A 4) and analog; Changing agent (B) employing chemical formula mutually is C nH 2n+1N +(CH 3) m B r - Class material, the n in the formula are any positive integer of 1-16, and m is another any positive integer of 1-4. as methyl bromide (B 1), bromination butane tetramethyl amine (B 2), bromination decane dimethyl amine (B 3), cetyltrimethylammonium base amine (B 4) and analog, this class material is to change agent mutually, also plays bactericidal action simultaneously.
In implementing process of the present invention, bacteriostatic agent (A) can be wherein a kind of or several mixing and a usefulness with changing agent (B) mutually respectively, can both play same effect.In view of the consumption that changes agent (B) mutually very few, so often only add wherein a kind of in force, to simplify the operation.
The present invention's technical scheme preferably also can be: the content of bacteriostatic agent in the antibacterial master batch (A) is 0.5%-1.0% (weight), the content that changes agent (B) mutually is 0.05%-0.07% (weight), polypropylene content is 98.93%-99.45% (weight), the consumption that presses down mattress agent (A) in the preparation is not wanted too much or very few, the highest described consumption can reach the fungistatic effect of expection fully, but then can not reach required fungistatic effect if its consumption is crossed when hanging down, especially negative bacillus such as proteus and Pseudomonas aeruginosa be lost fungistatic effect.
The present invention's technical scheme preferably can be again: when manufacturing presses down the mattress master batch, need earlier in bacteriostatic agent (A) and the mixed liquor that changes agent (B) mutually adding desire to prepare the water of antibacterial master batch gross weight 1%-3%, make bacteriostatic agent be transformed into emulsion, be convenient to bacteriostatic agent good dispersion is arranged in base-material, get the polypropylene powder of required polypropylene gross weight 10% then, stir, and under 100-110 ℃ temperature dry 3-4 hours, remove added water in the aforementioned process, again all the other 90% polypropylene powders or pellet are added and evenly mix.With granulation screw Cast Strip, pelletizing, promptly make the antibacterial master batch that contains 5000ppm-10000ppm (weight) bacteriostatic agent.In implementation process, described amount of water is not strict, as long as can make bacteriostatic agent be transformed into emulsion, and be convenient to make powder to disperse, stirring gets final product.
The present invention's technical scheme preferably can also be: get aforesaid antibacterial master batch, press the fibrous polypropylene pellet or the powder blend of master batch 5%-10% (weight) and 90%-95% (weight), spinning under 230-280 ℃ temperature, and then through drawing-off, curl and typing etc. a series of with make the plain polypropylene fiber same after processing, promptly obtain the bacteriostatic PP fiber that bacteriostatic agent content is 500ppm-1000ppm (weight).In specific implementation process, need control antibacterial master batch and polyacrylic ratio well, guarantee that the bacteriostatic agent content in the fiber is 500ppm-1000ppm (weight).
The present invention has following tangible advantage:
1, fungistatic effect is remarkable: product of the present invention carries out external bacteriostatic experiment analysis by training center of clinical pharmacology country of Hunan Medical University.
(1) bacterial strain: staphylococcus aureus, hemolytic streptococcus, proteus, Escherichia coli, Pseudomonas aeruginosa, candida albicans.
Cultivate: Mueler-Hinfon agar medium, husky Bao Shi agar medium.
(2) method: (the QninnShi method comes from H.Qnin:Appl Microbiol, 1962 to the seed agar cultivation; 10:75)
Adjusting bacteria concentration is 1.5 * 10 8CFU/ml is inoculated on the sample of 1 * 2cm size to be measured, and 37 ℃ of overnight incubation and suitably dry are affixed on fabric after the drying on the above-mentioned agar medium surface, abandon fabric.Operate as negative control by last method with identical big or small aseptic filter paper sheet simultaneously, place 37 ℃ of incubators to cultivate observed result 18 hours then.
(3) result judges: to cover with the bacterium person on the filter paper negative control culture medium, show that experiment condition is qualified.Criterion is as follows as a result:
Paste the full bacterium of fabric director on +++: the culture medium, be no bacteriostasis.
++: paste the fabric place long bacterium in half zone approximately on the culture medium, for there not being bacteriostasis substantially.
+: paste fabric director<5 bacterium colonies on the culture medium, for part antibacterial.
-: paste the not long bacterium in fabric place on the culture medium, for antibacterial.
(4) result
Project No. 8 No. 9 No. 10 No. 11 No. 0
Staphylococcus aureus---++ +++β-hemolytic streptococcus---++++proteus-+++ ++++++Escherichia coli--+++ +++Pseudomonas aeruginosa--+++++++candida albicans---++ +++
Annotate: No. 8 1000ppm bacteriostatic agents of sample polypropylene fabric
No. 9 500ppm bacteriostatic agent polypropylene fabrics
No. 10 250ppm bacteriostatic agent polypropylene fabrics
No. 11 virgin pp fabrics
No. 0 filter paper (No. one, Xinhua) (negative control)
6 kinds of bacteriums to test when bacteriostatic agent is higher than 500ppm in fabric all have significant bacteriostasis.
2, the bacteriostatic agent high effect nontoxic of the present invention's employing, it can be evenly dispersed in the raw material, and the spinnability of fiber is not had influence, and the fiber delivery of antimicrobials is evenly lasting, does not influence the physical property of fiber itself, and anti-soaping can effectively be killed the bacterium that is attached on the fabric.
3, easy to operate, production method is simple, in existing polypropylene fibre or polypropylene plastics products production, as long as add antibacterial master batch of the present invention, can produce remarkable bacteriostasis to various bacteria at fiber or product surface, without any harmful effect, need not increase special equipment to production technology yet.
Below be the specific embodiment of the present invention:
Embodiment 1: get bacteriostatic agent A 1Restrain 9.5 restrain and change agent B40.7 mutually, add water 30 grams, be emulsion form after mixing, add polypropylene powder 90 grams, stir, drying is 3.5 hours under 100-108 ℃ temperature, again to wherein adding 900 gram polypropylene granules, after mixing, get antibacterial master batch 996 grams with granulation screw Cast Strip, blank, again that whole master batches and 19000 gram polypropylene granules (fibre-grade) blend are even, spinning under 232-257 ℃ temperature, and through coiling, boundling, drawing-off, curl and HEAT SETTING etc. after manufacturing procedure promptly get the bacteriostatic PP fiber product.Contain bacteriostatic agent A in the antibacterial master batch of this example 10.95%, change agent B mutually 40.07%, polypropylene content is 98.98%, and bacteriostatic agent is 500ppm in the bacteriostatic fiber.
Embodiment 2: step is the same, adds A 38 grams, B 10.7 gram, water 30 restrains, and the system master batch adds the polypropylene amount for twice and is respectively 90 grams and 904 grams, and be 3.9 hours drying time, gets master batch 1001 grams, and co-blended spinning adds polypropylene 12020 grams, and spinning temperature is 249-264 ℃, contains bacteriostatic agent A in the antibacterial master batch of this example 30.8%, change agent B mutually 10.07%, polypropylene content is 99.13%, and containing in the bacteriostatic fiber and pressing down the mattress agent is 620ppm.
Embodiment 3: step is the same, adds A 45.5 gram, B 30.51 gram, water 10 restrains, and the system master batch adds the polypropylene amount for twice and is respectively 90 grams and 904 grams, and be 3.1 hours drying time, gets master batch 1000 grams, and co-blended spinning adds polypropylene 9000 grams, and spinning temperature is 238-260 ℃, contains bacteriostatic agent A in the antibacterial master batch of this example 40.55%, contain and change agent B mutually 3Be 0.051%, polypropylene content is 99.43%, bacteriostatic agent 550ppm in the bacteriostatic fiber.
Embodiment 4: step is the same, adds A 23.5 gram, A 46.0 gram, B 10.6 gram, water 20 restrains, and the system master batch adds the polypropylene amount for twice and is respectively 90 grams and 903 grams, and be 3.3 hours drying time, gets master batch 1000 grams, and co-blended spinning adds polypropylene 9000 grams, and spinning temperature is 253-278 ℃, bacteriostatic agent A in the antibacterial master batch of this example 2And A 4Count 0.95%, contain and change agent B mutually 1Be 0.06%, polypropylene content is 99.02%, bacteriostatic agent 950ppm in the fiber.
Embodiment 5: step is the same, adds A 14.5 gram, A 33.0 gram, B 20.52 restrain, water 25 grams, system master batch add the polypropylene amount for twice and are respectively 90 grams and 901 grams, be 3.7 hours drying time, gets master batch 997 grams, and co-blended spinning adds polypropylene 9700 grams, and spinning temperature is 247-266 ℃, contains bacteriostatic agent A in the antibacterial master batch of this example 1And A 3Count 0.75%, contain and change agent B mutually 20.052%, polypropylene content is 99.20%, bacteriostatic agent 700ppm in the fiber.

Claims (2)

  1. The manufacture method of 1 one kinds of bacteriostatic PP fibers, comprise antibacterial master batch manufacturing, master batch and polypropene blended, spinning, coiling, drawing-off, curl, process such as typing, the invention is characterized in:
    (1) weight percentage of antibacterial master batch each component is: bacteriostatic agent (A) 0.5%-1.0%, change agent (B) 0.05%-0.07% mutually, and polypropylene 98.93%-99.45%, wherein the chemical formula of bacteriostatic agent (A) is:
    Figure 9611835800021
    In the formula: R is a cycloalkyl, and R ' is H, CH 2CH 2NH 2, (CH 2CH 2NH) nCH 2CH 2NH 2, n is that the chemical formula that 1-2 positive integer changes agent (B) mutually is: C n H 2 n + 1 N + ( C H 3 ) m B r -
    In the formula: n is any positive integer of 1-16, and m is another any positive integer of 1-4;
    (2) with bacteriostatic agent (A), change agent (B) and 1%-3% water (weight mutually, by the antibacterial master batch total amount of preparation) mix, make bacteriostatic agent be transformed into emulsion, add 10% powder of required polypropylene gross weight again, stir, drying is 3-4 hours under 100-110 ℃ temperature, again the polypropylene of all the other 90% (weight) is added and mix, with granulation screw Cast Strip, pelletizing, making bacteriostatic agent content is the antibacterial master batch of 5000ppm-10000ppm (weight), then
    (3) with the polypropylene granules blend of the antibacterial master batch and 90%-95% (weight) of 5%-10% (weight), spinning under 230-280 ℃ temperature, and through after processed, make the polypropylene fibre that contains 500ppm-1000ppm (weight) bacteriostatic agent.
  2. The product that 2 bacteriostatic PP fiber manufacture methods according to claim 1 are obtained.
CN 96118358 1996-09-26 1996-09-26 Antibacterial polypropylene fiber and manufacturing method thereof Expired - Fee Related CN1060235C (en)

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Application Number Priority Date Filing Date Title
CN 96118358 CN1060235C (en) 1996-09-26 1996-09-26 Antibacterial polypropylene fiber and manufacturing method thereof

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CN1060235C true CN1060235C (en) 2001-01-03

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012058962A1 (en) 2010-11-03 2012-05-10 广东百合医疗科技有限公司 Antimicrobial fiber, fabric and wound dressing containing nano metal and preparation method thereof

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1091177C (en) * 2000-05-25 2002-09-18 舒军 Composite antibacterial fibre, its preparation method and application
CN102121174A (en) * 2010-12-24 2011-07-13 北京美格赛斯无纺科技有限公司 Nonwovens containing antibacterial and antiviral master batches and method and device for producing same
CN103628168A (en) * 2013-11-08 2014-03-12 绍兴东盛京纺织服装有限公司 Nature antibacterial health-care ultraviolet-proofing polypropylene fiber
CN106621572B (en) * 2016-11-17 2019-06-28 浙江水马环保科技有限公司 A kind of polybasic ion antibacterial PP fabric filter element and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012058962A1 (en) 2010-11-03 2012-05-10 广东百合医疗科技有限公司 Antimicrobial fiber, fabric and wound dressing containing nano metal and preparation method thereof

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