CN106496672B - A kind of preparation process based on quaternary ammonium salt antibacterial antiplaque agent natural latex products - Google Patents
A kind of preparation process based on quaternary ammonium salt antibacterial antiplaque agent natural latex products Download PDFInfo
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- CN106496672B CN106496672B CN201610911828.1A CN201610911828A CN106496672B CN 106496672 B CN106496672 B CN 106496672B CN 201610911828 A CN201610911828 A CN 201610911828A CN 106496672 B CN106496672 B CN 106496672B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/30—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by mixing gases into liquid compositions or plastisols, e.g. frothing with air
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
- C08K5/19—Quaternary ammonium compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2307/00—Characterised by the use of natural rubber
- C08J2307/02—Latex
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/14—Applications used for foams
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
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Abstract
One kind being based on quaternary ammonium salt antibacterial antiplaque agent natural latex products and its preparation process, belongs to latex material technical field.Include each component of following parts by weight：90~100 parts of natural emulsion, 1~9 part of sulphur, 1~5 part of vulcanization accelerator, 1.5~2 parts of antiaging agent, 1~6 part of zinc oxide, 0.5~2 part of prodan, 1~3 part of potassium ricinoleate, 0.1~2 part of potassium oleate, 0.5~1 part of potassium pyrophosphate, 0.1~3 part of quaternary ammonium salt antiseptic.The present invention is based on the quarternary ammonium salt compound of the low concentration antibacterial characteristics of itself.The quaternary ammonium compound of use is stablized with performance, is combined with emulsion polymer molecule in close, by the physicochemical properties of change material surface, the advantages of not penetrating into human or animal's epidermis.So that latex product made of the present invention has many advantages, such as high antibiotic property, health, highly practical, foreground is had a vast market.
Description
Technical field
The present invention relates to latex material manufacturing field more particularly to a kind of resisting based on quaternary ammonium compound antibacterial characteristics
Bacterium natural latex products and its preparation process.
Background technology
With the continuous improvement of living standards, demand of the people to high-quality life is also further urgent.In order to inhibit bacterium to give birth to
It is long, harm of the harmful bacteria to the mankind is reduced, develops the anti-biotic material with high antimicrobial efficiency always by of interest both at home and abroad.It
Right latex is the natural gum acquired from rubber tree, is a kind of milky white liquid.Natural latex products are in use because of environment
Factor can grow bacterium, and traditional sterilizing methods are easily reduced its service life, and cannot solve the problems, such as microbiological contamination again.
Invention content
The present invention in view of the above problems, provide a kind of green health, with antibacterial characteristics based on quaternary ammonium salt antibacterial
Agent antimicrobial natural latex product and its preparation process.
The technical scheme is that：Include each component of following parts by weight：90~100 parts of natural emulsion, sulphur 1~9
Part, 1~5 part of vulcanization accelerator, 1.5~2 parts of antiaging agent, 1~6 part of zinc oxide, 0.5~2 part of prodan, potassium ricinoleate
1~3 part, 0.1~2 part of potassium oleate, 0.5~1 part of potassium pyrophosphate, 0.1~3 part of quaternary ammonium salt antiseptic.
The quaternary ammonium salt antiseptic is monoalkyl quaternary ammonium salts, dialkyl quaternary ammonium salt, organosilicon quaternary ammonium salt, Organic fluoride quaternary ammonium
One or more in salt, organochlorine quaternary ammonium salt are used in combination.
A kind of preparation process based on quaternary ammonium salt antibacterial antiplaque agent natural latex products, which is characterized in that including following
Step：
1) natural emulsion, sulphur, potassium ricinoleate, potassium oleate, potassium pyrophosphate and antiaging agent mechanical agitation are mixed
Uniformly, vulcanization accelerator is added, continues stirring maturation in 8~12 hours, is subsequently added into zinc oxide and quaternary ammonium salt antiseptic stirs
It mixes 0.5~2 hour, forms liquid sizing material；
2) prodan and supply air are added in liquid sizing material, as bubbling raw material, high-speed stirred, machinery rises
Bubble；
3) high temperature steam treatment makes its gelling sizing, demoulding wash, and mechanical presses water dumping, Drying and cooling completes sizing, cuts out
Cut processing finished product.
The present invention is using the advantages of having both natural emulsion based on the antimicrobial natural latex product that quaternary ammonium salt antiseptic is researched and developed
And antibacterial characteristics.Quaternary ammonium salt antiseptic, which grafts on latex high polymer, can be made that toxicity is low, antibacterial time is long, environmental pollution is small
Antimicrobial natural latex product.
Quaternary ammonium salt antiseptic grafts on latex high polymer, changes the physicochemical properties on latex foam surface, increases just
The density of charge is easy to adsorb negatively charged bacterium, invades its cell wall and is combined with cell membrane, final destroying cells film,
The formation that bacterial biof iotalm is prevented from source reaches better antibacterial effect.
The preparation process is：It is kneaded, vulcanization, sizing, molding, processes finished product.First by natural emulsion and potassium oleate machine
Tool is uniformly mixed, and vulcanizing activator is added, and is stirred maturation in 8~12 hours, is continuously added zinc oxide, quaternary ammonium salt antiseptic
After antiseptic stirs 0.5~2 hour, prodan and supply air, high-speed stirred, in the short time are added in liquid sizing material
Blistering, 120 DEG C of steam treatments, 1~2 hour aftershaping wash with water clean, Drying and cooling, complete sizing, cutting processing finished product.
Compared with the prior art the present invention has the following advantages that：
1, the natural latex products that the present invention researches and develops have good tensile strength, elasticity modulus and compression set.
2, natural latex products prepared by the present invention have excellent inhibition to gram-positive bacteria and Gram-negative bacteria
Characteristic has wide spectrum, effective anti-microbial property, safe to the human body.
3, the invention belongs to daily necessities fields, and technological process is easy to operate, and product of the present invention also has wide city
Field foreground；Natural latex products are produced using the present invention, not only the high resiliency with natural emulsion product, the spies such as soft comfortable
Point, but also there is efficient fungistatic effect, play the role of improving people’s lives quality.
Description of the drawings
Fig. 1 be quaternary ammonium salt antiseptic in the present invention, natural emulsion sponge and antibacterial latex sponge infrared spectrum；
Fig. 2 is the scanning electron microscope (SEM) photograph of natural emulsion sponge in the present invention；
Fig. 3 is that the antibacterial width of natural emulsion sponge changes with time relational graph in the present invention；
Fig. 4 is that the antibacterial efficiency of natural emulsion sponge changes with time relational graph in the present invention；
Specific implementation mode
The present invention by natural emulsion, sulphur, vulcanization accelerator, antiaging agent, zinc oxide, prodan, potassium ricinoleate,
Potassium oleate, potassium pyrophosphate, quaternary ammonium salt antiseptic are made by being kneaded, vulcanizing maturation, be molded, and include each group of following parts by weight
Point：
90~100 parts of natural emulsion, 1~6 part of zinc oxide
1.5~2 parts of antiaging agent, 0.5~2 part of prodan
1~9 part of sulphur, 0.1~2 part of potassium ricinoleate
0.1~2 part of potassium oleate, 0.5~1 part of potassium pyrophosphate
1~5 part of vulcanization accelerator, 0.1~3 part of quaternary ammonium salt antiseptic.
Embodiment one：Include each component of following parts by weight：
90 parts of natural emulsion, 1 part of zinc oxide
1.5 parts of antiaging agent, 0.5 part of prodan
1 part of sulphur, 0.1 part of potassium ricinoleate
0.1 part of potassium oleate, 0.5 part of potassium pyrophosphate
1 part of vulcanization accelerator, 0.1 part of quaternary ammonium salt antiseptic.
Embodiment two：Include each component of following parts by weight：
95 parts of natural emulsion, 3 parts of zinc oxide
1.5 parts of antiaging agent, 1 part of prodan
5 parts of sulphur, 1 part of potassium ricinoleate
1 part of potassium oleate, 0.5 part of potassium pyrophosphate
2 parts of vulcanization accelerator, 2 parts of quaternary ammonium salt antiseptic.
Embodiment three：Include each component of following parts by weight：
100 parts of natural emulsion, 6 parts of zinc oxide
2 parts of antiaging agent, 2 parts of prodan
9 parts of sulphur, 2 parts of potassium ricinoleate
2 parts of potassium oleate, 1 part of potassium pyrophosphate
5 parts of vulcanization accelerator, 3 parts of quaternary ammonium salt antiseptic.
Each component effect is as follows：
Sulphur belongs to vulcanizing agent, generates cross-linking reaction with rubber, forms it into space network, make rubber by plasticity
Material becomes elastic material, has valuable use value；
Vulcanization accelerator, accelerating agent, which is added, so that vulcanizing agent is activated, to accelerate the crosslinking between vulcanizing agent and rubber molecule
Reaction shortens vulcanization time and reduces curing temperature；
Antiaging agent can prevent and delay ageing of rubber, such as rubber oxidation deterioration or ozonisation to go bad；
Zinc oxide is used as the inorganic active agent of latex, and sizing material, which is added, can not only accelerate curingprocess rate, moreover it is possible to improve crosslinking
Degree.
Prodan makes the slow gelling of foamed latex as delayer coagulant；
Potassium ricinoleate can prevent latex foam from rupturing as latex foam stabilizer, and foam is maintained to stablize；
Potassium oleate, as foaming agent, can be dissolved in water makes the reduction of Scatter Light of Bubble Interface in Water tension, and protection is formed around bubble
Layer, to generate foam；
Potassium pyrophosphate, the metal ions such as calcium, magnesium can be chelated as dispersant, chelating agent by belonging to anion surfactant；
Quaternary ammonium salt antiseptic, compared to other antiseptics are added, also makees foam rubber in addition to itself has antibacterial characteristics
Glue gelling stabilizer, in case lather collapse and contraction, can also improve the structural behaviour of foam.
The latex foam surface that the present invention is added to quaternary ammonium salt antiseptic is relatively smooth smooth, and improvement has become splitting for script
Line structure makes rubber molecule be connected with each other even closer, improves its structural behaviour.
The density of the latex product：70~100kg/m3；Hardness：100~200N；Tensile strength：20~50KPa；It is disconnected
Split elongation：150~250%；Compression set：1~5%；Resilience performance：>=80%；Compression set：1~5%.
The natural latex products are 15-25 millimeters to the antibacterial width of gold-coloured staphylococci, antibacterial efficiency 95-100%；
To antibacterial width 10-20 millimeters of Escherichia coli, antibacterial efficiency 70-85%.
In the implementation case, the natural latex products based on quaternary ammonium salt antibacterial antiplaque agent performance are to Escherichia coli
It is shown in Table 1 with the inhibition efficiency of staphylococcus aureus.
Table 1
Note：S.aureus：Staphylococcus aureus is clinically separated gained；E.coli：Escherichia coli ATCC25922；CFU：
Colonyunitforming, clump count；QAC：Quaternary ammonium compound.
In the implementation case, the quaternary ammonium salt antiseptic can be monoalkyl quaternary ammonium salts, dialkyl quaternary ammonium salt, organic
One kind in silicon quaternary ammonium salt, Organic fluoride quaternary ammonium salt, organochlorine quaternary ammonium salt, the organic antibacterial agent can be applied alone or a variety of mixing
It is used in combination.It is required that antiseptic is uniformly mixed in natural emulsion sizing material, in order to avoid influence foaming quality.
In the present embodiment, the concentration of the quaternary ammonium salt antiseptic can be between 0.01~0.5%, preferred quaternary ammonium
Salt antimicrobial agent concentration is between 0.01~0.3%.Unless stated otherwise, other percentages in these percentages and text are
Mass/mass percentage.
Latex product has several through-holes, can not only improve the gas permeability of latex material, convenient for heat dissipation, and also it is conveniently clear
It washes, conducive to drying after washing.
A kind of preparation process of the antimicrobial natural latex product based on quaternary ammonium salt antibacterial characteristics, includes the following steps：
1) natural emulsion, sulphur, potassium ricinoleate, potassium oleate, potassium pyrophosphate and antiaging agent mechanical agitation are mixed
Uniformly, vulcanization accelerator is added, continues stirring maturation in 8~12 hours, is subsequently added into zinc oxide and quaternary ammonium salt antiseptic stirs
It mixes 0.5~2 hour, forms liquid sizing material；
2) prodan and the constant normal temperature air of supply are added in liquid sizing material, as bubbling raw material, in high-speed stirring
It mixes and stirs under shear action, in a short time (0.5~1 hour) mechanical foaming；
3) (100~120 DEG C) processing of high-temperature steam make its gelling sizing, demoulding wash, mechanical presses water dumping, and drying is cold
But, sizing is completed, processing finished product is cut.
Disperse unevenness since zinc oxide exists, cause deposition and dead glue phenomenon, therefore, prepares modified zinc oxide, improve and divide
Dissipate uniformity.
The zinc oxide is modified zinc oxide, includes each component of following parts by weight：8-15 parts of water, sodium hydroxide 0.01-
0.1 part, 0.5-2 parts of 2-6 parts of zinc oxide and tetraethyl orthosilicate.
The preparation method of modified zinc oxide is：Water intaking is added sodium hydroxide and adjusts pH so that pH value 9-11；PH value is got over
Height, tetraethyl orthosilicate hydrolysis rate are faster；Zinc oxide is added to the water again and is dispersed with stirring uniformly；Add positive silicic acid tetrem
Ester is stood after persistently stirring 4-8h；It completes.
By modified zinc oxide, is hydrolyzed under alkaline condition using tetraethyl orthosilicate and generate silica, be coated on oxidation
The surface of zinc while improving zinc oxide dispersibility, and can prevent zinc oxide surface from being contacted with latex, slow down zinc oxide and foam
Gelation rate in the process, and when high temperature vulcanized, very thin silicon dioxide layer dissolves under alkaline condition, and alkaline condition is：
Potassium hydroxide is added in liquid sizing material in step 1) and adjusts pH so that potassium hydroxide is added convenient for corrosion two in pH value 8-12
Silica；Sulfurate activity effect just can be given full play at this time.
Compared to other antiseptics are added, difficult point of the invention is, in latex vulcanizate after the addition of quaternary ammonium salt antiseptic
When solidification, it can occur to solidify coking in advance because uneven, modified zinc oxide slows down gelation rate so that be uniformly mixed, improve
The reliability of product.
The latex foam surface that the present invention is added to quaternary ammonium salt antiseptic is relatively smooth smooth, and improvement has become splitting for script
Line structure makes rubber molecule be connected with each other even closer, improves its structural behaviour.
Fig. 1 is quaternary ammonium salt antiseptic (1) of the present invention, natural emulsion sponge (2), antibacterial latex sponge (3) it is red
Outer spectrogram.
In the infrared spectrum of quaternary ammonium salt antiseptic (1) of the present invention, 3441cm-1Place is the stretching vibration of N-H keys
Absorption peak, 2923,2853cm-1The strong of place absorbs the stretching vibration that can belong to c h bond, 1627cm-1The absorption peak at place
The C-C stretching vibrations on aromatic ring, 1465cm can be belonged to-1Neighbouring absorption peak be methylene scissoring vibration and methyl it is anti-
The superposition of symmetrical deformation vibration.891cm-1And 722cm-1Place's absorption peak is then attributable to the flat wagging vibration of methylene.
In the infrared spectrum of natural emulsion sponge (2), 2981cm-1Nearby there is the C-H that absorption peak can belong to methyl
Stretching vibration, 2885cm-1, 2818cm-1The absorption peak that place occurs can belong to the C-H stretching vibrations of methine, 1696cm-1
There is the stretching vibration that absorption peak can belong to aliphatic C=C, 1300cm in place-1The strong absworption peak that place occurs can belong to methyl
C-H in-plane bending vibrations, 961cm-1, 844cm-1The strong absworption peak that place occurs can belong to C-H out-of-plane bending vibrations, these
Peak is the principal character peak of natural rubber.
In the infrared spectrum of antibacterial latex sponge (3), big variation does not occur for the principal character peak of natural rubber,
3500cm-1The sharp absorption peak nearby occurred is the N-H keys of association, 1690cm-1, 1650cm-1The absorption peak at place can belong to
In the C-C stretching vibrations on aromatic ring, illustrate that quaternary ammonium compound can be good at being grafted on natural emulsion molecular structure.
Fig. 2 is the scanning electron microscope (SEM) photograph of natural emulsion sponge of the present invention.Wherein 1,2,3 do not add quaternary ammonium salt antiseptic respectively
For latex foam in 30 μm, the microscopic appearance of 200nm, 100nm engineer's scale, 4,5,6 be respectively to be added to quaternary ammonium salt antiseptic latex
Sponge is in 30 μm, the microscopic appearance of 200nm, 100nm scale.The 5 corresponding attached drawing of serial number from Fig. 2：Quaternary ammonium salt antibacterial
The addition of agent influences less latex foam aperture structure, is cellular, is not added with the control group tool of quaternary ammonium salt antiseptic
There is a certain size not equal crack structtire, surface is more coarse, is added to the latex foam surface of quaternary ammonium salt antiseptic more
It is smooth, the crack structtire of script is covered, is connected with each other even closer.
Fig. 3 is that the antibacterial width of natural emulsion sponge of the present invention changes with time relational graph.As seen from Figure 3：Day of the present invention
Right latex product slowly reduces the antibacterial width of gold-coloured staphylococci and Escherichia coli ATCC25922 with the variation of time,
Reach stationary value, it is seen that performance is stablized, and service life is long.
Fig. 4 is that the antibacterial efficiency of natural emulsion sponge of the present invention changes with time relational graph.As seen from Figure 4：Day of the present invention
Right latex product slowly reduces the antibacterial efficiency of gold-coloured staphylococci and Escherichia coli ATCC25922 with the variation of time,
Reach stationary value, it being capable of long-time Efficient antibacterial.
The present invention is based on the anti-microbial effects of the generation of the quaternary ammonium salt antiseptic of low concentration.The present invention not only maintains
The advantage of natural emulsion, such as super-elastic, orthopaedic function, ventilating mildew-resistant is super-silent etc., and the quaternary ammonium salt antiseptic used
Stablize with performance, non-volatile, service life is long, is combined with emulsion polymer molecule in close, and human or animal's epidermis is not penetrated into
The advantages that, and the physicochemical properties by changing material surface, the formation of bacterial biof iotalm can be prevented from source.This makes
It is of the invention made of latex foam have many advantages, such as high antibiotic property, health, highly practical, improve people’s lives matter
Amount.Therefore, the present invention has a vast market application prospect.
Claims (2)
1. a kind of preparation process based on quaternary ammonium salt antibacterial antiplaque agent natural latex products, includes each group of following parts by weight
Point：90~100 parts of natural emulsion, 1~9 part of sulphur, 1~5 part of vulcanization accelerator, 1.5~2 parts of antiaging agent, zinc oxide 1~6
Part, 0.5~2 part of prodan, 1~3 part of potassium ricinoleate, 0.1~2 part of potassium oleate, 0.5~1 part of potassium pyrophosphate, quaternary ammonium salt
0.1~3 part of antiseptic；
It is characterized in that：Include the following steps：
1) natural emulsion, sulphur, potassium ricinoleate, potassium oleate, potassium pyrophosphate and antiaging agent mechanical agitation are uniformly mixed,
Vulcanization accelerator is added, continues stirring maturation in 8~12 hours, is subsequently added into zinc oxide and quaternary ammonium salt antiseptic stirring 0.5
~2 hours, form liquid sizing material；
2) prodan and supply air are added in liquid sizing material, as bubbling raw material, high-speed stirred, mechanical foaming；
3) high temperature steam treatment makes its gelling sizing, demoulds washing, mechanical presses water dumping, and Drying and cooling completes sizing, cuts and adds
Work finished product；
The zinc oxide is modified zinc oxide, includes each component of following parts by weight：8-15 parts of water, sodium hydroxide 0.01-0.1
Part, 0.5-2 parts of 2-6 parts of zinc oxide and tetraethyl orthosilicate；
The preparation method of modified zinc oxide is：Water intaking is added sodium hydroxide and adjusts pH so that pH value 9-11；PH value is higher, just
Tetraethyl orthosilicate hydrolysis rate is faster；Zinc oxide is added to the water again and is dispersed with stirring uniformly；Tetraethyl orthosilicate is added, is continued
It is stood after stirring 4-8h；It completes；
Potassium hydroxide is added in liquid sizing material in step 1) and adjusts pH so that potassium hydroxide is added convenient for corruption in pH value 8-12
Lose silica.
2. a kind of preparation process based on quaternary ammonium salt antibacterial antiplaque agent natural latex products according to claim 1,
It is characterized in that：The quaternary ammonium salt antiseptic is monoalkyl quaternary ammonium salts, dialkyl quaternary ammonium salt, organosilicon quaternary ammonium salt, Organic fluoride season
One or more in ammonium salt, organochlorine quaternary ammonium salt are used in combination.
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