CN107652477A - A kind of environment-friendly antibacterial sponge and its preparation technology - Google Patents
A kind of environment-friendly antibacterial sponge and its preparation technology Download PDFInfo
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
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Abstract
Environment-friendly antibacterial sponge and its preparation technology that will not cause that environmental pollution, preparation method are safe and harmless and resilience is good, compression set value is low, have excellent antibacterial performance can be digested the present invention relates to a kind of composition natural degradable, nature, its advantage be the present invention it is raw materials used be pollution-free, non-harmful material, to more environment-friendly；High molecular weight chitosan is set to be broken into small molecule chitosan using the method for ultrasonic disruption, compared to high molecular weight chitosan, it is higher and the problems such as be not in hardened, matter crisp poor toughness that it forms combination stability after cavernous body, the elasticity and recoverable force of cavernous body are improved, there is larger lifting to its flexibility；Obtained cavernous body flexibility, resilience are high, and compression set value is low, has very good mechanical property；Obtained cavernous body has good anti-microbial property, has antibacterial, sterilizing function, makes relatively sanitary with each object of its preparation.
Description
Technical field
The present invention relates to a kind of sponge field, more particularly to a kind of composition natural degradable, nature can digest to make
Into environmental pollution, preparation method is safe and harmless and resilience is good, compression set value is low, has excellent antibacterial performance
Environment-friendly antibacterial sponge and its preparation technology.
Background technology
Sponge is a kind of extremely common porous material, has good water imbibition, partly with good elasticity, deformation
Restorative etc. performance, it can be used in clean article or for producing some comfortable soft seat cushions.
The sponge that people commonly use is made up of wood cellulose fibers or foamed plastic polymer.In addition, also have by spongia
Manufactured natural sponge, most of natural sponges are used for clean body or drawing.In addition, closed made of also three class other materials
Into sponge, respectively low-density polyethers（Not water-absorbing sponge）, polyvinyl alcohol（High-absorbent material, without obvious stomata）And polyester.
For at present, manufacturing cost and the sponge density of in the market sponge are proportionate, and density is higher, and cost is also higher, but
The physical property of low-density sponge is often not so good as high-density sponge, particularly in the use as seat cushion etc., thus seeks
A kind of low-density but have excellent mechanical performances can meet mechanical property standard needed for seat cushion sponge in the world low-density it is high-elastic
Property sponge is a great development direction.Caused pollution is larger in the preparation process of sponge at present simultaneously, and sponge is mostly artificial high poly-
Thing is difficult to degrade, and foaming agent damages to people in foaming process, environment is polluted, and one urgently to be resolved hurrily is asked
Topic.
Existing sponge does not often possess anti-microbial property simultaneously, on the beddings such as some sleeping pillows or seat cushion sponge, has
Good antibiotic property can be greatly promoted using sanitation degree.
Patent Office of the People's Republic of China was on 2 15th, 2017 hairs for disclosing an a kind of low-density high-mechanic sponge and manufacture craft
Bright patent application document, application publication number CN106397711A, the patent of invention is by reducing the expansion density of sponge so that
Required production material is greatly decreased when producing the sponge of same volume, reduces production cost, has on the other hand selected polyethers
Polyalcohol and polymer polyatomic alcohol improve the hardness of sponge, avoid because density is too low and caused by physical property decline ask
Topic.But its still suffer from the preparation process of sponge it is caused pollution it is larger, artificial high polymer is difficult to degrade, and foaming agent was foaming
People is damaged in journey, environment is polluted and does not possess the problem of antibiotic property.
The content of the invention
Too high to solve above-specified high density sponge production cost, low-density sponge mechanical property is poor can not to meet seat cushion sea
Continuous standard, and caused pollution is larger in the preparation process of sponge at present, artificial high polymer is difficult to degrade, and foaming agent was foaming
People is damaged in journey, environment is polluted and does not possess the problem of antibiotic property, there is provided a kind of composition natural degradable,
Nature, which can digest, will not cause that environmental pollution, preparation method are safe and harmless and resilience is good, compression set value is low,
With the environment-friendly antibacterial sponge of excellent antibacterial performance and its preparation technology.
It is a further object of the present invention to provide a kind of preparation technology of environment-friendly antibacterial sponge.
The present invention to achieve the above object, using following technical scheme：A kind of environment-friendly antibacterial sponge, the environment-friendly antibacterial sea
Continuous preparing raw material includes the material of following parts by weight：Small molecule chitosan 60-70 parts, guar hydroxypropyltrimonium chlorination
Ammonium 35-45 parts, sodium sulfate of polyethenoxy ether of fatty alcohol 0.45-0.95 parts, lauryl sodium sulfate 2.8-3.8 parts, glycerine 1-3
Part, boric acid 0.15-1 parts.
Preferably, the preparing raw material of the environment-friendly antibacterial sponge includes the material of following parts by weight：Small molecule shell gathers
Sugared 63-65 parts, guar hydroxypropyltrimonium ammonium chloride 35-40 parts, sodium sulfate of polyethenoxy ether of fatty alcohol 0.55-0.75 parts,
Lauryl sodium sulfate 3.2-3.5 parts, glycerine 1.5-2.5 parts, boric acid 0.45-0.60 parts.
Preferably, the method system that the small molecule chitosan is crushed by chitosan of the deacetylation more than 80% through physics
Standby, its preparation technology comprises the following steps：
a）Chitosan is dissolved in dilute acetic acid solution, the acetate concentration of dilute acetic acid solution is 5-10%, and dilute acetic acid solution dosage controls
Chitosan concentration is 1-2%, obtains chitosan acetic acid solution；
b）To step a）The chitosan acetic acid solution of gained applies ultrasonic radiation, radiated time 6-8h, and radiation obtains small after terminating
Molecular chitosan acetic acid solution；
c）By step b）The small molecule chitosan acetic acid solution of gained is neutralized to neutrality with ammoniacal liquor, and ammoniacal liquor is then slowly added dropwise to small
Molecular chitosan no longer separates out, and filter drying arrives small molecule chitosan.
Preferably, the step b）The ultrasonic power of middle ultrasonic radiation is 300-320W, ultrasonic frequency 1-
15MHz。
Preferably, the guar hydroxypropyltrimonium ammonium chloride is 2.2 × 10 from molecular weight6-2.4×106。
A kind of preparation technology of environment-friendly antibacterial sponge, it is characterised in that the preparation technology includes following preparation process：
1）Small molecule chitosan loaded on the acetum in container, being slowly added to 1% thereto and is stirred, until small point
Seed chitosan continues to stir 15-20min after being completely dissolved, and is then slowly added to 1% sodium hydroxide solution, until solution ph
For 6.8-7.2, separate out and be filtrated to get small molecule chitosan gel rubber；
2）By step 1）Obtained small molecule chitosan gel rubber is configured to the gel that mass fraction is 2% after being washed with deionized water
The aqueous solution, guar hydroxypropyltrimonium ammonium chloride powder is spent into ionized water and is configured to the aqueous solution that mass fraction is 2%, will
The aqueous solution mixes in equal volume with gel solution, stirs 25-30min, obtains mixed liquor；
3）To step 2）Sodium sulfate of polyethenoxy ether of fatty alcohol and lauryl sodium sulfate are added in obtained mixed liquor, is carried out fast
Speed stirring then adds glycerine and carries out even bubble stirring of slowing down, stir 15-20min, obtain expanding foam solution to a large amount of foaming；
4）To step 3）Boric acid is slowly added dropwise in the expanding foam solution of gained, and is mixed slowly, stirs 25-30min, obtains end
Liquid；
5）By step 4）Obtained whole liquid is transferred to progress pre-freeze shaping under low temperature environment after standing, pre-freeze time 12-18h, obtain
To pre-freeze body, pre-freeze body is freeze-dried, the environment-friendly antibacterial sponge is obtained after freeze-dried 17-25h.
Preferably, step 1）With step 2）The rotating speed of the stirring is 50-60r/min, step 3）Described quickly stirs
Mix rotating speed is 250-300r/min, and the even bubble speed of agitator that slows down is 120-150r/min.
Preferably, step 5）The low temperature environment is 5-10 DEG C, and the freeze-drying is divided into three phases：（I）Pre-freeze
2-3 hours, temperature are -20~-35 DEG C；（II）Low pressure dries 12-18 hours, and temperature is -20~-25 DEG C；（III）Heat up drying
3-4 hours, temperature are -5~5 DEG C.
Chitosan also known as chitosan, chemical name are Chitosan（1-4）- 2- amino-B-D glucose, it is
What the chitin being widely present by nature obtained by deacetylation.From 1859, after Frenchman Rouget is obtained first,
The premium properties such as biological functionality, compatibility, blood compatibility, security and the microbic resolvability of the natural polymer are each
Each industry extensive concern of row, but its slowly prominent application not in terms of sponge manufacturing field.
Guar hydroxypropyltrimonium ammonium chloride is a kind of with good filming, biocompatibility, biological degradability, day
So renewable and safe and non-toxic water-soluble swelling high polymer.
Because the cavernous body quality that list is prepared with chitosan is harder, the shortcomings of poor flexibility, easy fracture, thus chitosan be present
Even if material cavernous body possess the excellent specific properties such as good antibiotic property, microbial resistance, antiviral property and cancer resistance but always without
Method is widely used, and in the present invention, the mixing of guar hydroxypropyltrimonium ammonium chloride is added into chitosan so that sponge base
Body flexibility rises, while increases the water imbibition of cavernous body, water retention, when chitosan in such as present invention and guar gum hydroxypropyl trimethylammonium
Ammonium chloride component ratio is approximately 6：The water imbibition of sponge, water retention and flexibility index reach peak value when 4, and with glycerine
Addition can further lift water imbibition, water retention and the flexibility index of sponge, this is due to that glycerol molecule can disperse
And between embedded chitosan and the macromolecular of guar hydroxypropyltrimonium ammonium chloride mixed system, weaken molecule hydrogen bond, to mixed
Macromolecular structure in zoarium system has certain adjustment effect, and can increase chitosan macromolecular chain after glycerol molecule insertion
Relative length, form thread tissue, further improve sponge flexibility.
The present invention has done further optimization processing to chitosan material simultaneously, uses the shell of Ultrasonic Radiation HMW
Glycan, high molecular weight chitosan is set to be broken into small molecule chitosan using the method for ultrasonic disruption, compared to HMW shell
Glycan, small molecule chitosan are made after cavernous body due to its caused small molecule effect, and it forms combination stability after cavernous body
It is higher and the problems such as be not in hardened, matter crisp poor toughness, the elasticity and recoverable force of cavernous body are improved, to its flexibility
There is larger lifting, greatly optimize the usage comfort of the cavernous body of its generation.
The addition of boric acid can improve the flexibility of sponge, but can cause under water imbibition and water retention when addition is bigger than normal
Drop, this is due to can be with the production of guar hydroxypropyltrimonium ammonium chloride, the activity hydroxy of glycerine after boric acid adds mixed system
Raw coordination, when addition increases, coordination cross-linked degree greatly increases, and will cause mutually to bond between sponge inner pore, hole wall increases
Thickness, number of pores are reduced, and the compaction rate of sponge improves.
In addition biography instead of with sodium sulfate of polyethenoxy ether of fatty alcohol and lauryl sodium sulfate in technical solution of the present invention
The potassium oleate of system, ammonium sulfate etc. easily cause pollution or produce dysgenic foaming agent, the more value of environmental protection to human body.Dodecane
Base sodium sulphate is a kind of anion surfactant, belongs to surfactant-based foaming agent, can effectively reduce the surface of liquid
Tension force simultaneously arranges in liquid film surface electric double layer and surrounds air, forms bubble, then by single isolated bubbles and then forms foam group, has
There is extremely strong foaming capacity, and biological degradability degree can degrade greatly in recovery more than 90% and avoid polluting；Fat
Alcohol polyethenoxy ether sodium sulfate also known as ethoxylated alkyl sulfate, fatty alcohol-ether sodium sulfate, be equally a kind of anion table
Face activating agent, it is very gentle to human body, and be more than 50 DEG C or under mildly acidic conditions decomposable asymmetric choice net, that is, hydrolyze, production
Raw nuisanceless material, thus pollution environment also can be dramatically avoided in recovery.
And the addition of boric acid enables to the anti-microbial property of sponge further to improve, because the boron atom in boric acid is short of electricity
Sub- atom, complexation reaction easily occurs with polyols such as glycerine, guar hydroxypropyltrimonium ammonium chlorides, stable match somebody with somebody occurs
Compound and H+, enhancing is acid, promotes-the NH of chitosan2It is converted into-NH3 +Ion radical, easily contacted with the cell membrane of bacterium and with it is thin
The substance reactions such as peptide glycan, protein on cell wall, the barrier that bacterium depends on for existence is destroyed, cell breakage is occurred and ultimately results in
Cell death.
The beneficial effects of the invention are as follows：The raw materials used present invention is pollution-free, non-harmful material, more friendly to environment
It is good；High molecular weight chitosan is broken into small molecule chitosan using the method for ultrasonic disruption, gather compared to HMW shell
Sugar, it is higher and the problems such as be not in hardened, matter crisp poor toughness that it forms combination stability after cavernous body, improves cavernous body
Elasticity and recoverable force, there is larger lifting to its flexibility, greatly optimize the usage comfort of the cavernous body of its generation；
Obtained cavernous body is using chitosan as main base, but its flexibility, resilience are high, and compression set value is low, has
Very good mechanical property；Obtained cavernous body has good anti-microbial property, has antibacterial, sterilizing function, makes to make with it
Standby each object is relatively sanitary.
Embodiment
Embodiment 1
The preparation of small molecule chitosan：
a）Chitosan is dissolved in dilute acetic acid solution, the acetate concentration of dilute acetic acid solution is 5%, dilute acetic acid solution dosage control shell
Glycan concentration is 1%, obtains chitosan acetic acid solution；
b）To step a）The chitosan acetic acid solution of gained applies ultrasonic radiation, radiated time 6h, and radiation obtains small point after terminating
Seed chitosan acetic acid solution；
c）By step b）The small molecule chitosan acetic acid solution of gained is neutralized to neutrality with ammoniacal liquor, and ammoniacal liquor is then slowly added dropwise to small
Molecular chitosan no longer separates out, and filter drying arrives small molecule chitosan；
A kind of preparation technology of the antibacterial sponge of environment-friendly degradable, the preparation technology include following preparation process：
1）Small molecule chitosan loaded on the glacial acetic acid solution in container, being slowly added to 1% thereto and is stirred, stirring turns
Speed is 50r/min, until small molecule chitosan continues to stir 20min, speed of agitator 50r/min after being completely dissolved, it is then slow
The sodium hydroxide solution of slow addition 1%, until solution ph is 6.8, separates out and is filtrated to get small molecule chitosan gel rubber；
2）By step 1）Obtained small molecule chitosan gel rubber is configured to the gel that mass fraction is 2% after being washed with deionized water
The aqueous solution, guar hydroxypropyltrimonium ammonium chloride powder is spent into ionized water and is configured to the aqueous solution that mass fraction is 2%, will
The aqueous solution mixes in equal volume with gel solution, stirs 30min, speed of agitator 50r/min, obtains mixed liquor；
3）To step 2）Sodium sulfate of polyethenoxy ether of fatty alcohol and lauryl sodium sulfate are added in obtained mixed liquor, is carried out fast
Speed stirring rotating speed 250r/min, then adds glycerine and carries out even bubble stirring of slowing down, slow down even bubble speed of agitator to a large amount of foaming
For 120r/min, mixing time 20min, expanding foam solution is obtained；
4）To step 3）Boric acid is slowly added dropwise in the expanding foam solution of gained, and is mixed slowly, stirs 25min, mixing speed
25r/min, obtain whole liquid；
5）By step 4）Obtained whole liquid is transferred to progress pre-freeze shaping under 5 DEG C of low temperature environments after standing, pre-freeze time 12h, obtain
To pre-freeze body, pre-freeze body is freeze-dried, freeze-drying is divided into three phases：（I）Pre-freeze 2 hours, temperature are -35 DEG C；
（II）Low pressure is dried 12 hours, and temperature is -25 DEG C；（III）Heating is dried 3 hours, and temperature is -5 DEG C, and freeze-drying obtains after terminating
To the antibacterial sponge of the environment-friendly degradable.
The raw materials used parts by weight of the present embodiment are：60 parts of small molecule chitosan, guar hydroxypropyltrimonium chlorination
35 parts of ammonium, 0.95 part of sodium sulfate of polyethenoxy ether of fatty alcohol, 3.8 parts of lauryl sodium sulfate, 1 part of glycerine, 1 part of boric acid.
Embodiment 2
The preparation of small molecule chitosan：
a）Chitosan is dissolved in dilute acetic acid solution, the acetate concentration of dilute acetic acid solution is 10%, dilute acetic acid solution dosage control shell
Glycan concentration is 1-2%, obtains chitosan acetic acid solution；
b）To step a）The chitosan acetic acid solution of gained applies ultrasonic radiation, radiated time 6h, and radiation obtains small point after terminating
Seed chitosan acetic acid solution；
c）By step b）The small molecule chitosan acetic acid solution of gained is neutralized to neutrality with ammoniacal liquor, and ammoniacal liquor is then slowly added dropwise to small
Molecular chitosan no longer separates out, and filter drying arrives small molecule chitosan；
A kind of preparation technology of the antibacterial sponge of environment-friendly degradable, the preparation technology include following preparation process：
1）Small molecule Chitosan powder loaded on the glacial acetic acid solution in container, being slowly added to 1% thereto and is stirred, stirred
Mix rotating speed is 60r/min, until small molecule chitosan continues to stir 15min, speed of agitator 60r/min after being completely dissolved, with
1% sodium hydroxide solution is slowly added to afterwards, until solution ph is 7.2, is separated out and is filtrated to get small molecule chitosan gel rubber；
2）By step 1）Obtained small molecule chitosan gel rubber is configured to the gel that mass fraction is 2% after being washed with deionized water
The aqueous solution, guar hydroxypropyltrimonium ammonium chloride powder is spent into ionized water and is configured to the aqueous solution that mass fraction is 2%, will
The aqueous solution mixes in equal volume with gel solution, stirs 25min, speed of agitator 60r/min, obtains mixed liquor；
3）To step 2）Sodium sulfate of polyethenoxy ether of fatty alcohol is added in obtained mixed liquor and lauryl sodium sulfate is carried out soon
Speed stirring rotating speed 300r/min, then adds glycerine and carries out even bubble stirring of slowing down, slow down even bubble speed of agitator to a large amount of foaming
For 150r/min, mixing time 15min, expanding foam solution is obtained；
4）To step 3）Boric acid is slowly added dropwise in the expanding foam solution of gained, and is mixed slowly, stirs 30min, mixing speed
30r/min, obtain whole liquid；
5）By step 4）Obtained whole liquid is transferred to progress pre-freeze shaping under 10 DEG C of low temperature environments after standing, pre-freeze time 18h, obtain
To pre-freeze body, pre-freeze body is freeze-dried, freeze-drying is divided into three phases：（I）Pre-freeze 3 hours, temperature are -35 DEG C；
（II）Low pressure is dried 18 hours, and temperature is -20 DEG C；（III）Heating is dried 4 hours, and temperature is 5 DEG C, and freeze-drying obtains after terminating
To the antibacterial sponge of the environment-friendly degradable.
The raw materials used parts by weight of the present embodiment are：70 parts of small molecule chitosan, guar hydroxypropyltrimonium chlorination
45 parts of ammonium, 0.45 part of sodium sulfate of polyethenoxy ether of fatty alcohol, 2.8 parts of lauryl sodium sulfate, 3 parts of glycerine, 0.15 part of boric acid.
Embodiment 3
The preparation of small molecule chitosan：
a）Chitosan is dissolved in dilute acetic acid solution, the acetate concentration of dilute acetic acid solution is 10%, dilute acetic acid solution dosage control shell
Glycan concentration is 2%, obtains chitosan acetic acid solution；
b）To step a）The chitosan acetic acid solution of gained applies ultrasonic radiation, radiated time 8h, and radiation obtains small point after terminating
Seed chitosan acetic acid solution；
c）By step b）The small molecule chitosan acetic acid solution of gained is neutralized to neutrality with ammoniacal liquor, and ammoniacal liquor is then slowly added dropwise to small
Molecular chitosan no longer separates out, and filter drying arrives small molecule chitosan；
A kind of preparation technology of the antibacterial sponge of environment-friendly degradable, the preparation technology include following preparation process：
1）Small molecule Chitosan powder loaded on the glacial acetic acid solution in container, being slowly added to 1% thereto and is stirred, stirred
Mix rotating speed is 60r/min, until small molecule chitosan continues to stir 15min, speed of agitator 60r/min after being completely dissolved, with
1% sodium hydroxide solution is slowly added to afterwards, until solution ph is 7.2, is separated out and is filtrated to get small molecule chitosan gel rubber；
2）By step 1）Obtained small molecule chitosan gel rubber is configured to the gel that mass fraction is 2% after being washed with deionized water
The aqueous solution, guar hydroxypropyltrimonium ammonium chloride powder is spent into ionized water and is configured to the aqueous solution that mass fraction is 2%, will
The aqueous solution mixes in equal volume with gel solution, stirs 30min, speed of agitator 50r/min, obtains mixed liquor；
3）To step 2）Sodium sulfate of polyethenoxy ether of fatty alcohol and lauryl sodium sulfate are added in obtained mixed liquor, is carried out fast
Speed stirring rotating speed 250r/min, then adds glycerine and carries out even bubble stirring of slowing down, slow down even bubble speed of agitator to a large amount of foaming
For 120r/min, mixing time 20min, expanding foam solution is obtained；
4）To step 3）Boric acid is slowly added dropwise in the expanding foam solution of gained, and is mixed slowly, stirs 30min, mixing speed
25r/min, obtain whole liquid；
5）By step 4）Obtained whole liquid is transferred to progress pre-freeze shaping under 10 DEG C of low temperature environments after standing, pre-freeze time 18h, obtain
To pre-freeze body, pre-freeze body is freeze-dried, freeze-drying is divided into three phases：（I）Pre-freeze 3 hours, temperature are -35 DEG C；
（II）Low pressure is dried 18 hours, and temperature is -25 DEG C；（III）Heating is dried 4 hours, and temperature is -5 DEG C, and freeze-drying obtains after terminating
To the antibacterial sponge of the environment-friendly degradable.
The raw materials used parts by weight of the present embodiment are：63 parts of small molecule chitosan, guar hydroxypropyltrimonium chlorination
40 parts of ammonium, 0.55 part of sodium sulfate of polyethenoxy ether of fatty alcohol, 3.5 parts of lauryl sodium sulfate, 2.5 parts of glycerine, 0.60 part of boric acid.
Embodiment 4
The preparation of small molecule chitosan：
a）Chitosan is dissolved in dilute acetic acid solution, the acetate concentration of dilute acetic acid solution is 5%, dilute acetic acid solution dosage control shell
Glycan concentration is 2%, obtains chitosan acetic acid solution；
b）To step a）The chitosan acetic acid solution of gained applies ultrasonic radiation, radiated time 8h, and radiation obtains small point after terminating
Seed chitosan acetic acid solution；
c）By step b）The small molecule chitosan acetic acid solution of gained is neutralized to neutrality with ammoniacal liquor, and ammoniacal liquor is then slowly added dropwise to small
Molecular chitosan no longer separates out, and filter drying arrives small molecule chitosan；
A kind of preparation technology of the antibacterial sponge of environment-friendly degradable, the preparation technology include following preparation process：
1）Small molecule Chitosan powder loaded on the glacial acetic acid solution in container, being slowly added to 1% thereto and is stirred, stirred
Mix rotating speed is 60r/min, until small molecule chitosan continues to stir 20min, speed of agitator 50r/min after being completely dissolved, with
1% sodium hydroxide solution is slowly added to afterwards, until solution ph is 7.1, is separated out and is filtrated to get small molecule chitosan gel rubber；
2）By step 1）Obtained small molecule chitosan gel rubber is configured to the gel that mass fraction is 2% after being washed with deionized water
The aqueous solution, guar hydroxypropyltrimonium ammonium chloride powder is spent into ionized water and is configured to the aqueous solution that mass fraction is 2%, will
The aqueous solution mixes in equal volume with gel solution, stirs 30min, speed of agitator 60r/min, obtains mixed liquor；
3）To step 2）Sodium sulfate of polyethenoxy ether of fatty alcohol and lauryl sodium sulfate are added in obtained mixed liquor, is carried out fast
Speed stirring rotating speed 300r/min, then adds glycerine and carries out even bubble stirring of slowing down, slow down even bubble speed of agitator to a large amount of foaming
For 120r/min, mixing time 15min, expanding foam solution is obtained；
4）To step 3）Boric acid is slowly added dropwise in the expanding foam solution of gained, and is mixed slowly, stirs 30min, mixing speed
35r/min, obtain whole liquid；
5）By step 4）Obtained whole liquid is transferred to progress pre-freeze shaping under 5 DEG C of low temperature environments after standing, pre-freeze time 18h, obtain
To pre-freeze body, pre-freeze body is freeze-dried, freeze-drying is divided into three phases：（I）Pre-freeze 2 hours, temperature are -20 DEG C；
（II）Low pressure is dried 18 hours, and temperature is -20 DEG C；（III）Heating is dried 4 hours, and temperature is -5 DEG C, and freeze-drying obtains after terminating
To the antibacterial sponge of the environment-friendly degradable.
The raw materials used parts by weight of the present embodiment are：65 parts of small molecule chitosan, guar hydroxypropyltrimonium chlorination
35 parts of ammonium, 0.75 part of sodium sulfate of polyethenoxy ether of fatty alcohol, 3.2 parts of lauryl sodium sulfate, 1.5 parts of glycerine, 0.45 part of boric acid.
Embodiment 5
The preparation of small molecule chitosan：
a）Chitosan is dissolved in dilute acetic acid solution, the acetate concentration of dilute acetic acid solution is 5%, dilute acetic acid solution dosage control shell
Glycan concentration is 2%, obtains chitosan acetic acid solution；
b）To step a）The chitosan acetic acid solution of gained applies ultrasonic radiation, radiated time 6h, and radiation obtains small point after terminating
Seed chitosan acetic acid solution；
c）By step b）The small molecule chitosan acetic acid solution of gained is neutralized to neutrality with ammoniacal liquor, and ammoniacal liquor is then slowly added dropwise to small
Molecular chitosan no longer separates out, and filter drying arrives small molecule chitosan；
A kind of preparation technology of the antibacterial sponge of environment-friendly degradable, the preparation technology include following preparation process：
1）Small molecule Chitosan powder loaded on the glacial acetic acid solution in container, being slowly added to 1% thereto and is stirred, stirred
Mix rotating speed is 60r/min, until small molecule chitosan continues to stir 15min, speed of agitator 60r/min after being completely dissolved, with
1% sodium hydroxide solution is slowly added to afterwards, until solution ph is 7.2, is separated out and is filtrated to get small molecule chitosan gel rubber；
2）By step 1）Obtained small molecule chitosan gel rubber is configured to the gel that mass fraction is 2% after being washed with deionized water
The aqueous solution, guar hydroxypropyltrimonium ammonium chloride powder is spent into ionized water and is configured to the aqueous solution that mass fraction is 2%, will
The aqueous solution mixes in equal volume with gel solution, stirs 30min, speed of agitator 50r/min, obtains mixed liquor；
3）To step 2）Sodium sulfate of polyethenoxy ether of fatty alcohol is added in obtained mixed liquor and lauryl sodium sulfate is carried out soon
Speed stirring rotating speed 300r/min, then adds glycerine and carries out even bubble stirring of slowing down, slow down even bubble speed of agitator to a large amount of foaming
For 120r/min, mixing time 15min, expanding foam solution is obtained；
4）To step 3）Boric acid is slowly added dropwise in the expanding foam solution of gained, and is mixed slowly, stirs 25min, mixing speed
35r/min, obtain whole liquid；
5）By step 4）Obtained whole liquid is transferred to progress pre-freeze shaping under 5 DEG C of low temperature environments after standing, pre-freeze time 18h, obtain
To pre-freeze body, pre-freeze body is freeze-dried, freeze-drying is divided into three phases：（I）Pre-freeze 2 hours, temperature are -20 DEG C；
（II）Low pressure is dried 18 hours, and temperature is -20 DEG C；（III）Heating is dried 4 hours, and temperature is -5 DEG C, and freeze-drying obtains after terminating
To the antibacterial sponge of the environment-friendly degradable.
The raw materials used parts by weight of the present embodiment are：65 parts of small molecule chitosan, guar hydroxypropyltrimonium chlorination
39 parts of ammonium, 0.65 part of sodium sulfate of polyethenoxy ether of fatty alcohol, 3.35 parts of lauryl sodium sulfate, 2 parts of glycerine, 0.5 part of boric acid.
Above-described embodiment 1-5 is detected：
1）Water imbibition detects：The antibacterial sponge water imbibition of environment-friendly degradable obtained by embodiment 1-5 is more than 1900% after testing；
2）Water retention detects：The antibacterial sponge water retention of environment-friendly degradable obtained by embodiment 1-5 is more than 950% after testing；
3）Moisture-vapor transmission detects：The antibacterial sponge moisture-vapor transmission of environment-friendly degradable obtained by embodiment 1-5 is equal after testing
More than 70%；
4）Flexibility, elasticity and restorative detection：After testing flexible 330 ° of degradable high-elastic sponge obtained by embodiment 1-5 with
It is upper and bending be even rolled into it is bar-shaped after can recover in a short time, any breakage in surface has even without folding line is left
Very good flexibility, elasticity and restorative；
5）Anti-microbial property detects：Anti-microbial property test is carried out to embodiment 1-5, from Gram positive staphylococcus aureus and
Two kinds of bacteriums are suspended in 100 μm of ol/L of concentration, the phosphate of pH=7 by Gram-E. coli respectively as test strain
Bacterium solution needed for being prepared in buffer solution, bacterium solution is dropped on the antibacterial sponge of the environment-friendly degradable obtained by embodiment, and will be another
The antibacterial sponge of environment-friendly degradable obtained by piece embodiment is superimposed in the form of sandwich, is subject to sterile foundary weight pressure and is ensured carefully
Bacterium fully contacts the antibacterial sponge of the environment-friendly degradable to be measured obtained by embodiment, will receive antibiotic property survey after contacting 5-30min
The antibacterial sponge of environment-friendly degradable obtained by the embodiment of examination is put into the sterile hypo solution that concentration is 0.02mol/L
Centrifuge tube in and vibrate 2min, rear 100 μm of ol/L, the above-mentioned solution of phosphate buffer serial dilution of pH=7, during by being
The solution of time is placed in culture medium, the incubated 24h under the conditions of 37 DEG C, is finally counted surviving bacteria colony counts and is calculated anti-
Bacterium rate；Test obtains result, and the antibacterial sponge of the environment-friendly degradable obtained by above example is thin by two kinds in 5min
Bacterium all kills, and has very excellent antibiotic property.
Claims (8)
1. a kind of environment-friendly antibacterial sponge, it is characterised in that the preparing raw material of the environment-friendly antibacterial sponge includes following parts by weight
Material：Small molecule chitosan 60-70 parts, guar hydroxypropyltrimonium ammonium chloride 35-45 parts, AEO sulphur
Sour sodium 0.45-0.95 parts, lauryl sodium sulfate 2.8-3.8 parts, glycerine 1-3 parts, boric acid 0.15-1 parts.
2. a kind of environment-friendly antibacterial sponge according to claim 1, it is characterised in that the preparation of the environment-friendly antibacterial sponge is former
Material includes the material of following parts by weight：Small molecule chitosan 63-65 parts, guar hydroxypropyltrimonium ammonium chloride 35-40 parts,
Sodium sulfate of polyethenoxy ether of fatty alcohol 0.55-0.75 parts, lauryl sodium sulfate 3.2-3.5 parts, glycerine 1.5-2.5 parts, boric acid
0.45-0.60 parts.
3. a kind of environment-friendly antibacterial sponge according to claim 2, it is characterised in that the small molecule chitosan is by deacetylated
Prepared by the method that chitosan of the degree more than 80% crushes through physics, its preparation technology comprises the following steps：
a）Chitosan is dissolved in dilute acetic acid solution, the acetate concentration of dilute acetic acid solution is 5-10%, and dilute acetic acid solution dosage controls
Chitosan concentration is 1-2%, obtains chitosan acetic acid solution；
b）To step a）The chitosan acetic acid solution of gained applies ultrasonic radiation, radiated time 6-8h, and radiation obtains small after terminating
Molecular chitosan acetic acid solution；
c）By step b）The small molecule chitosan acetic acid solution of gained is neutralized to neutrality with ammoniacal liquor, and ammoniacal liquor is then slowly added dropwise to small
Molecular chitosan no longer separates out, and filter drying arrives small molecule chitosan.
A kind of 4. environment-friendly antibacterial sponge according to claim 3, it is characterised in that the step b）Middle ultrasonic radiation surpasses
Acoustic power is 300-320W, ultrasonic frequency 1-15MHz.
A kind of 5. environment-friendly antibacterial sponge according to claim 2, it is characterised in that the guar hydroxypropyltrimonium chlorine
It is 2.2 × 10 to change ammonium from molecular weight6-2.4×106。
A kind of 6. preparation technology of environment-friendly antibacterial sponge as described in any one in claim 1 to 5, it is characterised in that institute
Stating preparation technology includes following preparation process：
1）Small molecule chitosan loaded on the acetum in container, being slowly added to 1% thereto and is stirred, until small point
Seed chitosan continues to stir 15-20min after being completely dissolved, and is then slowly added to 1% sodium hydroxide solution, until solution ph
For 6.8-7.2, separate out and be filtrated to get small molecule chitosan gel rubber；
2）By step 1）Obtained small molecule chitosan gel rubber is configured to the gel that mass fraction is 2% after being washed with deionized water
The aqueous solution, guar hydroxypropyltrimonium ammonium chloride powder is spent into ionized water and is configured to the aqueous solution that mass fraction is 2%, will
The aqueous solution mixes in equal volume with gel solution, stirs 25-30min, obtains mixed liquor；
3）To step 2）Sodium sulfate of polyethenoxy ether of fatty alcohol and lauryl sodium sulfate are added in obtained mixed liquor, is carried out fast
Speed stirring then adds glycerine and carries out even bubble stirring of slowing down, stir 15-20min, obtain expanding foam solution to a large amount of foaming；
4）To step 3）Boric acid is slowly added dropwise in the expanding foam solution of gained, and is mixed slowly, stirs 25-30min, obtains end
Liquid；
5）By step 4）Obtained whole liquid is transferred to progress pre-freeze shaping under low temperature environment after standing, pre-freeze time 12-18h, obtain
To pre-freeze body, pre-freeze body is freeze-dried, the environment-friendly antibacterial sponge is obtained after freeze-dried 17-25h.
A kind of 7. preparation technology of environment-friendly antibacterial sponge according to claim 6, it is characterised in that step 1）With step 2）
The rotating speed of the stirring is 50-60r/min, step 3）Described quick speed of agitator is 250-300r/min, and the even bubble that slows down stirs
Mix rotating speed is 120-150r/min.
A kind of 8. preparation technology of environment-friendly antibacterial sponge according to claim 6, it is characterised in that step 5）The low temperature
Environment is 5-10 DEG C, and the freeze-drying is divided into three phases：（I）Pre-freeze 2-3 hours, temperature are -20~-35 DEG C；（II）It is low
Dry 12-18 hours are pressed dry, temperature is -20~-25 DEG C；（III）3-4 hours are dried in heating, and temperature is -5~5 DEG C.
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| CN112006471A (en) * | 2020-08-31 | 2020-12-01 | 江苏金太阳家用纺织品有限公司 | Mattress with adjustable hardness and left and right partitions and manufacturing method thereof |
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