CN108587167A - A kind of infusion medical resin and preparation method - Google Patents
A kind of infusion medical resin and preparation method Download PDFInfo
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- CN108587167A CN108587167A CN201810241387.8A CN201810241387A CN108587167A CN 108587167 A CN108587167 A CN 108587167A CN 201810241387 A CN201810241387 A CN 201810241387A CN 108587167 A CN108587167 A CN 108587167A
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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
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2203/02—Applications for biomedical use
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention discloses a kind of infusion medical resins and preparation method, are related to medical resin correlative technology field；Infusion medical treatment resin includes component：Zinc stearate, lauryl sodium sulfate, stabilizer, stearic acid, age resister, silicone adhesive, Archon, chloromethyl ether, ferric trichloride, sulfuric acid, methanol, vaseline, zinc carbonate, stearic acid, salicylic acid, clay, dibutyl ester, dioctyl ester, high-phenylethylene, nano modification alkyd resin；The medical resin indices of present invention infusion meet quality standard, and are better than the existing articles for use in market, and infusion is good with medical resin compatible, safe and non-toxic, harmful substance residual quantity is small, high-fire resistance, toughness, the stabilization to light and heat.
Description
Technical field：
The present invention relates to medical resin correlative technology fields, and in particular to a kind of infusion medical resin and preparation method.
Background technology：
Depressed, the excess capacity in market economy, downstream demand diversification, high-quality, safety and environmental protection require increasingly to improve
Complex environment under, production of resins enterprise only constantly reduces energy consumption by technological innovation, reduces pollution, reduces cost,
Thus there is PVC paste resin, CPVC resins, vinyl chloride-vinyl acetate resin, the third resin of chlorine, blending tree in the product function for improving product quality
Fat, high polymerization degree resin, matting resin, medical grade resins etc. are resin dedicated, to meet the market demand.
Wherein medical grade resins are mainly used in the pipeline of disposable transfusion device, blood transfusion apparatus and various medical extracorporal circulatory systems
With parts etc..As medical grade resins, it is desirable that it is without toxicant, stripping property is small, bio-compatible is on very good terms (such as hemolytic
It is low, anticoagulant property is good, hemoglobin denaturation degree is small etc.).Therefore, compared with universal resin, to the requirement of medical grade naval stores
Then more stringent, the residual quantity for essentially consisting in the noxious materials such as vinyl chloride, toluene, the nitrile group in medical grade resins requires to be micro-
Amount or zero.
With the improvement of people ' s living standards and the progress of medical technology, more and more disposable medical equipment are extensive
Applied to medical domain, develop in western developed country particularly rapid.The research of medical grade resins is concentrated mainly on resin modified
Aspect can reduce the toxicity of product by modification.
In terms of current statistical data, medical resin is applied to the quantity in medical field in China and only accounts for gross domestic product
1.2% or so, it can be seen that the annual requirement of medical resin be 150,000~300,000 t.But with domestic aging of population
With being gradually expanded for medical field, the demand to medical article will increasingly increase.In addition, as people are to consumption quality and body
The increasingly attention of health, toy for children raw material also gradually turn to medical grade resins, to improve the need of medical grade resins
Seek growth rate.
Invention content：
Technical problem to be solved by the present invention lies in provide a kind of infusion medical resin and preparation method, infusion doctor
Treatment resin compatible is good, safe and non-toxic, harmful substance residual quantity is small, high-fire resistance, toughness, the stabilization to light and heat.
It is realized using following technical scheme using the technical problems to be solved by the invention：
A kind of infusion is as follows with medical resin, including specific technical solution：Infusion provided by the invention medical resin, packet
Include following mass fraction component：1-2 parts of zinc stearate, 4-9 parts of lauryl sodium sulfate, 1.5-5 parts of stabilizer, stearic acid 0.5-
0.7 part, 1-4 parts of age resister, 77-94 parts of silicone adhesive, 4-12 parts of Archon, 0.5-5 parts of chloromethyl ether, 1-6 parts of ferric trichloride, sulfuric acid
6-13 parts, 4-12 parts of methanol, 15-20 parts of vaseline, 11-18 parts of zinc carbonate, 6-15 parts of stearic acid, 9-17 parts of salicylic acid, clay
30-40 parts, 5-10 parts of dibutyl ester, 10-17 parts of dioctyl ester, 12-19 parts of high-phenylethylene, 6-13 parts of nano modification alkyd resin.
The stabilizer is made from the following raw materials in parts by weight：3-5 parts of cattail Down Fiber element, carboxymethyl cellulose 0.6-
1.0 parts, 0.3-0.5 parts of trifluoro propyl methyl cyclotrisiloxane, 0.5-3 parts of dwarf lilyturf tuber total saponins, 1.5-3 parts of sodium alginate, bay
Sour monoglyceride 0.2-2 parts, 12-21 parts of water；The preparation method of stabilizer is first by cattail Down Fiber element and carboxymethyl cellulose
It is added to the water stirring and heats 50-70 DEG C up to being completely dissolved, dwarf lilyturf tuber total saponins, sodium alginate and trifluoro propyl first is then added
Basic ring trisiloxanes and lauric monoglyceride 800-1000r/min stir 0.5-1h, finally put into 70-80 DEG C of breast in mulser
Change reaction 2-4h, rear take out is put into quick freeze 2-6h in -50-100 DEG C of environment, takes out to put to room temperature afterwards and restore to room at once
Up to stabilizer after temperature.
The age resister is made from the following raw materials in parts by weight：4-13 parts of glycyrrhiza total flavonoid, ginkgo biloba p.e 4-12
Part, 5-20 parts of barren wort total chromocor, 7-15 parts of astragaloside, 0.5-1 parts of polydimethyl diallyl ammonium chloride, rilanit special
1-2 parts, 0.5-1 parts of kayexalate, 0.5-1 parts of N methyldiethanol amine；Preparation method：By glycyrrhiza total flavonoid, silver
Apricot leaf extract, barren wort total chromocor, astragaloside are added in 60-90% ethanol solutions and 600-1000rpm/min stirrings are molten
Solution is uniform, polydimethyl diallyl ammonium chloride is added into lysate, in microwave frequency 2450MHz, power after being sufficiently mixed
Microwave treatment 5-30min under 700W, adds rilanit special, kayexalate and N methyldiethanol amine, and mixing is equal
Continue microwave treatment 5min after even, is transferred to sealing and standing 3h in 0-5 DEG C of environment immediately after microwave treatment, is then heated to
125-130 DEG C of heat preservation mixing 10-30min, 6-8 parts of 0-5 DEG C of cold water are added into gained mixture, 1h is stood after being sufficiently mixed,
Then be heated to reflux state heat preservation mixing 5-30min, after by mixture as rotation volatilize distilling machinery in, disperse extra volatilization
Property ingredient, rear cooled to room temperature is finally sent into spray dryer, and dry gained particle is age resister.
The present invention also provides a kind of infusion preparation methods of medical resin, include the following steps：
(1) nitration mixture that silicone adhesive, lauryl sodium sulfate, nano modification alkyd resin are added to 8-10 times of its weight is molten
In liquid, it is 3-4 that the nitration mixture, which is by mass ratio,:The carbonic acid of 1 40-50% and the acetum composition of 70-80%, in 50-
Ultrasound 17-20 minutes at 60 DEG C, filtering are dried in vacuo 30-40 minutes at washing precipitation 2-3 times, 70-76 DEG C, obtain material I；
(2) 40-50% for taking I weight of above-mentioned material is mixed with zinc stearate, stabilizer, stearic acid, age resister, is added
Enter into the methanol solution of 3-5 times of mixture weight, it is 100-120 minutes ultrasonic, it is sent into reaction kettle, is passed through helium, increase temperature
Degree is 120-127 DEG C, insulation reaction 35-40 hours, and product is filtered, washed 3-4 times with 95% ethyl alcohol, be placed in 70-80 by discharging
DEG C baking oven in dry to constant weight, obtain material II；
(3) remaining material I, Archon, chloromethyl ether, ferric trichloride are mixed, is added to the bigcatkin willow of 6-7 times of mixture weight
It is 100-110 minutes ultrasonic in acid, it is sent into reaction kettle, is passed through helium, it is 68-70 DEG C to increase temperature, and insulation reaction 35-40 is small
When, product is filtered, is washed 3-4 times with 95% ethyl alcohol by discharging, is placed in 70-80 DEG C of baking oven and is dried to constant weight, obtains material
Ⅲ；
(4) it takes vaseline, zinc carbonate, stearic acid, clay, dibutyl ester to be added in the methanol solution of its weight 17-20%, stirs
Mixing 20-30 minutes is mixed, the sulfuric acid of a concentration of 3-6mol/L is added dropwise, adjusting pH is 5-6, is passed through helium, is heated to boiling, and is kept
Boiling 57-60 minutes, discharging, is cooled to room temperature, obtains material IV；
(5) above-mentioned material II, material III, material IV are mixed, is preheated 4-6 minutes at 87-90 DEG C, increasing temperature is
155-160 DEG C, insulated and stirred 3-4 minutes, filtering away big impurity material must be infused with medical resin basis bottom material；
(6) above-mentioned infusion is mixed with medical resin basis bottom material with remaining each raw material, is stirred evenly, homogeneous, refinery, it is high
200-360 DEG C of heat refining 2-5h of heating is up to the medical resin raw material of infusion in warm stove；
(7) step 6 is infused after and is put into resin processing draft machine with medical resin raw material, variously-shaped or face is prepared into
The medical resin articles for use of the infusion of color, and naval stores is post-processed.
Post-processing approach is described in above-mentioned steps 7：
(1) infusion obtained is passed through in the second sink and is bathed with medical resin articles for use, it is 35~40 DEG C of temperature to neutralize bath
Dilute sulfuric acid, the mass fraction of dilute sulfuric acid is 0.5~0.8%；
(2) it washes, by step 1, treated that infusion is washed with medical resin articles for use in third sink, and washing is warm
Degree is 55~65 DEG C；
(3), the infusion after step 2 being washed carries out hot gas spring with medical treatment resin articles for use, oils and drying and processing, that is, is made
The medical resin articles for use of infusion.
Wherein, in step 3, in the hot gas spring step, hot gas spring multiple be 2~3 times, hot gas spring temperature be 80~
100℃；Glycerol concentration is 2~4g/L in the process that oils, and oil applying rate is 0.12~0.25%, and temperature is 20~26 DEG C；
Drying temperature is 70~80 DEG C in the baking operation, and drying time is 14~18 hours.
The present invention is infused is with medical resin advantages and beneficial effects：
1, the present invention is in view of the deficienciess of the prior art, prepare a kind of medical resin of infusion, infusion medical treatment resin
Middle addition stabilizer can dramatically increase the plasticity and stability of the medical resinous polymer of infusion.
2, present invention infusion uses medical resin to be used as material by the way that Archon is added, and the microcosmic open structure in matrix is made to tend to
Densification further increases the obdurability of the medical resin of infusion；In addition Archon is the medical resin processing aid of infusion, for promoting
Into the infusion plasticizing of medical resin, the merging of bubble is prevented, to obtain even foaming, the infusion with good appearance cures
Resin is treated, the light and thermally stable and chemicals stability of the medical resin of infusion are remarkably improved.
3, the present invention use environmental friendly, simple using equipment, easy to operate, manufacturing cost is low, to improving use of being infused
The medical various performances of resin articles for use have very high practical value.
4, the medical resin articles for use of the infusion for preparing of the present invention, compatibility is good, high resistance to hot/cold, toughness, to light and heat
It is stable, safe and non-toxic, can still keep the good medical resin compatible of infusion in harsh environment, is high resistance to hot/cold, toughness, right
The stability of light and heat.
Specific implementation mode：
In order to make the technical means, the creative features, the aims and the efficiencies achieved by the present invention be easy to understand, tie below
Specific embodiment is closed, the present invention is further explained.
Embodiment 1：
A kind of infusion medical resin and preparation method；
The technical problems to be solved by the invention are realized using following technical scheme：
A kind of infusion is as follows with medical resin, including specific technical solution：Infusion provided by the invention medical resin, packet
Include following mass fraction component：It is 1 part of zinc stearate, 4 parts of lauryl sodium sulfate, 1.5 parts of stabilizer, 0.5 part of stearic acid, anti-ageing
3 parts of agent, 77 parts of silicone adhesive, 4 parts of Archon, 0.5 part of chloromethyl ether, 4 parts of ferric trichloride, 6 parts of sulfuric acid, 4 parts of methanol, vaseline 15
Part, 11 parts of zinc carbonate, 6 parts of stearic acid, 9 parts of salicylic acid, 30 parts of clay, 5 parts of dibutyl ester, 17 parts of dioctyl ester, 12 parts of high-phenylethylene,
6 parts of nano modification alkyd resin.
The stabilizer is made from the following raw materials in parts by weight：3 parts of cattail Down Fiber element, 0.6 part of carboxymethyl cellulose, three
0.3 part of fluoropropyl methyl cyclotrisiloxane, 0.5 part of dwarf lilyturf tuber total saponins, 1.5 parts of sodium alginate, 0.2 part of lauric monoglyceride,
15 parts of water；The preparation method of stabilizer is that cattail Down Fiber element and carboxymethyl cellulose are first added to the water stirring and heat 60 DEG C
Until being completely dissolved, dwarf lilyturf tuber total saponins, sodium alginate and trifluoro propyl methyl cyclotrisiloxane then is added and lauric acid list is sweet
Grease 800r/min stirs 0.8h, finally puts into 80 DEG C of emulsion reaction 2.5h in mulser, and rear take out is put into -100 DEG C at once
Quick freeze 2-6h in environment, it is rear take out put to room temperature restore to room temperature after up to stabilizer.
The age resister is made from the following raw materials in parts by weight：It is 10 parts of glycyrrhiza total flavonoid, 9 parts of ginkgo biloba p.e, excessive
13 parts of sheep leaves of pulse plants general flavone, 12 parts of astragaloside, 0.5 part of polydimethyl diallyl ammonium chloride, 2 parts of rilanit special, polyphenyl second
0.5 part of alkene sodium sulfonate, 0.8 part of N methyldiethanol amine；Preparation method：By glycyrrhiza total flavonoid, ginkgo biloba p.e, Herba Epimedii
General flavone, astragaloside are added in 90% ethanol solution and 1000rpm/min stirring and dissolvings are uniform, and poly- two are added into lysate
Methyl diallyl ammonium chloride, after being sufficiently mixed under microwave frequency 2450MHz, power 700W microwave treatment 15min, add
Rilanit special, kayexalate and N methyldiethanol amine continue microwave treatment 5min, microwave treatment after mixing
After be transferred to sealing and standing 3h in 0-5 DEG C of environment immediately, be then heated to 125 DEG C heat preservation mixing 15min, to gained mixture
6 parts of 0-5 DEG C of cold water of middle addition, stand 1h after being sufficiently mixed, be then heated to reflux state heat preservation mixing 20min, after will mixing
Object is volatilized as rotation in distilling machinery, disperses extra volatile ingredient, rear cooled to room temperature is finally sent into spray dryer
In, dry gained particle is age resister.
The present invention also provides a kind of infusion preparation methods of medical resin, include the following steps：
(1) silicone adhesive, lauryl sodium sulfate, nano modification alkyd resin are added to the mixed acid solution of 8 times of its weight
In, it is 3 that the nitration mixture, which is by mass ratio,:1 40% carbonic acid and 80% acetum composition, at 60 DEG C ultrasound 17 points
Clock, filtering are dried in vacuo 30 minutes at washing precipitation 3 times, 76 DEG C, obtain material I；
(2) the 50% of I weight of above-mentioned material is taken, mixes, is added to zinc stearate, stabilizer, stearic acid, age resister
In the methanol solution that 3 times of mixture weight, ultrasound 100 minutes is sent into reaction kettle, and helium is passed through, and it is 125 DEG C to increase temperature,
Insulation reaction 35 hours, discharging, product is filtered, is washed 3 times with 95% ethyl alcohol, is placed in 70 DEG C of baking oven and is dried to constant weight,
Obtain material II；
(3) remaining material I, Archon, chloromethyl ether, ferric trichloride are mixed, is added to the salicylic acid of 6 times of mixture weight
In, ultrasound 100 minutes is sent into reaction kettle, and helium is passed through, and it is 68 DEG C to increase temperature, insulation reaction 35 hours, and discharging will produce
Object filters, and is washed 3 times with 95% ethyl alcohol, is placed in 70 DEG C of baking oven and dries to constant weight, obtains material III；
(4) it takes vaseline, zinc carbonate, stearic acid, clay, dibutyl ester to be added in the methanol solution of its weight 20%, stirs
The sulfuric acid of a concentration of 3-6mol/L is added dropwise in mixing 20 minutes, and it is 5.5 to adjust pH, is passed through helium, is heated to boiling, and keeps boiling
57 minutes, discharging was cooled to room temperature, obtains material IV；
(5) above-mentioned material II, material III, material IV are mixed, is preheated 5 minutes at 85 DEG C, it is 155 DEG C to increase temperature,
Insulated and stirred 4 minutes, filtering away big impurity material must be infused with medical resin basis bottom material；
(6) above-mentioned infusion is mixed with medical resin basis bottom material with remaining each raw material, is stirred evenly, homogeneous, refinery, it is high
260 DEG C of heat refining 3h of heating are up to the medical resin raw material of infusion in warm stove；
(7) step 6 is infused after and is put into resin processing draft machine with medical resin raw material, variously-shaped or face is prepared into
The medical resin articles for use of the infusion of color, and naval stores is post-processed.
Post-processing approach is described in above-mentioned steps 7：
(1) infusion obtained is passed through in the second sink and is bathed with medical resin articles for use, it is 35~40 DEG C of temperature to neutralize bath
Dilute sulfuric acid, the mass fraction of dilute sulfuric acid is 0.5%；
(2) it washes, by step 1, treated that infusion is washed with medical resin articles for use in third sink, and washing is warm
Degree is 55 DEG C；
(3), the infusion after step 2 being washed carries out hot gas spring with medical treatment resin articles for use, oils and drying and processing, that is, is made
The medical resin articles for use of infusion.
Wherein, in step 3, in the hot gas spring step, hot gas spring multiple is 2 times, and hot gas spring temperature is 90 DEG C；It is described
The process that oils in glycerol concentration be 2.54g/L, oil applying rate be 0.12~0.25%, temperature be 24~26 DEG C；The drying
Drying temperature is 78~80 DEG C in process, and drying time is 14 hours.
Embodiment 2：
A kind of infusion medical resin and preparation method；
The technical problems to be solved by the invention are realized using following technical scheme：
A kind of infusion is as follows with medical resin, including specific technical solution：Infusion provided by the invention medical resin, packet
Include following mass fraction component：It is 2 parts of zinc stearate, 9 parts of lauryl sodium sulfate, 1.5 parts of stabilizer, 0.7 part of stearic acid, anti-ageing
2 parts of agent, 77 parts of silicone adhesive, 9 parts of Archon, 1.5 parts of chloromethyl ether, 4 parts of ferric trichloride, 8 parts of sulfuric acid, 9 parts of methanol, vaseline 16
Part, 13 parts of zinc carbonate, 11 parts of stearic acid, 12 parts of salicylic acid, 30 parts of clay, 8 parts of dibutyl ester, 12 parts of dioctyl ester, high-phenylethylene 13
Part, 9 parts of nano modification alkyd resin.
The stabilizer is made from the following raw materials in parts by weight：5 parts of cattail Down Fiber element, 1.0 parts of carboxymethyl cellulose, three
0.3 part of fluoropropyl methyl cyclotrisiloxane, 0.8 part of dwarf lilyturf tuber total saponins, 1.5 parts of sodium alginate, 0.2 part of lauric monoglyceride,
12 parts of water；The preparation method of stabilizer is that cattail Down Fiber element and carboxymethyl cellulose are first added to the water stirring and heat 68 DEG C
Until being completely dissolved, dwarf lilyturf tuber total saponins, sodium alginate and trifluoro propyl methyl cyclotrisiloxane then is added and lauric acid list is sweet
Grease 1000r/min stirs 0.5h, finally puts into 80 DEG C of emulsion reaction 3h in mulser, and rear taking-up is put into -90 DEG C of ring at once
Quick freeze 3h in border, it is rear take out put to room temperature restore to room temperature after up to stabilizer.
The age resister is made from the following raw materials in parts by weight：It is 8 parts of glycyrrhiza total flavonoid, 10 parts of ginkgo biloba p.e, excessive
9 parts of sheep leaves of pulse plants general flavone, 7 parts of astragaloside, 1 part of polydimethyl diallyl ammonium chloride, 1 part of rilanit special, polystyrene sulphur
0.8 part of sour sodium, 0.5 part of N methyldiethanol amine；Preparation method：Glycyrrhiza total flavonoid, ginkgo biloba p.e, Herba Epimedii is always yellow
Ketone, astragaloside are added in 75% ethanol solution and 600rpm/min stirring and dissolvings are uniform, and poly dimethyl is added into lysate
Diallyl ammonium chloride, after being sufficiently mixed under microwave frequency 2450MHz, power 700W microwave treatment 20min, add hydrogenation
Castor oil, kayexalate and N methyldiethanol amine, continue microwave treatment 5min after mixing, and microwave treatment terminates
It is transferred to sealing and standing 3h in 0-5 DEG C of environment immediately afterwards, is then heated to 130 DEG C of heat preservation mixing 15min, adds into gained mixture
Enter 6 parts of 0-5 DEG C of cold water, 1h stood after being sufficiently mixed, be then heated to reflux state heat preservation mixing 30min, after by mixture extremely
In distilling machinery is volatilized in rotation, extra volatile ingredient is dispersed, rear cooled to room temperature is finally sent into spray dryer,
Dry gained particle is age resister.
The present invention also provides a kind of infusion preparation methods of medical resin, include the following steps：
(1) silicone adhesive, lauryl sodium sulfate, nano modification alkyd resin are added to the mixed acid solution of 8 times of its weight
In, it is 4 that the nitration mixture, which is by mass ratio,:1 40% carbonic acid and 80% acetum composition, at 60 DEG C ultrasound 17 points
Clock, filtering are dried in vacuo 30 minutes at washing precipitation 2 times, 70 DEG C, obtain material I；
(2) the 40% of I weight of above-mentioned material is taken, mixes, is added to zinc stearate, stabilizer, stearic acid, age resister
In the methanol solution that 3 times of mixture weight, ultrasound 100 minutes is sent into reaction kettle, and helium is passed through, and it is 120 DEG C to increase temperature,
Insulation reaction 35 hours, discharging, product is filtered, is washed 3 times with 95% ethyl alcohol, is placed in 70 DEG C of baking oven and is dried to constant weight,
Obtain material II；
(3) remaining material I, Archon, chloromethyl ether, ferric trichloride are mixed, is added to the salicylic acid of 6 times of mixture weight
In, ultrasound 100 minutes is sent into reaction kettle, and helium is passed through, and it is 68 DEG C to increase temperature, insulation reaction 35 hours, and discharging will produce
Object filters, and is washed 3 times with 95% ethyl alcohol, is placed in 70 DEG C of baking oven and dries to constant weight, obtains material III；
(4) it takes vaseline, zinc carbonate, stearic acid, clay, dibutyl ester to be added in the methanol solution of its weight 17%, stirs
The sulfuric acid of a concentration of 3mol/L is added dropwise in mixing 20 minutes, and it is 5 to adjust pH, is passed through helium, is heated to boiling, and keeps 57 points of boiling
Clock, discharging, is cooled to room temperature, obtains material IV；
(5) above-mentioned material II, material III, material IV are mixed, is preheated 4 minutes at 87 DEG C, it is 155 DEG C to increase temperature,
Insulated and stirred 3 minutes, filtering away big impurity material must be infused with medical resin basis bottom material；
(6) above-mentioned infusion is mixed with medical resin basis bottom material with remaining each raw material, is stirred evenly, homogeneous, refinery, it is high
260- DEG C of heat refining 2h of heating is up to the medical resin raw material of infusion in warm stove；
(7) step 6 is infused after and is put into resin processing draft machine with medical resin raw material, variously-shaped or face is prepared into
The medical resin articles for use of the infusion of color, and naval stores is post-processed.
Post-processing approach is described in above-mentioned steps 7：
(1) infusion obtained is passed through in the second sink and is bathed with medical resin articles for use, it is the dilute of 40 DEG C of temperature to neutralize bath
The mass fraction of sulfuric acid, dilute sulfuric acid is 0.5%；
(2) it washes, by step 1, treated that infusion is washed with medical resin articles for use in third sink, and washing is warm
Degree is 65 DEG C；
(3), the infusion after step 2 being washed carries out hot gas spring with medical treatment resin articles for use, oils and drying and processing, that is, is made
The medical resin articles for use of infusion.
Wherein, in step 3, in the hot gas spring step, hot gas spring multiple is 2 times, and hot gas spring temperature is 80~85 DEG C；
Glycerol concentration is 2g/L in the process that oils, and oil applying rate is 0.12~0.25%, and temperature is 24~26 DEG C；The drying
Drying temperature is 75 DEG C in process, and drying time is 14 hours.
To carrying out experiment investigation respectively in embodiment provided by the invention, embodiment 1 and embodiment 2 are prepared into infusion doctor
Resin to be treated to be investigated, examination criteria refers to Q/GHBA8-2010, using market common transfusion medical transfusion pipe as reference examples, knot
Fruit is as shown in table 1；
The medical resin testing result of the infusion of table 1
| Detection project | Standard | Reference examples | Embodiment 1 | Embodiment 2 |
| Glutinous number/(mL/g) | 106-115 | 108.8 | 110.5 | 109.8 |
| K values | 65.0-67.6 | 66.3 | 66.7 | 66.2 |
| Average degree of polymerization | 1000-1100 | 1004 | 1086 | 1028 |
| Apparent density g/mL | 0.47-0.57 | 0.48.6 | 0.546 | 0.517 |
| Volatile matter %≤ | 0.30 | 0.23 | 0.058 | 0.067 |
| " flake " number (a/400cm2)≤ | 10 | 10 | 3 | 4 |
| Number of impurity particles /≤ | 16 | 14 | 2 | 5 |
| 100g resin plasticizers uptake/g >= | 22 | 38 | 56 | 49.8 |
| Whiteness/% (160 DEG C, 10min) >= | 74 | 80 | 89 | 91.5 |
| Residual polymerized ethylene content/(μ g/g)≤ | 0.4 | 0.35 | 0.12 | 0.098 |
| Residual toluene content/(μ g/g)≤ | It is not detected | It is not detected | It is not detected | It is not detected |
| Residual itrile group mass contg/(μ g/g)≤ | It is not detected | It is not detected | It is not detected | It is not detected |
| Residual 1,2- dichloroethane content/(μ g/g)≤ | 1.0 | 0.78 | 0.26 | 0.31 |
The present invention is infused to be shown with medical resin articles for use testing result：
Although common transfusion medical transfusion pipe items detection in market meets quality standard, find out from testing result, this hair
The medical resin articles for use index of the infusion of bright preparation meets quality standard, and parameter index is better than reference examples, and quality is high
In control；The medical resin articles for use of infusion prepared by the present invention, compatibility is good, high resistance to hot/cold, toughness, to the steady of light and heat
It is fixed, safe and non-toxic；It is simple using equipment, easy to operate, manufacturing cost is low and using environmental friendly, it is medical to improving infusion
The various performances of resin articles for use have very high practical value.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (2)
1. a kind of medical resin of infusion, it is characterised in that：Infusion medical treatment resin includes following mass fraction component：Stearic acid
1-2 parts of zinc, 4-9 parts of lauryl sodium sulfate, 1.5-5 parts of stabilizer, 0.5-0.7 parts of stearic acid, 1-4 parts of age resister, silicone
77-94 parts of glue, 4-12 parts of Archon, 0.5-5 parts of chloromethyl ether, 1-6 parts of ferric trichloride, 6-13 parts of sulfuric acid, 4-12 parts of methanol, vaseline
15-20 parts, it is 11-18 parts of zinc carbonate, 6-15 parts of stearic acid, 9-17 parts of salicylic acid, 30-40 parts of clay, 5-10 parts of dibutyl ester, two pungent
10-17 parts of ester, 12-19 parts of high-phenylethylene, 6-13 parts of nano modification alkyd resin；
The stabilizer is made from the following raw materials in parts by weight：3-5 parts of cattail Down Fiber element, 0.6-1.0 parts of carboxymethyl cellulose,
0.3-0.5 parts of trifluoro propyl methyl cyclotrisiloxane, 0.5-3 parts of dwarf lilyturf tuber total saponins, 1.5-3 parts of sodium alginate, lauric acid list are sweet
0.2-2 parts of grease, 12-21 parts of water；The preparation method of stabilizer is that water first is added in cattail Down Fiber element and carboxymethyl cellulose
Middle stirring simultaneously heats 50-70 DEG C up to being completely dissolved, and dwarf lilyturf tuber total saponins, sodium alginate and trifluoro propyl methyl ring three is then added
Siloxanes and lauric monoglyceride 800-1000r/min stir 0.5-1h, finally put into 70-80 DEG C of emulsion reaction in mulser
2-4h, rear take out are put into quick freeze 2-6h in -50-100 DEG C of environment at once, it is rear take out put to room temperature restore to room temperature after i.e.
Obtain stabilizer；
The age resister is made from the following raw materials in parts by weight：It is 4-13 parts of glycyrrhiza total flavonoid, 4-12 parts of ginkgo biloba p.e, excessive
5-20 parts of sheep leaves of pulse plants general flavone, 7-15 parts of astragaloside, 0.5-1 parts of polydimethyl diallyl ammonium chloride, rilanit special 1-2
Part, 0.5-1 parts of kayexalate, 0.5-1 parts of N methyldiethanol amine；Preparation method：By glycyrrhiza total flavonoid, ginkgo leaf
Extract, barren wort total chromocor, astragaloside are added in 60-90% ethanol solutions and 600-1000rpm/min stirring and dissolvings are equal
It is even, polydimethyl diallyl ammonium chloride is added into lysate, in microwave frequency 2450MHz, power 700W after being sufficiently mixed
Lower microwave treatment 5-30min, adds rilanit special, kayexalate and N methyldiethanol amine, after mixing
Continue microwave treatment 5min, is transferred to sealing and standing 3h in 0-5 DEG C of environment immediately after microwave treatment, is then heated to 125-
130 DEG C of heat preservation mixing 10-30min, 6-8 parts of 0-5 DEG C of cold water are added into gained mixture, 1h are stood after being sufficiently mixed, then
Be heated to reflux state heat preservation mixing 5-30min, after by mixture as rotation volatilize distilling machinery in, disperse extra volatility at
Point, rear cooled to room temperature is finally sent into spray dryer, and dry gained particle is age resister.
2. a kind of infusion preparation method of medical resin, includes the following steps：
(1) silicone adhesive, lauryl sodium sulfate, nano modification alkyd resin are added to the mixed acid solution of 8-10 times of its weight
In, it is 3-4 that the nitration mixture, which is by mass ratio,:The carbonic acid of 1 40-50% and the acetum composition of 70-80%, in 50-60
Ultrasound 17-20 minutes at DEG C, filtering are dried in vacuo 30-40 minutes at washing precipitation 2-3 times, 70-76 DEG C, obtain material I；
(2) 40-50% for taking I weight of above-mentioned material is mixed with zinc stearate, stabilizer, stearic acid, age resister, is added to
It is 100-120 minutes ultrasonic in the methanol solution of 3-5 times of mixture weight, it is sent into reaction kettle, is passed through helium, increasing temperature is
120-127 DEG C, product is filtered, is washed 3-4 times with 95% ethyl alcohol, be placed in 70-80 DEG C by insulation reaction 35-40 hours, discharging
It is dried to constant weight in baking oven, obtains material II；
(3) remaining material I, Archon, chloromethyl ether, ferric trichloride are mixed, is added to the salicylic acid of 6-7 times of mixture weight
In, it is 100-110 minutes ultrasonic, it is sent into reaction kettle, is passed through helium, it is 68-70 DEG C to increase temperature, insulation reaction 35-40 hours,
Discharging, product is filtered, is washed 3-4 times with 95% ethyl alcohol, is placed in 70-80 DEG C of baking oven and is dried to constant weight, obtains material III；
(4) vaseline, zinc carbonate, stearic acid, clay, dibutyl ester is taken to be added in the methanol solution of its weight 17-20%, stirring is mixed
It closes 20-30 minutes, the sulfuric acid of a concentration of 3-6mol/L is added dropwise, adjusting pH is 5-6, is passed through helium, is heated to boiling, and keeps boiling
57-60 minutes, discharging was cooled to room temperature, obtains material IV；
(5) above-mentioned material II, material III, material IV are mixed, is preheated 4-6 minutes at 87-90 DEG C, raising temperature is 155-
160 DEG C, insulated and stirred 3-4 minutes, filtering away big impurity material must be infused with medical resin basis bottom material；
(6) above-mentioned infusion is mixed with medical resin basis bottom material with remaining each raw material, is stirred evenly, homogeneous, refinery, high temperature furnace
200-360 DEG C of heat refining 2-5h of interior heating is up to the medical resin raw material of infusion；
(7) step 6 is infused after and is put into resin processing draft machine with medical resin raw material, is prepared into variously-shaped or color
The medical resin articles for use of infusion, and naval stores is post-processed；
Post-processing approach is described in above-mentioned steps 7：
(1) infusion obtained is passed through in the second sink and is bathed with medical resin articles for use, it is the dilute of 35~40 DEG C of temperature to neutralize bath
The mass fraction of sulfuric acid, dilute sulfuric acid is 0.5~0.8%；
(2) wash, by step 1 treated infusion with medical treatment resin articles for use washed in third sink, washing temperature is
55~65 DEG C；
(3), the infusion after step 2 being washed carries out hot gas spring with medical treatment resin articles for use, oils and drying and processing, that is, infusion is made
With medical resin articles for use；
Wherein, in step 3, in the hot gas spring step, hot gas spring multiple is 2~3 times, and hot gas spring temperature is 80~100 DEG C；
Glycerol concentration is 2~4g/L in the process that oils, and oil applying rate is 0.12~0.25%, and temperature is 20~26 DEG C；Described
Drying temperature is 70~80 DEG C in baking operation, and drying time is 14~18 hours.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810241387.8A CN108587167A (en) | 2018-03-22 | 2018-03-22 | A kind of infusion medical resin and preparation method |
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| CN201810241387.8A CN108587167A (en) | 2018-03-22 | 2018-03-22 | A kind of infusion medical resin and preparation method |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101696302A (en) * | 2009-10-29 | 2010-04-21 | 广州市合诚化学有限公司 | Self-lubricating polypropylene compound material for manufacturing medical injectors |
| CN103946277A (en) * | 2011-11-17 | 2014-07-23 | 道康宁公司 | Silicone resins |
| CN105555872A (en) * | 2013-09-27 | 2016-05-04 | 美国圣戈班性能塑料公司 | A silicone article, a tube and method of forming an article |
-
2018
- 2018-03-22 CN CN201810241387.8A patent/CN108587167A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101696302A (en) * | 2009-10-29 | 2010-04-21 | 广州市合诚化学有限公司 | Self-lubricating polypropylene compound material for manufacturing medical injectors |
| CN103946277A (en) * | 2011-11-17 | 2014-07-23 | 道康宁公司 | Silicone resins |
| CN105555872A (en) * | 2013-09-27 | 2016-05-04 | 美国圣戈班性能塑料公司 | A silicone article, a tube and method of forming an article |
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