CN107652651A - A kind of heparin tube plastic material and preparation method thereof - Google Patents
A kind of heparin tube plastic material and preparation method thereof Download PDFInfo
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- CN107652651A CN107652651A CN201710966170.9A CN201710966170A CN107652651A CN 107652651 A CN107652651 A CN 107652651A CN 201710966170 A CN201710966170 A CN 201710966170A CN 107652651 A CN107652651 A CN 107652651A
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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
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G64/00—Macromolecular compounds obtained by reactions forming a carbonic ester link in the main chain of the macromolecule
- C08G64/20—General preparatory processes
- C08G64/30—General preparatory processes using carbonates
- C08G64/305—General preparatory processes using carbonates and alcohols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/34—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives
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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
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Materials For Medical Uses (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a kind of heparin tube plastic material, and it is made up of the raw material of following weight parts:Kaolin 10 14, trimethylene carbonate 170 200, 1, 6 hexylene glycols 79, ethyl cellulose 34, DAA 56, calcium stearate 34, oleic acid diethyl amide 0.8 1, phytosterol 0.4 1, macromolecule emulsion 30 40, stannous octoate 23, the macromolecule emulsion that the present invention adds can effectively improve dispersiveness of the filler between polymeric matrix, improve the pliability of finished-product material, it is blended with ethyl cellulose, serve the effect of coordination plasticizing, phenomena such as effectively preventing heparin tube is cracking, the present invention uses makrolon as plastic raw materials, with the good feature of environmental protection and safety in utilization, degradability is good, it cannot be easily caused pollution.
Description
Technical field
The invention belongs to biochemical material field, and in particular to a kind of heparin tube plastic material and preparation method thereof.
Background technology
The material of vacuum blood collection tube:Heparin tube is mostly simple glass pipe and plastic tube.Simple glass pipe because pH value is larger,
Easily cause haemolysis, and the linear ditch of teat glass that tube-pulling craft makes gathers, depth thickness is without often resulting in cell wall built-up.Part
Company uses neutral density glass (pharmaceutical glass).Neutral density glass has pressure-resistant, and leachable is few, and molecules align is close, during stretching
The advantages that groove is few, test tube can tolerate 1.5 meters of level above freely falling bodies, effectively prevent from gathering, transport, test during sample
Leakage, environment is polluted, reduce the probability of resampling.And test tube bottom is handled by special strengthening, avoid producing during centrifugation
It is damaged.Vacuum blood collection tube has carried out inwall processing in process of production, i.e., dilutes silicone oil or emulsion by a certain percentage, uniformly applies
It is overlying on inside pipe wall.Because silicone oil is a kind of extremely strong mixture of inertia, inboard wall of test tube is adhered to, haemocyte is reduced and is glued with tube wall
It is right.Plastic vacuum heparin tube uses PET, and PET pipe has:Light weight, it is readily transported, tube wall breakage probability pole
Small, sample is transporting, and centrifuges and test the characteristics of possibility that process leaks is minimum, but it is difficult to degrade, pliability
Deficiency, it is poor using the feature of environmental protection.
The content of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of heparin tube plastic material and its
Preparation method.
To achieve the above object, the present invention uses following technical scheme:
A kind of heparin tube plastic material, it is made up of the raw material of following weight parts:
Kaolin 10-14, trimethylene carbonate 170-200,1,6-HD 7-9, ethyl cellulose 3-4, two acetone
Alcohol 5-6, calcium stearate 3-4, oleic acid diethyl amide 0.8-1, phytosterol 0.4-1, macromolecule emulsion 30-40, stannous octoate
2-3。
Described macromolecule emulsion is made up of the raw material of following weight parts:
Formamide 30-40, initiator 0.8-1, the tert-butyl group are to biphenol 0.6-1, pentaerythrite 5-7, trimethylolpropane
0.1-0.2。
Described initiator is one kind in ammonium persulfate, potassium peroxydisulfate, sodium peroxydisulfate.
The preparation method of described macromolecule emulsion comprises the following steps:
(1) initiator is taken, is added in the deionized water of 120-130 times of its weight, stirs, obtain initiator solution;
(2) take the tert-butyl group that biphenol is added in the absolute ethyl alcohol of 4-5 times of its weight, stirred, adds Ji Wusi
Alcohol, the insulated and stirred 16-20 minutes at 60-65 DEG C, above-mentioned formamide is added, is stirred, is sent in reactor, is passed through nitrogen
Gas, regulation temperature of reaction kettle is 75-80 DEG C, and above-mentioned initiator solution is added dropwise, rear insulated and stirred 3-4 hours are added dropwise, and is discharged,
Secure satisfactory grades sub- alcoholic solution;
(3) trimethylolpropane is taken, is added in above-mentioned high molecular alcohol solution, ultrasonic 3-4 minutes, ethanol is distilled off,
Produce the macromolecule emulsion.
A kind of preparation method of heparin tube plastic material, comprises the following steps:
(1) kaolin is taken, 1-2 hours are calcined at 700-800 DEG C, fine powder is worn into after cooling, is mixed with calcium stearate, added
Enter into above-mentioned Polymer Solution, be sent in boiling water bath, insulated and stirred 30-40 minutes, discharging cooling, obtain kaolin and disperse
Liquid;
(2) ethyl cellulose is taken, is added in the deionized water of 36-40 times of its weight, stirs, adds two acetone
Alcohol, insulated and stirred 5-10 minutes, obtain fiber dispersion at 50-60 DEG C;
(3) above-mentioned kaolin dispersion liquid, fiber dispersion mixing are taken, stirs, adds oleic acid diethyl amide, magnetic force
10-20 minutes are stirred, secure satisfactory grades subbundle dispersion liquid;
(4) trimethylene carbonate is taken, is added in above-mentioned macromolecular fibre dispersion liquid, stirs, adds plant steroid
Alcohol, it is sent in reactor, regulation temperature of reaction kettle is 110-120 DEG C, adds stannous octoate, insulated and stirred 3-5 hours, adds
1,6- hexylene glycol, it is 70-80 DEG C to reduce temperature, insulated and stirred 20-30 minutes, discharging, obtains polycarbonate solution;
(5) above-mentioned polycarbonate solution is taken, is mixed with calcium stearate, is stirred, is dehydrated, is sent in extruder, is melted
Melt extrusion, cool down, produce the heparin tube plastic material.
Advantages of the present invention:
The macromolecule emulsion that the present invention adds polymerize, Ran Houtong using formamide as monomer under the initiator effect of containing alcohol
Cross trimethylolpropane to disperse, the macromolecule emulsion that the present invention adds can effectively improve point of the filler between polymeric matrix
Property is dissipated, improves the pliability of finished-product material, is blended with ethyl cellulose, serves the effect of coordination plasticizing, effectively preventing
Phenomena such as heparin tube is cracking, the present invention use makrolon as plastic raw materials, with the good feature of environmental protection and safe to use
Property, degradability is good, it is not easy to pollutes.
Embodiment
Embodiment 1
A kind of heparin tube plastic material, it is made up of the raw material of following weight parts:
Kaolin 14, trimethylene carbonate 200,1,6-HD 9, ethyl cellulose 4, DAA 6, calcium stearate
4th, oleic acid diethyl amide 1, phytosterol 1, macromolecule emulsion 40, stannous octoate 3.
Described macromolecule emulsion is made up of the raw material of following weight parts:
Formamide 40, initiator 1, the tert-butyl group are to biphenol 1, pentaerythrite 7, trimethylolpropane 0.2.
Described initiator is sodium peroxydisulfate.
The preparation method of described macromolecule emulsion comprises the following steps:
(1) initiator is taken, is added in the deionized water of 130 times of its weight, is stirred, obtain initiator solution;
(2) take the tert-butyl group that biphenol is added in the absolute ethyl alcohol of 5 times of its weight, stirred, adds Ji Wusi
Alcohol, insulated and stirred 20 minutes at 65 DEG C, adds above-mentioned formamide, stirs, be sent in reactor, is passed through nitrogen, adjusts
It is 80 DEG C to save temperature of reaction kettle, and above-mentioned initiator solution is added dropwise, rear insulated and stirred is added dropwise 4 hours, is discharged, secure satisfactory grades sub- alcohol
Solution;
(3) trimethylolpropane is taken, is added in above-mentioned high molecular alcohol solution, ultrasound 4 minutes, ethanol is distilled off, i.e.,
Obtain the macromolecule emulsion.
A kind of preparation method of heparin tube plastic material, comprises the following steps:
(1) kaolin is taken, is calcined 2 hours at 800 DEG C, fine powder is worn into after cooling, is mixed with calcium stearate, is added to
State in Polymer Solution, be sent in boiling water bath, insulated and stirred 40 minutes, discharging cooling, obtain kaolin dispersion liquid;
(2) ethyl cellulose is taken, is added in the deionized water of 40 times of its weight, stirs, adds DAA,
Insulated and stirred 10 minutes, obtain fiber dispersion at 60 DEG C;
(3) above-mentioned kaolin dispersion liquid, fiber dispersion mixing are taken, stirs, adds oleic acid diethyl amide, magnetic force
Stirring 20 minutes, secure satisfactory grades subbundle dispersion liquid;
(4) trimethylene carbonate is taken, is added in above-mentioned macromolecular fibre dispersion liquid, stirs, adds plant steroid
Alcohol, be sent in reactor, regulation temperature of reaction kettle be 120 DEG C, add stannous octoate, insulated and stirred 5 hours, add 1,6- oneself
Glycol, it is 80 DEG C to reduce temperature, insulated and stirred 30 minutes, discharging, obtains polycarbonate solution;
(5) above-mentioned polycarbonate solution is taken, is mixed with calcium stearate, is stirred, is dehydrated, is sent in extruder, is melted
Melt extrusion, cool down, produce the heparin tube plastic material.
Embodiment 2
A kind of heparin tube plastic material, it is made up of the raw material of following weight parts:
Kaolin 10, trimethylene carbonate 170,1,6-HD 7, ethyl cellulose 3, DAA 5, calcium stearate
3rd, oleic acid diethyl amide 0.8, phytosterol 0.4, macromolecule emulsion 30, stannous octoate 2.
Described macromolecule emulsion is made up of the raw material of following weight parts:
Formamide 30, initiator 0.8, the tert-butyl group are to biphenol 0.6, pentaerythrite 5, trimethylolpropane 0.1.
Described initiator is ammonium persulfate.
The preparation method of described macromolecule emulsion comprises the following steps:
(1) initiator is taken, is added in the deionized water of 120 times of its weight, is stirred, obtain initiator solution;
(2) take the tert-butyl group that biphenol is added in the absolute ethyl alcohol of 4 times of its weight, stirred, adds Ji Wusi
Alcohol, the clock of insulated and stirred 16 at 60 DEG C, adds above-mentioned formamide, stirs, be sent in reactor, is passed through nitrogen, regulation
Temperature of reaction kettle is 75 DEG C, and above-mentioned initiator solution is added dropwise, rear insulated and stirred is added dropwise 3 hours, is discharged, and the sub- alcohol that secures satisfactory grades is molten
Liquid;
(3) trimethylolpropane is taken, is added in above-mentioned high molecular alcohol solution, ultrasound 3 minutes, ethanol is distilled off, i.e.,
Obtain the macromolecule emulsion.
A kind of preparation method of heparin tube plastic material, comprises the following steps:
(1) kaolin is taken, is calcined 1 hour at 700 DEG C, fine powder is worn into after cooling, is mixed with calcium stearate, is added to
State in Polymer Solution, be sent in boiling water bath, insulated and stirred 30 minutes, discharging cooling, obtain kaolin dispersion liquid;
(2) ethyl cellulose is taken, is added in the deionized water of 36 times of its weight, stirs, adds DAA,
Insulated and stirred 5 minutes, obtain fiber dispersion at 50 DEG C;
(3) above-mentioned kaolin dispersion liquid, fiber dispersion mixing are taken, stirs, adds oleic acid diethyl amide, magnetic force
Stirring 10 minutes, secure satisfactory grades subbundle dispersion liquid;
(4) trimethylene carbonate is taken, is added in above-mentioned macromolecular fibre dispersion liquid, stirs, adds plant steroid
Alcohol, be sent in reactor, regulation temperature of reaction kettle be 110 DEG C, add stannous octoate, insulated and stirred 3 hours, add 1,6- oneself
Glycol, it is 70 DEG C to reduce temperature, insulated and stirred 20 minutes, discharging, obtains polycarbonate solution;
(5) above-mentioned polycarbonate solution is taken, is mixed with calcium stearate, is stirred, is dehydrated, is sent in extruder, is melted
Melt extrusion, cool down, produce the heparin tube plastic material.
Performance test:
Heparin tube plastic material and commercially available heparin tube plastics prepared by the present invention is respectively under the conditions of ASTM D-638
Measure tensile strength;
As a result:Heparin tube prepared by the present invention with the tensile strength of plastic material is 55-65MPa, bending strength 70-
80MPa;The tensile strength of commercially available heparin tube plastics is 20-30MPa, the bending strength of commercially available heparin tube plastics is 50-60MPa;
As can be seen that the material of the present invention has more preferable mechanical property.
Claims (5)
1. a kind of heparin tube plastic material, it is characterised in that it is made up of the raw material of following weight parts:
Kaolin 10-14, trimethylene carbonate 170-200,1,6-HD 7-9, ethyl cellulose 3-4, DAA 5-
6th, calcium stearate 3-4, oleic acid diethyl amide 0.8-1, phytosterol 0.4-1, macromolecule emulsion 30-40, stannous octoate 2-3.
A kind of 2. heparin tube plastic material according to claim 1, it is characterised in that described macromolecule emulsion be by
The raw material composition of following weight parts:
Formamide 30-40, initiator 0.8-1, the tert-butyl group are to biphenol 0.6-1, pentaerythrite 5-7, trimethylolpropane 0.1-
0.2。
3. a kind of heparin tube plastic material according to claim 2, it is characterised in that described initiator is persulfuric acid
One kind in ammonium, potassium peroxydisulfate, sodium peroxydisulfate.
A kind of 4. heparin tube plastic material according to claim 2, it is characterised in that the system of described macromolecule emulsion
Preparation Method comprises the following steps:
(1) initiator is taken, is added in the deionized water of 120-130 times of its weight, stirs, obtain initiator solution;
(2) take the tert-butyl group to be added in the absolute ethyl alcohol of 4-5 times of its weight, stir biphenol, add pentaerythrite,
The insulated and stirred 16-20 minute at 60-65 DEG C, above-mentioned formamide is added, is stirred, is sent in reactor, is passed through nitrogen,
It is 75-80 DEG C to adjust temperature of reaction kettle, and above-mentioned initiator solution is added dropwise, rear insulated and stirred 3-4 hours are added dropwise, and discharges, obtains
High molecular alcohol solution;
(3) trimethylolpropane is taken, is added in above-mentioned high molecular alcohol solution, ultrasonic 3-4 minutes, ethanol is distilled off, produces
The macromolecule emulsion.
5. a kind of preparation method of heparin tube plastic material as claimed in claim 1, it is characterised in that including following step
Suddenly:
(1) kaolin is taken, 1-2 hours are calcined at 700-800 DEG C, fine powder is worn into after cooling, is mixed with calcium stearate, is added to
In above-mentioned Polymer Solution, it is sent in boiling water bath, insulated and stirred 30-40 minutes, discharging cooling, obtains kaolin dispersion liquid;
(2) ethyl cellulose is taken, is added in the deionized water of 36-40 times of its weight, stirs, adds DAA,
Insulated and stirred 5-10 minutes, obtain fiber dispersion at 50-60 DEG C;
(3) above-mentioned kaolin dispersion liquid, fiber dispersion mixing are taken, stirs, adds oleic acid diethyl amide, magnetic agitation
10-20 minutes, secure satisfactory grades subbundle dispersion liquid;
(4) trimethylene carbonate is taken, is added in above-mentioned macromolecular fibre dispersion liquid, stirs, phytosterol is added, send
Enter into reactor, regulation temperature of reaction kettle is 110-120 DEG C, adds stannous octoate, insulated and stirred 3-5 hours, adds 1,6-
Hexylene glycol, it is 70-80 DEG C to reduce temperature, insulated and stirred 20-30 minutes, discharging, obtains polycarbonate solution;
(5) above-mentioned polycarbonate solution is taken, is mixed with calcium stearate, is stirred, is dehydrated, is sent in extruder, melting is squeezed
Go out, cool down, produce the heparin tube plastic material.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110951247A (en) * | 2019-04-29 | 2020-04-03 | 山东祥龙新材料股份有限公司 | Transparent nylon material and preparation method thereof |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105504514A (en) * | 2016-01-11 | 2016-04-20 | 宁波高新区辉门科技有限公司 | Environment-friendly plastic toughened through fibers and preparation method thereof |
CN105907052A (en) * | 2016-06-23 | 2016-08-31 | 吴国庆 | Environment-friendly impact resistant PC (polycarbonate)/PBT (polybutylene terephthalate)/PP (polypropylene) plastic alloy and preparation method thereof |
CN106398155A (en) * | 2016-06-23 | 2017-02-15 | 吴国庆 | An impact-resistant toughened PC/ABS plastic alloy and a preparing method thereof |
-
2017
- 2017-10-17 CN CN201710966170.9A patent/CN107652651A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105504514A (en) * | 2016-01-11 | 2016-04-20 | 宁波高新区辉门科技有限公司 | Environment-friendly plastic toughened through fibers and preparation method thereof |
CN105907052A (en) * | 2016-06-23 | 2016-08-31 | 吴国庆 | Environment-friendly impact resistant PC (polycarbonate)/PBT (polybutylene terephthalate)/PP (polypropylene) plastic alloy and preparation method thereof |
CN106398155A (en) * | 2016-06-23 | 2017-02-15 | 吴国庆 | An impact-resistant toughened PC/ABS plastic alloy and a preparing method thereof |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110951247A (en) * | 2019-04-29 | 2020-04-03 | 山东祥龙新材料股份有限公司 | Transparent nylon material and preparation method thereof |
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Application publication date: 20180202 |