CN107603454A - A kind of antibiont sticks the preparation method of surfacing - Google Patents
A kind of antibiont sticks the preparation method of surfacing Download PDFInfo
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- CN107603454A CN107603454A CN201710928803.7A CN201710928803A CN107603454A CN 107603454 A CN107603454 A CN 107603454A CN 201710928803 A CN201710928803 A CN 201710928803A CN 107603454 A CN107603454 A CN 107603454A
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Abstract
The present invention relates to the preparation method that a kind of antibiont sticks surfacing, belong to field of material technology.Remove ionized water, boiled silk and ethanol solution to be placed in beaker, stir, heat, cooling, filter to get filtrate, obtain fibroin liquid；Take fresh camphortree leaf, pulverize and sieve, obtain the stirring of camphortree leaf powder, heat and distill extraction, collect distillate and stratification, upper strata grease is collected, by anhydrous calcium chloride and upper strata grease hybrid reaction, cyclodextrin granule is added in fibroin liquid and reacts to obtain mixed liquor, camphor tree leaf volatile oil is added dropwise in mixed liquor and reacted, collect lower sediment and wash, dry, modified powder of milling to obtain；Weigh PPG, deionized water modified powder and methyl diphenylene diisocyanate to be placed in beaker, stir, heating, cool down coating liquid and to coat coating liquid to glass pane surface, after the completion of to be coated, simultaneously mulching treatment is dried, you can be prepared into a kind of antibiont and stick surfacing.
Description
Technical field
The present invention relates to the preparation method that a kind of antibiont sticks surfacing, belong to field of material technology.
Background technology
Bio-adhesive typically refers to two kinds of materials, and wherein at least one is the material for having natural biological attribute（Such as：It is raw
Thing molecule, protein, cell, microorganism, aquatile etc.）, state together is sticked by the persistent of interfacial force.
It is a kind of interface behavior, is prevalent in nature and actual life.The bio-adhesive behavior of nature（Such as：Cobweb
Net-fault insect is sticked, marine organisms the sticking on rock such as barnacle, oyster, mussel, algae, some probiotics in people and
The mucous membrane of different parts or surface epithelial cell sticks in organism）Often biology obtains during long-term evolution
A kind of specific function or survival ability.However, in many applications, from biology device, cistern, underwater facility to ship
Oceangoing ship, the attachment on surface such as nonspecific biomolecule, microorganism how is resisted, that is, improve the antibiont adhesion energy on surface
Power, all it is a very big challenge.For example, the nonspecific proteins absorption of biosensor surface can make degradation, cause
Detection or diagnosis misalignment；Nonspecific protein absorption can be to man-made organ or orthopedic implants（Such as：It is joint prosthesis, artificial
Bone, heart valve prosthesis, artificial blood vessel, support etc.）Treatment and reparation have a negative impact；Algae or microorganism are in water-supply-pipe
The attachment and growth of the pool wall and bottom of pond surface of road inwall and cistern or swimming pool can cause water degradation；Bio-adhesive can make
There is biofouling blocking in bio-chemistry separation film；Attachment and breeding of the marine organisms such as barnacle, bacterium, shellfish and algae in hull surface
Ship resistance and energy consumption can be greatly increased, this problem makes various countries' shipbuilding industry headache endlessly always for many years.In case of human, this
A little is the example of very typical " bad " bio-adhesive.Therefore, the harm of " bad " bio-adhesive be bio-medical material,
The researchs such as biochemical analysis, biochemical industry, marine ship be antifouling and be related in application field it is a general character, have it is basic and
The problem of generality.According to the analysis of the process and mechanism of foregoing various bio-adhesive phenomenons, either marine organisms
Stick, or the formation of thrombus and sticking for bacterium, all there is significantly similitude.From the point of view of molecular level,
Incipient stage is all one layer of basement membrane, such as protein, is promptly adsorbed in unshielded material surface；Then, cell, microorganism etc.
The biomolecule of various different sizes and property or organism, start to be attached to material surface formation biomembrane, so that slowly shape
Into huge and complicated bio-adhesive system, then trigger a series of problem.Therefore, anti-protein absorption, antibacterium are studied
It is that ship and underwater facility are prevented to stick and can resist the antibiont pasting material that the aquatic organisms such as algae, shellfish stick
The important topic in the fields such as dirt, bio-medical material, biochemical industry, new function material.Obviously, people can not possibly change nature
The bio-adhesive characteristic of microorganism, shellfish, aquatile in boundary etc..Therefore, scientifically design and build and sticked with antibiont
The surface of attached characteristic is reduction and eliminates the unique channel of the negative effect of bio-adhesive.
The content of the invention
The technical problems to be solved by the invention：Poor, the Yi for the anti-anti- Adhesion property in pasting material surface of traditional biological
Biomembrane is formed in material surface, so as to the problem of slowly forming huge and complicated bio-adhesive system, there is provided Yi Zhongkang
The preparation method of bio-adhesive surfacing.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
Specifically preparation process is：
（1）Count in parts by weight, choose 65~70 parts of deionized water, 10~15 parts of boiled silk and 55~60 parts of ethanol
Solution is placed in beaker, is stirred and heating water bath, standing are cooled to room temperature, filter to get filtrate, obtain fibroin liquid；
（2）In mass ratio 1:10, camphortree leaf powder is stirred and heated with deionized water and is boiled, is carried by steam distillation
Take, collect distillate and stratification, collect upper strata grease and in mass ratio 1:5, by anhydrous calcium chloride and upper strata grease
Mixing, filters to obtain oily filtrate, is prepared into camphor tree leaf volatile oil；
（3）In mass ratio 1:50, cyclodextrin granule is added in fibroin liquid, simultaneously heating water bath is stirred, must mix
Liquid, in mass ratio 1:30, camphor tree leaf volatile oil is added dropwise in mixed liquor, it is still aging and centrifuge after being added dropwise to complete,
Collect lower sediment and wash, dry, modified powder of milling to obtain；
（4）Count in parts by weight, weigh 45~60 parts of PPGs, 2~3 parts of deionized waters, 3~5 parts of modified powders respectively
It is stirred with 55~60 parts of methyl diphenylene diisocyanates, obtains mixed liquor and heating water bath, standing, which is cooled to room temperature, to be applied
Film liquid；
（5）Coating liquid is uniformly coated to the glass pane surface of clean dried, after the completion of to be coated, vacuum freeze drying and take off film
Processing, you can be prepared into a kind of antibiont and stick surfacing.
Step（3）Described camphor tree leaf volatile oil drop rate is 1~2mL/min.
Step（4）Described PPG is any in PPG 4410, PPG 330N and 3050
It is a kind of.
Step（5）Described coating liquid coating thickness is 0.8~1.0mm.
Compared with other method, advantageous effects are the present invention：
（1）The present invention is embedded to cyclodextrin inner by using camphortree leaf as raw material, extracting camphor tree leaf volatile oil, due to
Camphor tree liquid volatile oil can effectively reduce capillary permeability, effectively suppress neutrophil infiltration, and antihistaminicum is reduced
Capillary permeability, effectively suppress the Adhesion property of biological cell, so by being embedded and being filled to membrane material surface,
Effectively reduce Adhesion property of the biology to material surface；
（2）The present invention by fibroin is carrier, is filled by embedded particles and it is formed on polyurethane film surface micro-
The projection of small structure, the Adhesion property of material surface is effectively improved, further improves polyurethane film surface antibiont adhesion
Energy.
Embodiment
Count in parts by weight, choose 65~70 parts of deionized water, 10~15 parts of boiled silk and 55~60 parts of matter
The amount ethanol solution of fraction 75% is placed in beaker, is stirred and is placed in 1~2h of heating water bath, standing at 55~60 DEG C and is cooled to
Room temperature, filter to get filtrate, obtain fibroin liquid；Fresh camphortree leaf is taken, crushed 50 mesh sieves, obtains camphortree leaf powder, in mass ratio
1:10, camphortree leaf powder and deionized water are stirred and are placed in flask, heating is boiled and extracts 2 by steam distillation
~3h, distillate and stratification are collected, collect upper strata grease and in mass ratio 1:5, by anhydrous calcium chloride and upper strata oily
Thing mixes, and filters to obtain oily filtrate, is prepared into camphor tree leaf volatile oil；In mass ratio 1:50, cyclodextrin granule is added to silk
In protein liquid, it is stirred and is placed in 10~15min of heating water bath at 45~50 DEG C, obtain mixed liquor, in mass ratio 1:30, by camphor tree
Leaf volatile oil is added dropwise in mixed liquor, and it is 1~2mL/min to control drop rate, after being added dropwise to complete, still aging 3~5h,
10~15min is centrifuged under 2500~3000r/min, lower sediment is collected and is washed 3~5 times with absolute ethyl alcohol, 55
6~8h, modified powder of milling to obtain are dried at~60 DEG C；Count in parts by weight, weigh 45~60 parts of PPGs, 2~3 respectively
Part deionized water, 3~5 parts of modified powders and 55~60 parts of methyl diphenylene diisocyanates are placed in beaker, 3500~
It is stirred under 4000r/min, obtains mixed liquor and be placed in 3~5h of heating water bath at 75~80 DEG C, standing, which is cooled to room temperature, to be applied
Film liquid is simultaneously uniformly coated coating liquid to the glass pane surface of clean dried, and it is 0.8~1.0mm to control coating thickness, to be coated
After the completion of, vacuum freeze drying and mulching treatment, you can be prepared into a kind of antibiont and stick surfacing.Described polyether polyols
Alcohol is any one in PPG 4410, PPG 330N and 3050
Example 1
Count in parts by weight, it is molten to choose 65 parts of deionized water, 10 parts of boiled silk and 55 parts of the ethanol of mass fraction 75%
Liquid is placed in beaker, is stirred and is placed in heating water bath 1h at 55 DEG C, and standing is cooled to room temperature, filters to get filtrate, obtains silk
Protein liquid；Fresh camphortree leaf is taken, crushed 50 mesh sieves, obtains camphortree leaf powder, in mass ratio 1:10, by camphortree leaf powder and go from
Sub- water, which is stirred, to be placed in flask, and heating is boiled and extracts 2h by steam distillation, collects distillate and stratification,
Collect upper strata grease and in mass ratio 1:5, anhydrous calcium chloride is mixed with upper strata grease, filters to obtain oily filtrate, is prepared
Obtain camphor tree leaf volatile oil；In mass ratio 1:50, cyclodextrin granule is added in fibroin liquid, is stirred and is placed in 45 DEG C
Lower heating water bath 10min, obtains mixed liquor, in mass ratio 1:30, camphor tree leaf volatile oil is added dropwise in mixed liquor, speed is added dropwise in control
Rate is 1mL/min, after being added dropwise to complete, still aging 3h, 10min is centrifuged under 2500r/min, collects lower sediment simultaneously
Washed 3 times with absolute ethyl alcohol, 6h, modified powder of milling to obtain are dried at 55 DEG C；Count in parts by weight, weigh 45 parts of polyethers respectively
4410,2 parts of deionized waters of polyalcohol, 3 parts of modified powders and 55 parts of methyl diphenylene diisocyanates are placed in beaker,
It is stirred under 3500r/min, obtains mixed liquor and be placed in heating water bath 3h at 75 DEG C, standing is cooled to room temperature and obtains coating liquid and incite somebody to action
Uniformly coating is to the glass pane surface of clean dried for coating liquid, and it is 0.8mm to control coating thickness, and after the completion of to be coated, vacuum is cold
Freeze dry and mulching treatment, you can be prepared into a kind of antibiont and stick surfacing.
Example 2
Count in parts by weight, it is molten to choose 67 parts of deionized water, 13 parts of boiled silk and 57 parts of the ethanol of mass fraction 75%
Liquid is placed in beaker, is stirred and is placed in heating water bath 1h at 57 DEG C, and standing is cooled to room temperature, filters to get filtrate, obtains silk
Protein liquid；Fresh camphortree leaf is taken, crushed 50 mesh sieves, obtains camphortree leaf powder, in mass ratio 1:10, by camphortree leaf powder and go from
Sub- water, which is stirred, to be placed in flask, and heating is boiled and extracts 2h by steam distillation, collects distillate and stratification,
Collect upper strata grease and in mass ratio 1:5, anhydrous calcium chloride is mixed with upper strata grease, filters to obtain oily filtrate, is prepared
Obtain camphor tree leaf volatile oil；In mass ratio 1:50, cyclodextrin granule is added in fibroin liquid, is stirred and is placed in 47 DEG C
Lower heating water bath 13min, obtains mixed liquor, in mass ratio 1:30, camphor tree leaf volatile oil is added dropwise in mixed liquor, speed is added dropwise in control
Rate is 2mL/min, after being added dropwise to complete, still aging 4h, 12min is centrifuged under 2700r/min, collects lower sediment simultaneously
Washed 4 times with absolute ethyl alcohol, 7h, modified powder of milling to obtain are dried at 57 DEG C；Count in parts by weight, weigh 47 parts of polyethers respectively
Polyalcohol 330N, 2 parts of deionized waters, 4 parts of modified powders and 57 parts of methyl diphenylene diisocyanates are placed in beaker,
It is stirred under 3700r/min, obtains mixed liquor and be placed in heating water bath 4h at 77 DEG C, standing is cooled to room temperature and obtains coating liquid and incite somebody to action
Uniformly coating is to the glass pane surface of clean dried for coating liquid, and it is 0.9mm to control coating thickness, and after the completion of to be coated, vacuum is cold
Freeze dry and mulching treatment, you can be prepared into a kind of antibiont and stick surfacing.
Example 3
Count in parts by weight, it is molten to choose 70 parts of deionized water, 15 parts of boiled silk and 60 parts of the ethanol of mass fraction 75%
Liquid is placed in beaker, is stirred and is placed in heating water bath 2h at 60 DEG C, and standing is cooled to room temperature, filters to get filtrate, obtains silk
Protein liquid；Fresh camphortree leaf is taken, crushed 50 mesh sieves, obtains camphortree leaf powder, in mass ratio 1:10, by camphortree leaf powder and go from
Sub- water, which is stirred, to be placed in flask, and heating is boiled and extracts 3h by steam distillation, collects distillate and stratification,
Collect upper strata grease and in mass ratio 1:5, anhydrous calcium chloride is mixed with upper strata grease, filters to obtain oily filtrate, is prepared
Obtain camphor tree leaf volatile oil；In mass ratio 1:50, cyclodextrin granule is added in fibroin liquid, is stirred and is placed in 50 DEG C
Lower heating water bath 15min, obtains mixed liquor, in mass ratio 1:30, camphor tree leaf volatile oil is added dropwise in mixed liquor, speed is added dropwise in control
Rate is 2mL/min, after being added dropwise to complete, still aging 5h, 15min is centrifuged under 3000r/min, collects lower sediment simultaneously
Washed 5 times with absolute ethyl alcohol, 8h, modified powder of milling to obtain are dried at 60 DEG C；Count in parts by weight, weigh 60 parts of polyethers respectively
3050,3 parts of deionized waters of polyalcohol, 5 parts of modified powders and 60 parts of methyl diphenylene diisocyanates are placed in beaker,
It is stirred under 4000r/min, obtains mixed liquor and be placed in heating water bath 5h at 80 DEG C, standing is cooled to room temperature and obtains coating liquid and incite somebody to action
Uniformly coating is to the glass pane surface of clean dried for coating liquid, and it is 1.0mm to control coating thickness, and after the completion of to be coated, vacuum is cold
Freeze dry and mulching treatment, you can be prepared into a kind of antibiont and stick surfacing.
The Cu-base composites that the antibiont being prepared into is sticked to surfacing and the production of Shanghai company are detected, and are had
Physical examination is surveyed as follows：
（1）Surface wettability performance is tested
Material sample is cut into fritter, material surface and the contact angle CA of deionized water are determined using contact angle measurement, and
Contact angle photo acquisition is carried out, experimental result is the average value tested three times.
（2）Antibiont Adhesion property is tested
The deep green alga nutrient solutions of 35cm are added in high 4 cm glass container, the sample prepared is suspended in device vertically
Face, it is standing and soak for；Container is placed out of doors（The western beautiful University Town of Shenzhen in Nanshan District of Shenzhen City）, routine observation and record sample shape
State, and photo acquisition and stored frozen sample are carried out, to be observed with SEM the status conditions that stick of sample surfaces.Tool
Body examination test result such as table 1.
The antibiont of table 1 sticks surfacing performance characterization
As shown in Table 1, a kind of obtained antibiont of the present invention sticks surfacing, effectively reduces adhesion of the biology to material surface
Energy.
Claims (4)
1. a kind of antibiont sticks the preparation method of surfacing, it is characterised in that specifically preparation process is：
（1）Count in parts by weight, choose 65~70 parts of deionized water, 10~15 parts of boiled silk and 55~60 parts of ethanol
Solution is placed in beaker, is stirred and heating water bath, standing are cooled to room temperature, filter to get filtrate, obtain fibroin liquid；
（2）In mass ratio 1:10, camphortree leaf powder is stirred and heated with deionized water and is boiled, is carried by steam distillation
Take, collect distillate and stratification, collect upper strata grease and in mass ratio 1:5, by anhydrous calcium chloride and upper strata grease
Mixing, filters to obtain oily filtrate, is prepared into camphor tree leaf volatile oil；
（3）In mass ratio 1:50, cyclodextrin granule is added in fibroin liquid, simultaneously heating water bath is stirred, must mix
Liquid, in mass ratio 1:30, camphor tree leaf volatile oil is added dropwise in mixed liquor, it is still aging and centrifuge after being added dropwise to complete,
Collect lower sediment and wash, dry, modified powder of milling to obtain；
（4）Count in parts by weight, weigh 45~60 parts of PPGs, 2~3 parts of deionized waters, 3~5 parts of modified powders respectively
It is stirred with 55~60 parts of methyl diphenylene diisocyanates, obtains mixed liquor and heating water bath, standing, which is cooled to room temperature, to be applied
Film liquid；
（5）Coating liquid is uniformly coated to the glass pane surface of clean dried, after the completion of to be coated, vacuum freeze drying and take off film
Processing, you can be prepared into a kind of antibiont and stick surfacing.
2. a kind of antibiont according to claim 1 sticks the preparation method of surfacing, it is characterised in that：Step（3）
Described camphor tree leaf volatile oil drop rate is 1~2mL/min.
3. a kind of antibiont according to claim 1 sticks the preparation method of surfacing, it is characterised in that：Step（4）
Described PPG is any one in PPG 4410, PPG 330N and 3050.
4. a kind of antibiont according to claim 1 sticks the preparation method of surfacing, it is characterised in that：Step（5）
Described coating liquid coating thickness is 0.8~1.0mm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110437473A (en) * | 2019-08-19 | 2019-11-12 | 上海万华科聚化工科技发展有限公司 | A kind of polymer powder surface treatment method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105534869A (en) * | 2016-01-30 | 2016-05-04 | 常州市鼎升环保科技有限公司 | Preparation method for anti-ultraviolet silk fibroin |
| CN107027820A (en) * | 2017-05-10 | 2017-08-11 | 南宁为辰科技有限公司 | A kind of pesticide synergistic composition of leaf essential oil containing camphor tree and phoxim |
-
2017
- 2017-10-09 CN CN201710928803.7A patent/CN107603454A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105534869A (en) * | 2016-01-30 | 2016-05-04 | 常州市鼎升环保科技有限公司 | Preparation method for anti-ultraviolet silk fibroin |
| CN107027820A (en) * | 2017-05-10 | 2017-08-11 | 南宁为辰科技有限公司 | A kind of pesticide synergistic composition of leaf essential oil containing camphor tree and phoxim |
Non-Patent Citations (2)
| Title |
|---|
| 刘云鸿: "《中国博士学位论文全文数据库 基础科学辑》", 15 November 2013 * |
| 肖珊美等: "樟树叶挥发油β-环糊精包合物的制备研究", 《光谱实验室》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110437473A (en) * | 2019-08-19 | 2019-11-12 | 上海万华科聚化工科技发展有限公司 | A kind of polymer powder surface treatment method |
| CN110437473B (en) * | 2019-08-19 | 2022-07-12 | 万华化学集团股份有限公司 | Polymer powder surface treatment method |
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Effective date of registration: 20180426 Address after: 213000 Tianhong science and technology building, 801 Changwu Middle Road, Wujin District, Changzhou, Jiangsu 416 Applicant after: Lei Chunsheng Address before: 213102 No. 6-205 Business Plaza, Nuo Cheng Gao Di, Tianning District, Changzhou, Jiangsu Applicant before: Changzhou Kay Textile Co., Ltd. |
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