CN113549349A - Preparation method of surface treating agent for pipette tip - Google Patents
Preparation method of surface treating agent for pipette tip Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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- 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
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/60—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which all the silicon atoms are connected by linkages other than oxygen atoms
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- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
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- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
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- C09D183/00—Coating compositions based on 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; Coating compositions based on derivatives of such polymers
- C09D183/16—Coating compositions based on 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; Coating compositions based on derivatives of such polymers in which all the silicon atoms are connected by linkages other than oxygen atoms
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
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- C08J2483/00—Characterised by the use 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; Derivatives of such polymers
- C08J2483/16—Characterised by the use 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; Derivatives of such polymers in which all the silicon atoms are connected by linkages other than oxygen atoms
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Abstract
The invention relates to the field of preparation of surface treating agents, in particular to a preparation method of a surface treating agent for a pipette tip; the surface treating agent for the pipette head prepared by the method takes modified organic polysilazane and organic silicon modified silica sol as main components, and fluorine-containing acrylic acid copolymer is prepared and added; the two organic components can be grafted on the polypropylene surface of the common pipette tip material, the use method is simple, the surface performance of the treated pipette tip is more stable, the treated pipette tip has excellent chemical resistance, and the treated pipette tip can keep very good lyophobicity in various organic solvents, solutions with different pH values and salt solutions, and is suitable for taking and using various reagents in the fields of medical research, biological research, drug development and the like; the pipette tip treated by the method disclosed by the invention has good lyophobicity for both aqueous solution and organic solution, can completely avoid contamination and residue of reagents, achieves the most accurate taking, and reduces experimental errors.
Description
Technical Field
The invention relates to the field of preparation of surface treating agents, in particular to a preparation method of a surface treating agent for a pipette tip.
Background
In medical research, biological research, drug development laboratories, and other biotechnology applications, it is often desirable to manipulate laboratory samples using pipette tips, which are large consumables, in various laboratory protocols.
CN204522998U discloses liquid-transfering gun rifle head dress box auxiliary device, including the box body, the front of box body is slide damper, and slide damper passes through the mode of spout slide rail with the box body inner wall and is connected, is equipped with the sliding bottom plate in the bottom of box body, and the sliding bottom plate is connected through the mode of spout slide rail with box body inner wall bottom, is equipped with vertical, just the baffle that is parallel to each other in the box body. The invention greatly reduces the time for boxing the gun heads, changes the working mode of manually boxing the gun heads, can insert a row of gun heads into the box at the same time and reduces the error probability. The invention has the advantages of simple structure, convenient operation and low price, brings great convenience to experimenters, saves time, ensures the continuous operation of experiments, overcomes the problems of time and labor waste and the like of the operation of the existing experiment method, and can be popularized and used in schools, laboratories of research institutions and the like.
CN201520043430.1 relates to a pipette head, which comprises a tubular pipette head body, wherein the top of the pipette head body is provided with a pipette head opening, the part of the pipette head opening of the pipette head body, which is connected with a pipette, is provided with a soft rubber layer, the soft rubber layer surrounds the pipette head opening for a circle to form a sleeve-shaped structure, the added soft rubber layer of the utility model can be in closer contact with the nozzle of the pipette to realize sealing by utilizing the elastic performance, the sealing effect is good, the sealing is reliable, and the required sealing effect can be achieved by only needing smaller clamping force between the pipette head body and the nozzle of the pipette, the pipette head body can be installed and withdrawn by only using smaller force, the operation is more labor-saving, and the comfortable sensation of assembly and disassembly operation is good; in addition, the soft rubber layer and the gun head opening of the gun head body are combined to form an integrated structure in a double-material injection molding integrated forming mode, so that the soft rubber layer and the gun head body are combined more tightly and firmly, the sealing effect is better, and the sealing is more reliable.
CN107413410A discloses liquid-transfering gun rifle head dress box auxiliary device, including the box body, the front of box body is slide damper, and slide damper passes through the mode of spout slide rail with the box body inner wall and is connected, is equipped with the sliding bottom plate in the bottom of box body, and the sliding bottom plate is connected through the mode of spout slide rail with box body inner wall bottom, is equipped with vertical, just the baffle that is parallel to each other in the box body. The invention greatly reduces the time for boxing the gun heads, changes the working mode of manually boxing the gun heads, can insert a row of gun heads into the box at the same time and reduces the error probability. The invention has the advantages of simple structure, convenient operation and low price, brings great convenience to experimenters, saves time, ensures the continuous operation of experiments, overcomes the problems of time and labor waste and the like of the operation of the existing experiment method, and can be popularized and used in schools, laboratories of research institutions and the like.
The improvement of the pipette tip in the invention and the prior art mainly focuses on how to conveniently and orderly take the pipette tip, and the problem that the surface of the pipette tip is stained with liquid is basically not concerned. The pipette is used as a tool for quantitatively measuring a small amount of solution (1-20 μ L), and if the surface of the pipette is stained with some liquid when absorbing the solution or a small amount of liquid remains on the inner surface of the pipette when extruding the solution, the pipette causes large errors, thereby causing great errors in experiments and further causing experimental failure. The pipette head of the liquid-transfering gun produced in China at present is mainly made of polypropylene materials, and the problem generally exists.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a surface treating agent for a pipette tip.
A preparation method of a liquid-transfering gun head surface treating agent comprises the following specific scheme:
adding 20-35 parts of dimethylbenzene and 10-20 parts of isopropyl acetate into a reaction kettle according to the mass parts, uniformly mixing to form a mixed solution, using nitrogen for protection, controlling the temperature to be 65-85 ℃, then uniformly mixing 6-12 parts of octyl dodecafluoro-7- (trifluoromethyl) acrylate, 15-20 parts of hydroxyethyl methacrylate, 0.1-0.6 part of initiator and 20-30 parts of isopropyl acetate, slowly adding into the reaction kettle, controlling the adding for 1-5h, adding 0.01-0.1 part of initiator after the completion of the reaction, continuing to react for 90-180min, cooling to room temperature after the completion of the reaction, filtering after mechanical demulsification, washing, then mixing 0.5-1.8 parts of obtained solid, 10-18 parts of modified organic polysilazane and 60-120 parts of acetone, performing ultrasonic treatment for 30-90min, after the solution is fully dissolved, 20-40 parts of organic silicon modified silica sol is added, and the surface treating agent for the pipette tip can be obtained after ultrasonic treatment for 10-30 min;
the preparation method of the organic silicon modified silica sol comprises the following steps:
according to the mass portion, under the condition of rapid stirring, 5-10 portions of 0.1% -0.5% hydrochloric acid are added into 50-80 portions of silica sol, then 0.1-0.8 part of ethyl orthosilicate and 0.05-0.3 part of dodecyl trimethoxy silane are added into a reaction kettle, and the mixture is stirred and reacted for 24-48h under the condition of room temperature, thus obtaining the organic silicon modified silica sol.
The solid content of the silica sol is 18-25%.
The initiator is azobisisobutyronitrile or benzoyl peroxide.
The mechanical demulsification method is a centrifugal demulsification method.
The modified organic polysilazane is prepared by the following method:
adding 5-12 parts of mercaptopropyl methyl dimethoxysilane, 10-18 parts of 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclo-tetrasilazane into 200 parts of chloroform according to the mass parts, stirring and mixing uniformly, adding 0.05-0.5 part of ultraviolet initiator, reacting for 60-120min under ultraviolet irradiation after mixing uniformly, and evaporating the solvent after completion to obtain the modified organic polysilazane.
The ultraviolet light initiator is benzoyl formate or dimethoxy-alpha-phenyl acetophenone or 1-hydroxy cyclohexyl phenyl ketone.
The application method of the surface treating agent for the pipette tip comprises the following steps: immersing the head of the liquid-transferring gun in the surface treating agent, controlling the temperature to be 35-45 ℃, carrying out ultrasonic treatment for 10-30min, then taking out, drying the residual liquid, and carrying out treatment at the temperature of 110-130 ℃ for 20-30 min.
The invention relates to a preparation method of a pipette tip surface treating agent, which is prepared by taking modified organic polysilazane and organic silicon modified silica sol as main components and adding a fluorine-containing acrylic copolymer; the two organic components can be grafted on the polypropylene surface of the common pipette tip material, the use method is simple, the surface performance of the treated pipette tip is more stable, the treated pipette tip has excellent chemical resistance, and the treated pipette tip can keep very good lyophobicity in various organic solvents, solutions with different pH values and salt solutions, and is suitable for taking and using various reagents in the fields of medical research, biological research, drug development and the like; the pipette tip treated by the method disclosed by the invention has good lyophobicity for both aqueous solution and organic solution, can completely avoid contamination and residue of reagents, achieves the most accurate taking, and reduces experimental errors.
Detailed Description
The invention is further illustrated by the following specific examples:
the performance of the surface treating agent prepared by the experiment is measured, the polypropylene sheet is immersed in the surface treating agent, the temperature is controlled at 40 ℃, the ultrasonic treatment is carried out for 30min, then the polypropylene sheet is taken out, the residual liquid is dried, and the test is carried out after the polypropylene sheet is treated for 20-30min at 120 ℃; the contact angle of the material is measured by using a contact angle measuring instrument (OCA 20), and the drops of the test liquid are 10 mu L of distilled water and 10 mu L of n-hexadecane respectively. To reduce experimental error, the same sample was measured 6 times and the average was calculated. Meanwhile, pure water is used for a blank experiment. The chemical stability evaluation method of the coating is to soak the coating in n-hexane, p-xylene, ethanol, acetone, ethyl acetate, solutions with different pH values (pH values of 1, 7 and 14) and 1mol L respectively-1Was added to the NaCl solution for 10 hours, and then the contact angle thereof was measured to investigate the resistance of the coating to organic solvents, acids, bases and salt solutions.
Example 1
A preparation method of a liquid-transfering gun head surface treating agent comprises the following specific scheme:
adding 20g of dimethylbenzene and 10g of isopropyl acetate into a reaction kettle according to the mass parts, uniformly mixing to form a mixed solution, controlling the temperature to be 65 ℃ by using nitrogen protection, then slowly adding 6g of octyl dodecafluoro-7- (trifluoromethyl) acrylate, 15g of hydroxyethyl methacrylate, 0.1g of initiator and 20g of isopropyl acetate into the reaction kettle after uniformly mixing, controlling the adding for 1h to be finished, then adding 0.01g of initiator to continue to react for 90min, cooling to room temperature after the reaction is finished, filtering and washing after mechanical emulsion breaking, then carrying out ultrasonic treatment for 30min after mixing 0.5g of obtained solid, 10g of modified organic polysilazane and 60g of acetone, adding 20g of organic silicon modified silica sol after full dissolution, and carrying out ultrasonic treatment for 10min to obtain the surface treating agent for the pipette tip;
the preparation method of the organic silicon modified silica sol comprises the following steps:
according to the mass portion, under the condition of rapid stirring, 5g of 0.1% hydrochloric acid is added into 50g of silica sol, then 0.1g of tetraethoxysilane and 0.05g of dodecyl trimethoxy silane are added into a reaction kettle, and the mixture is stirred and reacted for 24 hours under the condition of room temperature, thus obtaining the organic silicon modified silica sol.
The solid content of the silica sol is 18 percent.
The initiator is azobisisobutyronitrile.
The mechanical demulsification method is a centrifugal demulsification method.
The modified organic polysilazane is prepared by the following method:
according to the mass portion, 5g of mercaptopropyl methyldimethoxysilane and 10g of 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclotetrasilazane are added into 100g of chloroform, stirred and mixed evenly, then 0.05g of ultraviolet initiator is added, the mixture is reacted for 60min under the irradiation of ultraviolet light after being mixed evenly, and the solvent is evaporated after the reaction is finished, thus obtaining the modified organic polysilazane.
The ultraviolet light initiator is benzoyl formic ether.
Example 2
A preparation method of a liquid-transfering gun head surface treating agent comprises the following specific scheme:
adding 28g of dimethylbenzene and 15g of isopropyl acetate into a reaction kettle according to the mass parts, uniformly mixing to form a mixed solution, controlling the temperature to be 75 ℃ by using nitrogen protection, then slowly adding 9g of dodecyl-7- (trifluoromethyl) octyl acrylate, 18g of hydroxyethyl methacrylate, 0.3g of initiator and 25g of isopropyl acetate into the reaction kettle after uniformly mixing, controlling the adding for 3h to be finished, then adding 0.06g of initiator to continue to react for 120min, cooling to room temperature after the reaction is finished, filtering and washing after mechanical emulsion breaking, then mixing 1.2g of the obtained solid, 16g of modified organic polysilazane and 90g of acetone, carrying out ultrasonic treatment for 60min, adding 30g of organic silicon modified silica sol after full dissolution, and carrying out ultrasonic treatment for 20min to obtain the surface treating agent for the pipette tip;
the preparation method of the organic silicon modified silica sol comprises the following steps:
according to the mass parts, under the condition of rapid stirring, 8g of 0.3% hydrochloric acid is added into 60g of silica sol, then 0.5g of tetraethoxysilane and 0.15g of dodecyl trimethoxy silane are added into a reaction kettle, and the mixture is stirred and reacted for 36 hours under the condition of room temperature, thus obtaining the organic silicon modified silica sol.
The solid content of the silica sol is 22 percent.
The initiator is benzoyl peroxide.
The mechanical demulsification method is a centrifugal demulsification method.
The modified organic polysilazane is prepared by the following method:
adding 8g of mercaptopropyl methyldimethoxysilane, 14g of 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinylcyclotetrasilazane into 150g of chloroform according to the mass parts, stirring and mixing uniformly, adding 0.25g of ultraviolet initiator, mixing uniformly, reacting for 90min under the irradiation of ultraviolet light, and evaporating the solvent after the reaction is finished to obtain the modified organic polysilazane.
The ultraviolet light initiator is dimethoxy-alpha-phenylacetophenone.
Example 3
A preparation method of a liquid-transfering gun head surface treating agent comprises the following specific scheme:
adding 35g of xylene and 20g of isopropyl acetate into a reaction kettle according to the mass parts, uniformly mixing to form a mixed solution, controlling the temperature to be 85 ℃ by using nitrogen protection, then slowly adding 12g of dodecyl-7- (trifluoromethyl) octyl acrylate, 20g of hydroxyethyl methacrylate, 0.6g of initiator and 30g of isopropyl acetate into the reaction kettle after uniformly mixing, controlling the adding for 5h to be finished, adding 0.1g of initiator after finishing the adding, continuing to react for 180min, cooling to room temperature after the reaction is finished, filtering and washing after mechanical emulsion breaking, then mixing 1.8g of the obtained solid, 18g of modified organic polysilazane and 120g of acetone, carrying out ultrasonic treatment for 90min, adding 40g of organic silicon modified silica sol after full dissolution, and carrying out ultrasonic treatment for 30min to obtain the surface treating agent for the pipette tip;
the preparation method of the organic silicon modified silica sol comprises the following steps:
according to the mass portion, under the condition of rapid stirring, 10g of 0.5% hydrochloric acid is added into 80g of silica sol, then 0.8 g of ethyl orthosilicate and 0.3g of dodecyl trimethoxy silane are added into a reaction kettle, and the mixture is stirred and reacted for 48 hours under the condition of room temperature, thus obtaining the organic silicon modified silica sol.
The solid content of the silica sol is 25 percent.
The initiator is benzoyl peroxide.
The mechanical demulsification method is a centrifugal demulsification method.
The modified organic polysilazane is prepared by the following method:
according to the mass portion, 12g of mercaptopropyl methyldimethoxysilane, 18g of 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclotetrasilazane are added into 200g of chloroform, 0.5g of ultraviolet initiator is added after stirring and mixing uniformly, reaction is carried out for 120min under the irradiation of ultraviolet light after mixing uniformly, and the solvent is evaporated after completion, thus obtaining the modified organic polysilazane.
The ultraviolet initiator is 1-hydroxycyclohexyl phenyl ketone.
Surface contact angle data for polypropylene sheets treated in examples 1-3 and the blank control.
Comparative example 1
A preparation method of a liquid-transfering gun head surface treating agent comprises the following specific scheme:
adding 20g of dimethylbenzene and 10g of isopropyl acetate into a reaction kettle according to the mass parts, uniformly mixing to form a mixed solution, using nitrogen for protection, controlling the temperature to be 65 ℃, then slowly adding 6g of octyl dodecafluoro-7- (trifluoromethyl) acrylate, 15g of hydroxyethyl methacrylate, 0.1g of initiator and 20g of isopropyl acetate into the reaction kettle after uniformly mixing, controlling the adding for 1h to be finished, adding 0.01g of initiator after finishing the adding, continuing to react for 90min, cooling to room temperature after the reaction is finished, filtering and washing after mechanical emulsion breaking, then mixing 0.5g of obtained solid, 10g of modified organic polysilazane and 60g of acetone, and carrying out ultrasonic treatment for 30min to obtain the surface treating agent for the pipette tip;
the initiator is azobisisobutyronitrile.
The mechanical demulsification method is a centrifugal demulsification method.
The modified organic polysilazane is prepared by the following method:
according to the mass portion, 5g of mercaptopropyl methyldimethoxysilane and 10g of 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclotetrasilazane are added into 100g of chloroform, stirred and mixed evenly, then 0.05g of ultraviolet initiator is added, the mixture is reacted for 60min under the irradiation of ultraviolet light after being mixed evenly, and the solvent is evaporated after the reaction is finished, thus obtaining the modified organic polysilazane.
The ultraviolet light initiator is benzoyl formic ether.
Comparative example 2
A preparation method of a liquid-transfering gun head surface treating agent comprises the following specific scheme:
mixing 10g of modified organic polysilazane and 60g of acetone according to the parts by mass, carrying out ultrasonic treatment for 30min, adding 20g of organic silicon modified silica sol after fully dissolving, and carrying out ultrasonic treatment for 10min to obtain the surface treating agent for the pipette tip;
the preparation method of the organic silicon modified silica sol comprises the following steps:
according to the mass portion, under the condition of rapid stirring, 5g of 0.1% hydrochloric acid is added into 50g of silica sol, then 0.1g of tetraethoxysilane and 0.05g of dodecyl trimethoxy silane are added into a reaction kettle, and the mixture is stirred and reacted for 24 hours under the condition of room temperature, thus obtaining the organic silicon modified silica sol.
The solid content of the silica sol is 18 percent.
The modified organic polysilazane is prepared by the following method:
according to the mass portion, 5g of mercaptopropyl methyldimethoxysilane and 10g of 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclotetrasilazane are added into 100g of chloroform, stirred and mixed evenly, then 0.05g of ultraviolet initiator is added, the mixture is reacted for 60min under the irradiation of ultraviolet light after being mixed evenly, and the solvent is evaporated after the reaction is finished, thus obtaining the modified organic polysilazane.
The ultraviolet light initiator is benzoyl formic ether.
Comparative example 3
A preparation method of a liquid-transfering gun head surface treating agent comprises the following specific scheme:
adding 20g of dimethylbenzene and 10g of isopropyl acetate into a reaction kettle according to the mass parts, uniformly mixing to form a mixed solution, controlling the temperature to be 65 ℃ by using nitrogen protection, then slowly adding 6g of octyl dodecafluoro-7- (trifluoromethyl) acrylate, 15g of hydroxyethyl methacrylate, 0.1g of initiator and 20g of isopropyl acetate into the reaction kettle after uniformly mixing, controlling the adding for 1h to be finished, adding 0.01g of initiator after finishing the adding, continuing to react for 90min, cooling to the room temperature after the reaction is finished, filtering and washing after mechanical emulsion breaking, then mixing 0.5g of obtained solid with 60g of acetone, carrying out ultrasonic treatment for 30min, adding 20g of organic silicon modified silica sol after full dissolution, and carrying out ultrasonic treatment for 10min to obtain the surface treating agent for the pipette tip;
the preparation method of the organic silicon modified silica sol comprises the following steps:
according to the mass portion, under the condition of rapid stirring, 5g of 0.1% hydrochloric acid is added into 50g of silica sol, then 0.1g of tetraethoxysilane and 0.05g of dodecyl trimethoxy silane are added into a reaction kettle, and the mixture is stirred and reacted for 24 hours under the condition of room temperature, thus obtaining the organic silicon modified silica sol.
The solid content of the silica sol is 18 percent.
The initiator is azobisisobutyronitrile.
The mechanical demulsification method is a centrifugal demulsification method.
Surface contact angle data for comparative examples 1-3 and the blank control treated polypropylene sheets.
| Contact angle (Water/n-hexadecane) | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Is not aged | 137.1°/141.4° | 138.4°/143.5° | 131.7°/140.9° |
| N-hexane | 131.4°/127.1° | 121.7°/126.4° | 124.7°/128.1° |
| Para-xylene | 132.1°/122.7° | 118.7°/120.8° | 112.3°/115.1° |
| Ethanol | 135.7°/132.9° | 124.7°/128.1° | 121.0°/125.1° |
| Acetone (II) | 131.9°/131.7° | 126.1°/131.8° | 123.1°/124.8° |
| Ethyl acetate | 127.1°/121.8° | 123.7°/129.2° | 120.7°/121.4° |
| pH value of 1 | 129.8°/119.6° | 114.0°/119.4° | 103.7°/111.3° |
| pH 7 | 136.8°/140.8° | 136.1°/143.2° | 128.7°/139.1° |
| The pH value is 14 | 132.9°/123.6° | 104.7°/115.6° | 101.3°/112.5° |
| NaCl solution | 137.0°/140.7° | 133.9°/142.1° | 131.6°/139.7° |
Claims (7)
1. A preparation method of a liquid-transfering gun head surface treating agent comprises the following specific scheme:
adding 20-35 parts of dimethylbenzene and 10-20 parts of isopropyl acetate into a reaction kettle according to the mass parts, uniformly mixing to form a mixed solution, using nitrogen for protection, controlling the temperature to be 65-85 ℃, then uniformly mixing 6-12 parts of octyl dodecafluoro-7- (trifluoromethyl) acrylate, 15-20 parts of hydroxyethyl methacrylate, 0.1-0.6 part of initiator and 20-30 parts of isopropyl acetate, slowly adding into the reaction kettle, controlling the adding for 1-5h, adding 0.01-0.1 part of initiator after the completion of the reaction, continuing to react for 90-180min, cooling to room temperature after the completion of the reaction, filtering after mechanical demulsification, washing, then mixing 0.5-1.8 parts of obtained solid, 10-18 parts of modified organic polysilazane and 60-120 parts of acetone, performing ultrasonic treatment for 30-90min, after the solution is fully dissolved, 20-40 parts of organic silicon modified silica sol is added, and the surface treating agent for the pipette tip can be obtained after ultrasonic treatment for 10-30 min;
the preparation method of the organic silicon modified silica sol comprises the following steps:
according to the mass portion, under the condition of rapid stirring, 5-10 portions of 0.1% -0.5% hydrochloric acid are added into 50-80 portions of silica sol, then 0.1-0.8 part of ethyl orthosilicate and 0.05-0.3 part of dodecyl trimethoxy silane are added into a reaction kettle, and the mixture is stirred and reacted for 24-48h under the condition of room temperature, thus obtaining the organic silicon modified silica sol.
2. The preparation method of the surface treating agent for the pipette tip according to claim 1, characterized by comprising the following steps: the modified organic polysilazane is prepared by the following method:
adding 5-12 parts of mercaptopropyl methyl dimethoxysilane, 10-18 parts of 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclo-tetrasilazane into 200 parts of chloroform according to the mass parts, stirring and mixing uniformly, adding 0.05-0.5 part of ultraviolet initiator, reacting for 60-120min under ultraviolet irradiation after mixing uniformly, and evaporating the solvent after completion to obtain the modified organic polysilazane.
3. The preparation method of the surface treating agent for the pipette tip according to claim 2, characterized by comprising the following steps: the ultraviolet light initiator is benzoyl formate or dimethoxy-alpha-phenyl acetophenone or 1-hydroxy cyclohexyl phenyl ketone.
4. The preparation method of the surface treating agent for the pipette tip according to claim 1, characterized by comprising the following steps: the initiator is azobisisobutyronitrile or benzoyl peroxide.
5. The preparation method of the surface treating agent for the pipette tip according to claim 1, characterized by comprising the following steps: the mechanical demulsification method is a centrifugal demulsification method.
6. The preparation method of the surface treating agent for the pipette tip according to claim 1, characterized by comprising the following steps: the solid content of the silica sol is 18-25%.
7. The preparation method of the surface treating agent for the pipette tip according to claim 1, characterized by comprising the following steps: the application method of the surface treating agent for the pipette tip comprises the following steps: immersing the head of the liquid-transferring gun in the surface treating agent, controlling the temperature to be 35-45 ℃, carrying out ultrasonic treatment for 10-30min, then taking out, drying the residual liquid, and carrying out treatment at the temperature of 110-130 ℃ for 20-30 min.
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| CN115403810A (en) * | 2022-09-29 | 2022-11-29 | 浙江首康生物科技有限公司 | High-oleophobic pipette head and preparation method thereof |
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