CN107441563A - A kind of medicine equipment imports the preparation method of lubricant - Google Patents
A kind of medicine equipment imports the preparation method of lubricant Download PDFInfo
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- CN107441563A CN107441563A CN201710500335.3A CN201710500335A CN107441563A CN 107441563 A CN107441563 A CN 107441563A CN 201710500335 A CN201710500335 A CN 201710500335A CN 107441563 A CN107441563 A CN 107441563A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/04—Macromolecular materials
- A61L31/06—Macromolecular materials obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/04—Macromolecular materials
- A61L31/042—Polysaccharides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0215—Sulfur-containing compounds
- B01J31/0225—Sulfur-containing compounds comprising sulfonic acid groups or the corresponding salts
- B01J31/0227—Sulfur-containing compounds comprising sulfonic acid groups or the corresponding salts being perfluorinated, i.e. comprising at least one perfluorinated moiety as substructure in case of polyfunctional compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
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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
- 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
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
- C08G77/08—Preparatory processes characterised by the catalysts used
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/10—Materials for lubricating medical devices
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
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- Polymers & Plastics (AREA)
- Lubricants (AREA)
- Medicinal Preparation (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses the preparation method that a kind of medicine equipment imports lubricant, comprise the following steps：Dimethicone is prepared first, according to each component dosage, glycerine, xanthans, dimethicone, potassium sorbate, flavoring essence, purified water are weighed respectively, and load weighted each raw material is poured into mixer, 20min is stirred under 600r/min rotating speed, the mixed liquor obtained after stirring pours into filling in bottle placer, plastic sealing bag is then charged into, 200 DEG C of sealings, the product and specification of good seal are put into carton, irradiation sterilization, medicine equipment is made and imports lubricant.Medicine equipment disclosed by the invention imports lubricant, and when apparatus imports with good lubrication, to the corrosion-free effect of equipment surfaces, chemical stability is good, harmless.
Description
Technical field：
The present invention relates to biomedical materials field, is specifically related to the preparation side that a kind of medicine equipment imports lubricant
Method.
Background technology：
The usage amount of medicine equipment is very big, and use range is also very extensive.With the development of modern science and technology, medicine equipment
Effect in modern medical service diagnosis is more and more obvious.However, clinically the requirement to medicine equipment is very strict, because
It usually needs the skin with human body in use, tissue, and the contact such as body fluid, some also needs to be chronically implanted in vivo, this
Require conduit not only to meet the requirement of organism mechanical property in itself, will also have good blood compatibility, lubricity,
Histocompatbility and biocompatibility etc..
Domestic current medical device materials are mostly hydrophobic material, and such as polyvinyl chloride, silicon rubber, it is controlled to clinic
While treatment brings convenient, there is also some problems.Larger friction resistance can be produced due to being hydrophobic material, during use
Power, blood vessel is easily caused, cavity organization is damaged and causes other inflammation, pain is often brought to patient.Solves the problem therewith
Method be medical apparatus surface coat one layer of lubricant.Following condition must be possessed by importing lubricant as medicine equipment：
(1) there is excellent lubricity；(2) it must be the aqueous solution；(3) it is nontoxic to human body；(4) to human epidermal without repulsive interaction；(5) most
It is well macromolecular, it is impossible to through the epidermal cell of human body, can excrete external；(6) sterilization treatment is had to pass through.
The content of the invention：
It is an object of the invention to provide a kind of medicine equipment to import lubricant, and its greasy property is good, has certain antibacterial
Effect, chemical stability is good, harmless.
It is a further object to provide the preparation method that the medicine equipment imports lubricant.
To achieve the above object, the present invention uses following technical scheme：
A kind of medicine equipment imports the preparation method of lubricant, comprises the following steps：
(1) chrome green and deionized water are mixed, in the state of 10-15 DEG C of temperature, speed of agitator 1000r/min
Then stirring is added dropwise the concentrated sulfuric acid, continues to stir 30min, obtained solution A after being added dropwise while stirring to solid dissolving；
(2) poly glycol monomethyl ether and absolute ethyl alcohol are mixed into solid dissolving, step (1) system is then slowly added dropwise
The solution A obtained, stirring reaction 15-20h, toward addition isopropanol terminating reaction in reaction system after the completion of reaction, is filtered at room temperature,
Filtrate adds deionized water, and rotary evaporation removes absolute ethyl alcohol, adds sodium acid carbonate in remaining filtrate until without gas in filtrate
Bubble produces, and then removes the water in filtrate, and remaining filtrate removes chloroform with chloroform extraction, suction filtration, filtrate, then
Hydrochloric acid solution is added into remnants filtrate to filtrate pH to 1-2, then steams water and hydrogen chloride gas, last remaining material
With chloroform extraction, filter, filtrate steams chloroform, and carboxylated poly glycol monomethyl ether is made after cooling；
(3) it will be placed in after y-type zeolite steam treatment in deionized water, 1h be ultrasonically treated under 500W power, is then added
Carboxylated poly glycol monomethyl ether obtained above, and the concentrated sulfuric acid is added dropwise, after being well mixed, 90 DEG C are to slowly warm up to, backflow is anti-
Answer 5-10h, backflow to be cooled to room temperature after terminating, filter, solid is washed repeatedly with absolute ethyl alcohol, is dried, and obtains being modified the boiling of Y types
Stone；
(4) modified zeolite of Y-type obtained above is placed in pressure ＜ 0.1MPa reaction vessel, then by trifluoromethyl
Sulfonic acid is slowly injected into reaction vessel, obtains loaded catalyst；
(5) it is added to after being well mixed the methyl cyclosiloxane mixed methylcyclosiloxane after drying process and HMDO
In reaction vessel, under nitrogen protection, loaded catalyst obtained above is added into reactor, slowly heating after being well mixed
To 60-70 DEG C, isothermal reaction 2-4h, reaction is cooled to room temperature after terminating, and filters, and obtained filtrate is washed with deionized into
Property simultaneously removes low-boiling-point substance, obtains dimethicone；
(6) according to each component dosage, glycerine, xanthans, dimethicone, potassium sorbate, flavoring essence, pure is weighed respectively
Change water, load weighted each raw material is poured into mixer, 20min is stirred under 600r/min rotating speed, is mixed after stirring
Close liquid；
(7) mixed liquor obtained above is poured into filling in bottle placer, is then charged into plastic sealing bag, 200 DEG C of sealings are close
The product and specification sealed are put into carton, irradiation sterilization, medicine equipment are made and imports lubricant.
As the preferred of above-mentioned technical proposal, each component dosage is respectively in parts by weight：Glycerine 3-6 parts, xanthans
0.1-0.5 parts, dimethicone 8-12 parts, potassium sorbate 0.03-0.07 parts, flavoring essence 0.1-0.3 parts, purified water 80-85
Part.
As the preferred of above-mentioned technical proposal, each component dosage is respectively in parts by weight：5 parts of glycerine, xanthans 0.5
Part, 10 parts of dimethicone, 0.05 part of potassium sorbate, 0.1 part of flavoring essence, 84.35 parts of purified water.
As the preferred of above-mentioned technical proposal, in step (1), the amount ratio of the chrome green and deionized water is
2.35g：40mL.
As the preferred of above-mentioned technical proposal, in step (1), the volume ratio of the concentrated sulfuric acid and deionized water is 1:13.
As the preferred of above-mentioned technical proposal, in step (2), the mass ratio of the poly glycol monomethyl ether and solution A is
1g：(0.95-1)mL.
It is the y-type zeolite, carboxylated poly glycol monomethyl ether, dense in step (3) as the preferred of above-mentioned technical proposal
The mass ratio of sulfuric acid is 1:0.5:0.033.
As the preferred of above-mentioned technical proposal, in step (4), the modified zeolite of Y-type, the mass ratio of trifluoromethane sulfonic acid
For 3：(1-2).
As the preferred of above-mentioned technical proposal, in step (5), methyl cyclosiloxane mixed methylcyclosiloxane, HMDO,
The mass ratio of loaded catalyst is 5：(0.8-2.8)：(0.5-1).
The invention has the advantages that：
Medicinal dimethicone is made in the present invention first, and its high income, purity is high, and viscosity is controllable, and in dimethicone
Trifluoromethane sulfonic acid is loaded as catalyst using y-type zeolite during preparation, it can effectively control the catalysis of catalyst
Effect, so as to control the viscosity of obtained dimethicone, and the high income of the dimethicone, modest viscosity；And in order to change
The compatibility of kind catalyst and reactant, the present invention effectively increase the catalysis effect of catalyst by being modified to y-type zeolite
Fruit；
Lubricant high lubricating effect produced by the present invention, and preparation cost is low, nontoxic, chemical stability is good.
Embodiment：
In order to be better understood from the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solving
The present invention is released, any restriction will not be formed to the present invention.
Embodiment 1
A kind of medicine equipment imports lubricant, in parts by weight, including following components：
5 parts of glycerine, 0.5 part of xanthans,
10 parts of dimethicone, 0.05 part of potassium sorbate,
0.1 part of flavoring essence, 84.35 parts of purified water,
Its preparation method comprises the following steps：
(1) chrome green and deionized water are mixed, in the state of 10-15 DEG C of temperature, speed of agitator 1000r/min
Then stirring is added dropwise the concentrated sulfuric acid, continues to stir 30min, obtained solution A after being added dropwise while stirring to solid dissolving；
Wherein, chrome green and the amount ratio of deionized water are 2.35g：The volume ratio of 40mL, the concentrated sulfuric acid and deionized water is 1:13；
(2) poly glycol monomethyl ether and absolute ethyl alcohol are mixed into solid dissolving, step (1) system is then slowly added dropwise
The solution A obtained, stirring reaction 15h, toward addition isopropanol terminating reaction in reaction system after the completion of reaction, is filtered, filter at room temperature
Liquid adds deionized water, and rotary evaporation removes absolute ethyl alcohol, and sodium acid carbonate is added in remaining filtrate up to bubble-free in filtrate
Produce, then remove the water in filtrate, remaining filtrate removes chloroform, Ran Houxiang with chloroform extraction, suction filtration, filtrate
Hydrochloric acid solution is added in remaining filtrate to filtrate pH to 1-2, then steams water and hydrogen chloride gas, last remaining material is used
Chloroform extraction, filter, filtrate steams chloroform, and carboxylated poly glycol monomethyl ether is made after cooling；Wherein, poly- second two
Alcohol monomethyl ether and the mass ratio of solution A are 1g：0.95mL；
(3) it will be placed in after y-type zeolite steam treatment in deionized water, 1h be ultrasonically treated under 500W power, is then added
Carboxylated poly glycol monomethyl ether obtained above, and the concentrated sulfuric acid is added dropwise, after being well mixed, 90 DEG C are to slowly warm up to, backflow is anti-
Answer 5h, backflow to be cooled to room temperature after terminating, filter, solid is washed repeatedly with absolute ethyl alcohol, is dried, is obtained modified zeolite of Y-type；Its
In, y-type zeolite, carboxylated poly glycol monomethyl ether, the mass ratio of the concentrated sulfuric acid are 1:0.5:0.033；
(4) modified zeolite of Y-type obtained above is placed in pressure ＜ 0.1MPa reaction vessel, then by trifluoromethyl
Sulfonic acid is slowly injected into reaction vessel, obtains loaded catalyst；Wherein, the quality of modified zeolite of Y-type, trifluoromethane sulfonic acid
Than for 3：1；
(5) it is added to after being well mixed the methyl cyclosiloxane mixed methylcyclosiloxane after drying process and HMDO
In reaction vessel, under nitrogen protection, loaded catalyst obtained above is added into reactor, slowly heating after being well mixed
To 60-70 DEG C, isothermal reaction 2h, reaction is cooled to room temperature after terminating, and filters, and obtained filtrate is washed with deionized to neutrality
And low-boiling-point substance is removed, obtain dimethicone；Wherein, methyl cyclosiloxane mixed methylcyclosiloxane, HMDO, support type are urged
The mass ratio of agent is 5：0.8：0.5；
(6) according to each component dosage, glycerine, xanthans, dimethicone, potassium sorbate, flavoring essence, pure is weighed respectively
Change water, load weighted each raw material is poured into mixer, 20min is stirred under 600r/min rotating speed, is mixed after stirring
Close liquid；
(7) mixed liquor obtained above is poured into filling in bottle placer, is then charged into plastic sealing bag, 200 DEG C of sealings are close
The product and specification sealed are put into carton, irradiation sterilization, medicine equipment are made and imports lubricant.
Embodiment 2
A kind of medicine equipment imports lubricant, in parts by weight, including following components：
3 parts of glycerine, 0.1 part of xanthans,
8 parts of dimethicone, 0.03 part of potassium sorbate,
0.1 part of flavoring essence, 80 parts of purified water,
Its preparation method comprises the following steps：
(1) chrome green and deionized water are mixed, in the state of 10-15 DEG C of temperature, speed of agitator 1000r/min
Then stirring is added dropwise the concentrated sulfuric acid, continues to stir 30min, obtained solution A after being added dropwise while stirring to solid dissolving；
Wherein, chrome green and the amount ratio of deionized water are 2.35g：The volume ratio of 40mL, the concentrated sulfuric acid and deionized water is 1:13；
(2) poly glycol monomethyl ether and absolute ethyl alcohol are mixed into solid dissolving, step (1) system is then slowly added dropwise
The solution A obtained, stirring reaction 20h, toward addition isopropanol terminating reaction in reaction system after the completion of reaction, is filtered, filter at room temperature
Liquid adds deionized water, and rotary evaporation removes absolute ethyl alcohol, and sodium acid carbonate is added in remaining filtrate up to bubble-free in filtrate
Produce, then remove the water in filtrate, remaining filtrate removes chloroform, Ran Houxiang with chloroform extraction, suction filtration, filtrate
Hydrochloric acid solution is added in remaining filtrate to filtrate pH to 1-2, then steams water and hydrogen chloride gas, last remaining material is used
Chloroform extraction, filter, filtrate steams chloroform, and carboxylated poly glycol monomethyl ether is made after cooling；Wherein, poly- second two
Alcohol monomethyl ether and the mass ratio of solution A are 1g：1mL；
(3) it will be placed in after y-type zeolite steam treatment in deionized water, 1h be ultrasonically treated under 500W power, is then added
Carboxylated poly glycol monomethyl ether obtained above, and the concentrated sulfuric acid is added dropwise, after being well mixed, 90 DEG C are to slowly warm up to, backflow is anti-
Answer 10h, backflow to be cooled to room temperature after terminating, filter, solid is washed repeatedly with absolute ethyl alcohol, is dried, is obtained modified zeolite of Y-type；
Wherein, y-type zeolite, carboxylated poly glycol monomethyl ether, the mass ratio of the concentrated sulfuric acid are 1:0.5:0.033；
(4) modified zeolite of Y-type obtained above is placed in pressure ＜ 0.1MPa reaction vessel, then by trifluoromethyl
Sulfonic acid is slowly injected into reaction vessel, obtains loaded catalyst；Wherein, the quality of modified zeolite of Y-type, trifluoromethane sulfonic acid
Than for 3：2；
(5) it is added to after being well mixed the methyl cyclosiloxane mixed methylcyclosiloxane after drying process and HMDO
In reaction vessel, under nitrogen protection, loaded catalyst obtained above is added into reactor, slowly heating after being well mixed
To 60-70 DEG C, isothermal reaction 4h, reaction is cooled to room temperature after terminating, and filters, and obtained filtrate is washed with deionized to neutrality
And low-boiling-point substance is removed, obtain dimethicone；Wherein, methyl cyclosiloxane mixed methylcyclosiloxane, HMDO, support type are urged
The mass ratio of agent is 5：2.8：1；
(6) according to each component dosage, glycerine, xanthans, dimethicone, potassium sorbate, flavoring essence, pure is weighed respectively
Change water, load weighted each raw material is poured into mixer, 20min is stirred under 600r/min rotating speed, is mixed after stirring
Close liquid；
(7) mixed liquor obtained above is poured into filling in bottle placer, is then charged into plastic sealing bag, 200 DEG C of sealings are close
The product and specification sealed are put into carton, irradiation sterilization, medicine equipment are made and imports lubricant.
Embodiment 3
A kind of medicine equipment imports lubricant, in parts by weight, including following components：
6 parts of glycerine, 0.5 part of xanthans,
12 parts of dimethicone, 0.07 part of potassium sorbate,
0.3 part of flavoring essence, 85 parts of purified water,
Its preparation method comprises the following steps：
(1) chrome green and deionized water are mixed, in the state of 10-15 DEG C of temperature, speed of agitator 1000r/min
Then stirring is added dropwise the concentrated sulfuric acid, continues to stir 30min, obtained solution A after being added dropwise while stirring to solid dissolving；
Wherein, chrome green and the amount ratio of deionized water are 2.35g：The volume ratio of 40mL, the concentrated sulfuric acid and deionized water is 1:13；
(2) poly glycol monomethyl ether and absolute ethyl alcohol are mixed into solid dissolving, step (1) system is then slowly added dropwise
The solution A obtained, stirring reaction 17h, toward addition isopropanol terminating reaction in reaction system after the completion of reaction, is filtered, filter at room temperature
Liquid adds deionized water, and rotary evaporation removes absolute ethyl alcohol, and sodium acid carbonate is added in remaining filtrate up to bubble-free in filtrate
Produce, then remove the water in filtrate, remaining filtrate removes chloroform, Ran Houxiang with chloroform extraction, suction filtration, filtrate
Hydrochloric acid solution is added in remaining filtrate to filtrate pH to 1-2, then steams water and hydrogen chloride gas, last remaining material is used
Chloroform extraction, filter, filtrate steams chloroform, and carboxylated poly glycol monomethyl ether is made after cooling；Wherein, poly- second two
Alcohol monomethyl ether and the mass ratio of solution A are 1g：0.96mL；
(3) it will be placed in after y-type zeolite steam treatment in deionized water, 1h be ultrasonically treated under 500W power, is then added
Carboxylated poly glycol monomethyl ether obtained above, and the concentrated sulfuric acid is added dropwise, after being well mixed, 90 DEG C are to slowly warm up to, backflow is anti-
Answer 6h, backflow to be cooled to room temperature after terminating, filter, solid is washed repeatedly with absolute ethyl alcohol, is dried, is obtained modified zeolite of Y-type；Its
In, y-type zeolite, carboxylated poly glycol monomethyl ether, the mass ratio of the concentrated sulfuric acid are 1:0.5:0.033；
(4) modified zeolite of Y-type obtained above is placed in pressure ＜ 0.1MPa reaction vessel, then by trifluoromethyl
Sulfonic acid is slowly injected into reaction vessel, obtains loaded catalyst；Wherein, the quality of modified zeolite of Y-type, trifluoromethane sulfonic acid
Than for 3：1.5；
(5) it is added to after being well mixed the methyl cyclosiloxane mixed methylcyclosiloxane after drying process and HMDO
In reaction vessel, under nitrogen protection, loaded catalyst obtained above is added into reactor, slowly heating after being well mixed
To 60-70 DEG C, isothermal reaction 3h, reaction is cooled to room temperature after terminating, and filters, and obtained filtrate is washed with deionized to neutrality
And low-boiling-point substance is removed, obtain dimethicone；Wherein, methyl cyclosiloxane mixed methylcyclosiloxane, HMDO, support type are urged
The mass ratio of agent is 5：:1：0.7；
(6) according to each component dosage, glycerine, xanthans, dimethicone, potassium sorbate, flavoring essence, pure is weighed respectively
Change water, load weighted each raw material is poured into mixer, 20min is stirred under 600r/min rotating speed, is mixed after stirring
Close liquid；
(7) mixed liquor obtained above is poured into filling in bottle placer, is then charged into plastic sealing bag, 200 DEG C of sealings are close
The product and specification sealed are put into carton, irradiation sterilization, medicine equipment are made and imports lubricant.
Embodiment 4
A kind of medicine equipment imports lubricant, in parts by weight, including following components：
5 parts of glycerine, 0.3 part of xanthans,
10 parts of dimethicone, 0.05 part of potassium sorbate,
0.2 part of flavoring essence, 82 parts of purified water,
Its preparation method comprises the following steps：
(1) chrome green and deionized water are mixed, in the state of 10-15 DEG C of temperature, speed of agitator 1000r/min
Then stirring is added dropwise the concentrated sulfuric acid, continues to stir 30min, obtained solution A after being added dropwise while stirring to solid dissolving；
Wherein, chrome green and the amount ratio of deionized water are 2.35g：The volume ratio of 40mL, the concentrated sulfuric acid and deionized water is 1:13；
(2) poly glycol monomethyl ether and absolute ethyl alcohol are mixed into solid dissolving, step (1) system is then slowly added dropwise
The solution A obtained, stirring reaction 18h, toward addition isopropanol terminating reaction in reaction system after the completion of reaction, is filtered, filter at room temperature
Liquid adds deionized water, and rotary evaporation removes absolute ethyl alcohol, and sodium acid carbonate is added in remaining filtrate up to bubble-free in filtrate
Produce, then remove the water in filtrate, remaining filtrate removes chloroform, Ran Houxiang with chloroform extraction, suction filtration, filtrate
Hydrochloric acid solution is added in remaining filtrate to filtrate pH to 1-2, then steams water and hydrogen chloride gas, last remaining material is used
Chloroform extraction, filter, filtrate steams chloroform, and carboxylated poly glycol monomethyl ether is made after cooling；Wherein, poly- second two
Alcohol monomethyl ether and the mass ratio of solution A are 1g：0.97mL；
(3) it will be placed in after y-type zeolite steam treatment in deionized water, 1h be ultrasonically treated under 500W power, is then added
Carboxylated poly glycol monomethyl ether obtained above, and the concentrated sulfuric acid is added dropwise, after being well mixed, 90 DEG C are to slowly warm up to, backflow is anti-
Answer 8h, backflow to be cooled to room temperature after terminating, filter, solid is washed repeatedly with absolute ethyl alcohol, is dried, is obtained modified zeolite of Y-type；Its
In, y-type zeolite, carboxylated poly glycol monomethyl ether, the mass ratio of the concentrated sulfuric acid are 1:0.5:0.033；
(4) modified zeolite of Y-type obtained above is placed in pressure ＜ 0.1MPa reaction vessel, then by trifluoromethyl
Sulfonic acid is slowly injected into reaction vessel, obtains loaded catalyst；Wherein, the quality of modified zeolite of Y-type, trifluoromethane sulfonic acid
Than for 3：1.5；
(5) it is added to after being well mixed the methyl cyclosiloxane mixed methylcyclosiloxane after drying process and HMDO
In reaction vessel, under nitrogen protection, loaded catalyst obtained above is added into reactor, slowly heating after being well mixed
To 60-70 DEG C, isothermal reaction 3.5h, reaction is cooled to room temperature after terminating, and filters, and obtained filtrate is washed with deionized into
Property simultaneously removes low-boiling-point substance, obtains dimethicone；Wherein, methyl cyclosiloxane mixed methylcyclosiloxane, HMDO, support type
The mass ratio of catalyst is 5：:1.5：0.8；
(6) according to each component dosage, glycerine, xanthans, dimethicone, potassium sorbate, flavoring essence, pure is weighed respectively
Change water, load weighted each raw material is poured into mixer, 20min is stirred under 600r/min rotating speed, is mixed after stirring
Close liquid；
(7) mixed liquor obtained above is poured into filling in bottle placer, is then charged into plastic sealing bag, 200 DEG C of sealings are close
The product and specification sealed are put into carton, irradiation sterilization, medicine equipment are made and imports lubricant.
In order to determine the greasy property of lubricant obtained above, catheter is immersed in by the present invention by taking catheter as an example
Keep 30min in lubricant obtained above, dried at 50 DEG C to constant weight, and by weight be 1500g, floor space 38.5cm2、
The counterweight of bottom surface roughness is put above catheter after treatment, is advanced with 0.4m/min speed horizontally tracting counterweight, measure
Tractive force, and coefficient of friction is calculated, after testing, the coefficient of friction of the catheter after processing is 0.0012-0.0013, and untreated
The coefficient of friction of catheter surface be 0.3722, illustrate that the catheter surface after the obtained lubricant coating of the present invention has very
Good greasy property.
Claims (9)
1. a kind of medicine equipment imports the preparation method of lubricant, it is characterised in that comprises the following steps：
(1) chrome green and deionized water are mixed, stirred in the state of 10-11 DEG C of temperature, speed of agitator 1000r/min
To solid dissolving, the concentrated sulfuric acid is then added dropwise while stirring, continues to stir 30min, obtained solution A after being added dropwise；
(2) poly glycol monomethyl ether and absolute ethyl alcohol are mixed into solid dissolving, it is obtained that step (1) is then slowly added dropwise
Solution A, stirring reaction 11-20h, toward addition isopropanol terminating reaction in reaction system after the completion of reaction, is filtered, filtrate at room temperature
Deionized water is added, rotary evaporation removes absolute ethyl alcohol, adds sodium acid carbonate in remaining filtrate until bubble-free is produced in filtrate
It is raw, then remove the water in filtrate, remaining filtrate with chloroform extraction, filter, filtrate removes chloroform, then to residual
Hydrochloric acid solution is added in remaining filtrate to filtrate pH to 1-2, then steams water and hydrogen chloride gas, last remaining material is with three
Chloromethanes extracts, and filters, and filtrate steams chloroform, and carboxylated poly glycol monomethyl ether is made after cooling；
(3) it will be placed in after y-type zeolite steam treatment in deionized water, 1h be ultrasonically treated under 100W power, is then added above-mentioned
Obtained carboxylated poly glycol monomethyl ether, and the concentrated sulfuric acid is added dropwise, after being well mixed, 90 DEG C are to slowly warm up to, back flow reaction 1-
10h, backflow are cooled to room temperature after terminating, and filter, and solid is washed repeatedly with absolute ethyl alcohol, dry, obtain modified zeolite of Y-type；
(4) modified zeolite of Y-type obtained above is placed in pressure ＜ 0.1MPa reaction vessel, then by trifluoromethane sulfonic acid
It is slowly injected into reaction vessel, obtains loaded catalyst；
(1) reaction is added to after being well mixed the methyl cyclosiloxane mixed methylcyclosiloxane after drying process and HMDO
In container, under nitrogen protection, loaded catalyst obtained above is added into reactor, is to slowly warm up to after well mixed
60-70 DEG C, isothermal reaction 2-4h, reaction is cooled to room temperature after terminating, and filters, and obtained filtrate is washed with deionized to neutrality
And low-boiling-point substance is removed, obtain dimethicone；
(6) according to each component dosage, glycerine, xanthans, dimethicone, potassium sorbate, flavoring essence, purifying are weighed respectively
Water, load weighted each raw material is poured into mixer, 20min is stirred under 600r/min rotating speed, is mixed after stirring
Liquid；
(7) mixed liquor obtained above is poured into filling in bottle placer, is then charged into plastic sealing bag, 200 DEG C of sealings, good seal
Product and specification be put into carton, irradiation sterilization, medicine equipment is made and imports lubricant.
2. a kind of medicine equipment as claimed in claim 1 imports the preparation method of lubricant, it is characterised in that each component dosage
It is respectively in parts by weight：Glycerine 3-6 parts, xanthans 0.1-0.1 parts, dimethicone 8-12 parts, potassium sorbate 0.03-0.07
Part, flavoring essence 0.1-0.3 parts, purified water 80-81 parts.
3. a kind of medicine equipment as claimed in claim 2 imports the preparation method of lubricant, it is characterised in that each component dosage
It is respectively in parts by weight：1 part of glycerine, 0.1 part of xanthans, 10 parts of dimethicone, 0.01 part of potassium sorbate, flavoring essence
0.1 part, 84.31 parts of purified water.
4. a kind of medicine equipment as claimed in claim 1 imports the preparation method of lubricant, it is characterised in that in step (1),
The chrome green and the amount ratio of deionized water are 2.31g：40mL.
5. a kind of medicine equipment as claimed in claim 1 imports the preparation method of lubricant, it is characterised in that in step (1),
The volume ratio of the concentrated sulfuric acid and deionized water is 1:13.
6. a kind of medicine equipment as claimed in claim 1 imports the preparation method of lubricant, it is characterised in that in step (2),
The poly glycol monomethyl ether and the mass ratio of solution A are 1g：(0.91-1)mL.
7. a kind of medicine equipment as claimed in claim 1 imports the preparation method of lubricant, it is characterised in that in step (3),
The y-type zeolite, carboxylated poly glycol monomethyl ether, the mass ratio of the concentrated sulfuric acid are 1:0.1:0.033.
8. a kind of medicine equipment as claimed in claim 1 imports the preparation method of lubricant, it is characterised in that in step (4),
The modified zeolite of Y-type, the mass ratio of trifluoromethane sulfonic acid are 3：(1-2).
9. a kind of medicine equipment as claimed in claim 1 imports the preparation method of lubricant, it is characterised in that in step (1),
Methyl cyclosiloxane mixed methylcyclosiloxane, HMDO, the mass ratio of loaded catalyst are 1：(0.8-2.8)：(0.1-
1)。
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| CN201710500335.3A CN107441563B (en) | 2017-06-27 | 2017-06-27 | Preparation method of medical instrument introduction lubricant |
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