CN113370548A - Polyurethane condom forming method based on wet process - Google Patents
Polyurethane condom forming method based on wet process Download PDFInfo
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- CN113370548A CN113370548A CN202110139645.3A CN202110139645A CN113370548A CN 113370548 A CN113370548 A CN 113370548A CN 202110139645 A CN202110139645 A CN 202110139645A CN 113370548 A CN113370548 A CN 113370548A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C69/00—Combinations of shaping techniques not provided for in a single one of main groups B29C39/00 - B29C67/00, e.g. associations of moulding and joining techniques; Apparatus therefore
- B29C69/02—Combinations of shaping techniques not provided for in a single one of main groups B29C39/00 - B29C67/00, e.g. associations of moulding and joining techniques; Apparatus therefore of moulding techniques only
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C37/00—Component parts, details, accessories or auxiliary operations, not covered by group B29C33/00 or B29C35/00
- B29C37/0003—Discharging moulded articles from the mould
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C37/00—Component parts, details, accessories or auxiliary operations, not covered by group B29C33/00 or B29C35/00
- B29C37/0092—Drying moulded articles or half products, e.g. preforms, during or after moulding or cooling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
- B29C41/02—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor for making articles of definite length, i.e. discrete articles
- B29C41/14—Dipping a core
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
- B29C41/02—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor for making articles of definite length, i.e. discrete articles
- B29C41/22—Making multilayered or multicoloured articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C67/00—Shaping techniques not covered by groups B29C39/00 - B29C65/00, B29C70/00 or B29C73/00
- B29C67/0044—Shaping techniques not covered by groups B29C39/00 - B29C65/00, B29C70/00 or B29C73/00 for shaping edges or extremities
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/02—Direct processing of dispersions, e.g. latex, to articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2075/00—Use of PU, i.e. polyureas or polyurethanes or derivatives thereof, as moulding material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2031/00—Other particular articles
- B29L2031/753—Medical equipment; Accessories therefor
- B29L2031/7538—Condoms
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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Abstract
The invention relates to a polyurethane condom forming method based on a wet process, which comprises the processes of emulsion preparation (preparation of emulsion of a plurality of isolation layers), film forming, formation of a tail edge of a condom, immersion of a mould and a film sleeve layer in a swelling agent, washing and demoulding of the film sleeve layer from the mould and the like, and finally polyurethane condom forming is completed. The invention adopts a wet water demoulding process, greatly reduces the labor cost, improves the product stability and the yield, and can greatly reduce the total production cost.
Description
Technical Field
The invention relates to a preparation process of condoms, in particular to wet preparation of condoms with polyurethane as a main component.
Background
The polyurethane material is a synthetic material and has the characteristics of high strength, high compactness, biocompatibility and the like. Compared with the traditional natural latex condom, the polyurethane condom can be thinner, has higher strength and is not allergic.
Much research in the prior art has been directed to improving polyurethane materials as a raw material for condoms, for example, to improving the strength, thickness, resilience, chemical resistance, puncture resistance, etc. of the materials. However, the demolding process of the polyurethane condom is difficult, special equipment and labor consumption are needed, and the production efficiency is low.
Disclosure of Invention
The invention aims to provide a polyurethane condom forming method based on a wet process, which comprises the following steps:
the method comprises the following steps:
preparation of emulsion:
1-1) preparation of emulsion of a third isolating layer:
the third isolating layer emulsion comprises the following components in parts by weight:
1-2) preparation of emulsion of a second isolation layer:
99.94-99.98 parts of waterborne polyurethane emulsion B
0.01 to 0.03 portion of defoaming agent
0.01-0.03 part of flatting agent
1-3 preparation of emulsion of a first isolation layer:
film forming:
respectively immersing the condom die into the third isolation layer emulsion, the second isolation layer emulsion and the first isolation layer emulsion to form a film sleeve layer with a multilayer film structure on the surface of the condom die;
curling the surface film layer on the mould to form the tail edge of the condom;
completely immersing the mould and the membrane sleeve layer into a swelling agent;
and 5, adopting high-pressure fluid to wash the film sleeve layer from the mould and demould the film sleeve layer to finish the forming of the polyurethane condom.
Scheme two, including the following steps:
preparation of emulsion:
1-1) preparation of emulsion of a second isolation layer:
99.94-99.98 parts of waterborne polyurethane emulsion B
0.01 to 0.03 portion of defoaming agent
0.01-0.03 part of flatting agent
1-2) preparing emulsion of a first isolation layer:
film forming:
respectively immersing the condom die into the second isolation layer emulsion and the first isolation layer emulsion to form a film sleeve layer with a multilayer film structure on the surface of the condom die;
curling the surface film layer on the mould to form the tail edge of the condom;
completely immersing the mould and the membrane sleeve layer into a swelling agent;
and 5, adopting high-pressure fluid to wash the film sleeve layer from the mould and demould the film sleeve layer to finish the forming of the polyurethane condom.
Further, the preparation process of the emulsion of the third isolating layer is as follows: mixing the fumed silica with a dispersing agent and water, grinding and dispersing by adopting a nano sand mill or a circulating grinder, and stopping grinding when the particle size of the fumed silica is detected to reach 50-500nm to obtain the fumed silica aqueous dispersion. And stirring and mixing the dispersion liquid, the waterborne polyurethane emulsion A, the film forming agent, the defoaming agent and the flatting agent to obtain a third isolation layer emulsion.
Further, the preparation process of the emulsion of the second isolating layer comprises the following steps: and stirring and mixing the aqueous polyurethane emulsion B, the defoaming agent and the flatting agent to obtain a second isolation layer emulsion.
Further, the preparation process of the emulsion of the first isolating layer comprises the following steps: mixing the fumed silica with a dispersing agent and water, grinding and dispersing by adopting a nano sand mill or a circulating grinder, and stopping grinding when the particle size of the fumed silica is detected to reach 50-500nm to obtain the fumed silica aqueous dispersion. And stirring and mixing the dispersion liquid, the waterborne polyurethane emulsion C, the film forming agent, the defoaming agent and the flatting agent to obtain the first isolation layer emulsion.
The film forming agent, the flatting agent, the defoaming agent and the dispersing agent used in the invention are commercially available nontoxic finished products.
Further, in the first embodiment, the aqueous polyurethane emulsion a, the aqueous polyurethane emulsion B and the aqueous polyurethane emulsion C are different types of polyurethane materials.
Further, in the second embodiment, the aqueous polyurethane emulsion B and the aqueous polyurethane emulsion C are different types of polyurethane materials.
Further, in the first scheme, the aqueous polyurethane emulsion A, the aqueous polyurethane emulsion B and the aqueous polyurethane emulsion C are polyurethane materials of the same type. Further, in the second scheme, the aqueous polyurethane emulsion B and the aqueous polyurethane emulsion C are polyurethane materials of the same type.
Further, in the film forming process of the step 2), when the condom die is respectively immersed into various isolating layer emulsions, one emulsion is immersed for multiple times each time, so that a film sleeve layer with a multilayer film structure is formed on the surface of the condom die;
further, in the film forming process of the step 2), respectively immersing the condom die into various isolation layer emulsions, and repeating the step 2) for a plurality of times when a film sheath layer with a multilayer film structure is formed on the surface of the condom die, so that the film sheath layer with the multilayer film structure is formed on the surface of the condom die; repeating the step 2 every time, drying the surface of the condom die firstly.
Further, when the condom die is immersed into the emulsion of the third isolation layer, the temperature of the emulsion is 20-35 ℃, the time of the die in the emulsion is 10-60 seconds, and after the condom die is taken out of the emulsion of the third isolation layer, the condom die is dried in a drying tunnel at the temperature of 90-120 ℃;
further, when the condom die is immersed into the emulsion of the second isolation layer, the temperature of the emulsion is 20-35 ℃, the time of the die in the emulsion is 10-60 seconds, and after the condom die is taken out of the emulsion of the second isolation layer, the condom die is dried in a drying tunnel at the temperature of 90-120 ℃;
further, when the condom die is immersed into the emulsion of the first isolation layer, the temperature of the emulsion is 20-35 ℃, the time of the die in the emulsion is 10-60 seconds, and after the condom die is taken out of the emulsion of the first isolation layer, the condom die is dried in a drying tunnel at the temperature of 90-120 ℃.
Further, in the step 3, a rubber roller is adopted to brush the surface film sleeve layer on the die in a rolling manner, so that the opening end of the film sleeve layer forms a tail edge.
Further, in step 4), the swelling agent is: one or a mixture of water, methanol, ethanol, isopropanol, butanol, isobutanol, ethylene glycol methyl ether, ethylene glycol ethyl ether, ethylene glycol butyl ether, ethylene glycol monomethyl ether, ethylene glycol monobutyl ether, propylene glycol methyl ether, propylene glycol butyl ether, propylene glycol methyl ether acetate, propylene glycol ethyl ether acetate, ethylene glycol methyl ether acetate, acetone, butanone, cyclohexanone, methyl isobutyl ketone, ethyl acetate, butyl acetate, tetrahydrofuran, dichloromethane, dimethylformamide and dimethylacetamide, and the temperature is 20-40 ℃.
Further, step 5, after demoulding, drying the obtained film sleeve; and (4) sequentially inspecting the dried film sleeve, adding lubricating oil and packaging to obtain the finished product condom.
Further, when drying, the film sleeve is firstly immersed into the desiccant water dispersion liquid to obtain the condom with the surface adsorbed with the desiccant dispersion liquid; and then putting the condom with the surface adsorbed with the drying agent dispersion liquid into a dryer for baking to remove the moisture in the condom, wherein the baking temperature is 60-100 ℃.
The preparation method of the polyurethane material which can be adopted by the invention comprises the following steps:
1S ] synthesis of aqueous polyurethane emulsion:
1S-1 ] prepolymer synthesis:
in a reactor, stirring and mixing dehydrated polymer polyol, hydroxyl-terminated siloxane diol and diisocyanate, heating for reaction, adding a hydrophilic chain extender and a diluent, continuing the reaction, and cooling to obtain a prepolymer;
1S-S2, neutralizing the prepolymer and emulsifying;
1S-S3, adding an amine chain extender aqueous solution into the product treated in the step S1-2 for post chain extension to obtain an emulsion product.
And 1S-4, removing the solvent in the products of the steps S1-S3 by reduced pressure distillation to obtain the aqueous polyurethane emulsion.
S2 preparation of curing agent emulsion: and sequentially adding epoxy modified silicone oil and an emulsifier into a reaction kettle, stirring to uniformly mix, adding deionized water, and continuously stirring to emulsify a product to obtain a curing agent emulsion.
S3 preparation of waterborne polyurethane condom emulsion: and (4) mixing the aqueous polyurethane emulsion obtained in the step S1 with the curing agent emulsion obtained in the step S2 to obtain the aqueous polyurethane condom emulsion.
Further, in step S1-1, the raw materials and the mixture ratio for synthesizing the prepolymer are as follows:
further, in step S1-1, the polymer diol is selected from polymers having low crystallinity and being liquid at room temperature. Further, in the step S1-1, the polymer diol is selected from polyether diol or polyester diol. Further, in the step S1-1, the molecular weight of the polymer diol is 800-3000.
Further, in step S1-1, the hydroxyl-terminated siloxane diol has a molecular weight of 600-800, contains a plurality of siloxane groups, and has hydroxyl-reactive functional groups at both ends. Further, in step S1-1, the chemical formula of the hydroxyl-terminated siloxane diol is as follows:
or
Or
Or
Wherein: r is' CH3- "or" CH3CH2- ", m, n, k, j and u are all natural numbers.
Further, in step S1-1, the diisocyanate is isophorone diisocyanate, toluene diisocyanate, or hydrogenated phenyl methane diisocyanate.
Further, in step S1-1, the hydrophilic chain extender is selected from any one of dimethylolpropionic acid (DMPA) or dimethylolbutyric acid (DMBA).
Further, in the step S1-1, the amine chain extender is polyetheramine with a molecular weight of 200-400, and the concentration of the aqueous solution of the amine chain extender is 5-15%.
Further, in the step S1-1, the diluent is any one selected from the group consisting of acetone, butanone, N-methylpyrrolidone, and N, N-dimethylformamide.
Further, in the step S1-1, the polymer polyol, the hydroxyl-terminated siloxane diol and the diisocyanate are stirred and mixed, heated to 70-90 ℃, reacted for 2-3 hours, added with the hydrophilic chain extender and the diluent, continuously reacted for 2-3 hours, cooled to 40-60 ℃, added with the diluent and adjusted in viscosity, and the prepolymer is obtained.
Further, in the steps S1 to S2, after neutralization with triethylamine, an ice-water mixture is added to carry out high-speed emulsification.
Further, in the step S1-S3, the amine chain extender is selected from polyether amine 400 or polyether amine 200. Slowly (about half an hour) dripping the amine chain extender aqueous solution, continuously stirring for about 1 hour after dripping, and standing for defoaming to obtain an emulsion product.
In a preferred scheme, in the step S1, all the raw materials are in the following ratio:
further, in step S2, the raw materials are in the following mixture ratio:
30-40 parts of epoxy modified silicone oil
1-3 parts of emulsifier
60-70 parts of deionized water
Further, in step S2, the epoxy-modified silicone oil is any one of a double-end epoxy silicone oil and a side chain epoxy silicone oil.
Further, in step S2, the emulsifier is an anionic or nonionic emulsifier. Further, in step S2, the emulsifier is selected from anionic emulsifiers (selected from any one of sodium lauryl alcohol succinate monoester sulfonate, disodium nonylphenol polyoxyethylene (9) ether sulfosuccinate, disodium alkanolamide succinate monoester, sodium cocoamidoalkanol sulfate, anionic polyurethane surfactant and sodium methyl stearate sulfonate), and the nonionic emulsifiers are selected from any one of polyoxypropylene polyoxyethylene ether propylene glycol ether, polyglycerol fatty acid ester, polyoxyethylene (60) sorbitan monostearate, polyethylene glycol distearate, polyethylene glycol (600) dilaurate, hydroxypropyl methyl cellulose and dodecylphenol polyoxyethylene ether.)
The epoxy value of the epoxy modified silicone oil is between 0.1 and 0.9.
Further, in step S2, deionized water is added, the stirring speed is adjusted to 2000r/min, and emulsification is carried out for 30-60 min.
Further, in step S3, the mass ratio of the aqueous polyurethane emulsion to the curing agent emulsion is (5-15) to 1.
The technical effect of the invention is undoubtedly that the wet water demoulding process is adopted, thereby greatly reducing the labor cost, improving the product stability and the yield and greatly reducing the total production cost.
Drawings
FIG. 1 is a water-based polyurethane condom without adhesion, which is taken out after drying;
FIG. 2 is a scanning electron microscope image of the washed waterborne polyurethane condom, and it can be seen that a layer of separant silicon dioxide powder is adsorbed on the surface of the film.
Detailed Description
The present invention is further illustrated by the following examples, but it should not be construed that the scope of the above-described subject matter is limited to the following examples. Various substitutions and alterations can be made without departing from the technical idea of the invention and the scope of the invention is covered by the present invention according to the common technical knowledge and the conventional means in the field.
Example 1:
a polyurethane condom forming method based on wet process technology comprises the following steps:
the method comprises the following steps:
preparation of emulsion:
1-1) preparation of emulsion of a third isolating layer:
the third isolating layer emulsion comprises the following components in parts by weight:
mixing the fumed silica with a dispersing agent and water, grinding and dispersing by adopting a nano sand mill or a circulating grinder, and stopping grinding when the particle size of the fumed silica is detected to reach 50-500nm to obtain the fumed silica aqueous dispersion. And stirring and mixing the dispersion liquid, the waterborne polyurethane emulsion A, the film forming agent, the defoaming agent and the flatting agent to obtain a third isolation layer emulsion.
1-2) preparation of emulsion of a second isolation layer:
99.94 parts of waterborne polyurethane emulsion B
0.01 part of defoaming agent
0.01 part of flatting agent
And stirring and mixing the aqueous polyurethane emulsion B, the defoaming agent and the flatting agent to obtain a second isolation layer emulsion.
1-3 preparation of emulsion of a first isolation layer:
and (3) mixing the fumed silica with a dispersing agent and water, grinding and dispersing by adopting a nano sand mill or a circulating grinder, and stopping grinding when the particle size of the fumed silica reaches 50nm to obtain the fumed silica aqueous dispersion. And stirring and mixing the dispersion liquid, the waterborne polyurethane emulsion C, the film forming agent, the defoaming agent and the flatting agent to obtain the first isolation layer emulsion.
Film forming:
respectively immersing the condom die into the third isolation layer emulsion, the second isolation layer emulsion and the first isolation layer emulsion to form a film sleeve layer with a multilayer film structure on the surface of the condom die;
when the condom die is immersed in the emulsion of the third isolation layer, the temperature of the emulsion is 20 ℃, the time of the die in the emulsion is 10 seconds, and after the condom die is taken out of the emulsion of the third isolation layer, the condom die is dried in a drying tunnel at the temperature of 90 ℃;
when the condom die is immersed in the emulsion of the second isolation layer, the temperature of the emulsion is 20 ℃, the time of the die in the emulsion is 10 seconds, and after the condom die is taken out of the emulsion of the second isolation layer, the condom die is dried in a drying tunnel at the temperature of 90 ℃;
when the condom die is immersed in the emulsion of the first isolation layer, the temperature of the emulsion is 20 ℃, the time of the die in the emulsion is 10 seconds, and after the condom die is taken out of the emulsion of the first isolation layer, the condom die is dried in a drying tunnel at 90 ℃.
And 3, curling the surface film layer on the mould to form the tail edge of the condom. Namely, the rubber roller is adopted to carry out rolling brush curling treatment on the film sleeve layer on the surface of the die, so that the opening end of the film sleeve layer forms the tail edge of the condom.
Completely immersing the mould and the membrane sleeve layer into a swelling agent; the swelling agent is: ethanol at 20 ℃.
And 5, adopting high-pressure fluid to wash the film sleeve layer from the mould and demould the film sleeve layer to finish the forming of the polyurethane condom.
After demolding, drying the obtained film sleeve; and (4) sequentially inspecting the dried film sleeve, adding lubricating oil and packaging to obtain the finished product condom.
When drying, firstly, immersing the film sleeve into the desiccant water dispersion liquid to obtain the condom with the surface adsorbed with the desiccant dispersion liquid; and then putting the condom with the surface adsorbed with the drying agent dispersion liquid into a dryer for baking to remove the moisture in the condom, wherein the baking temperature is 60-100 ℃.
Example 2:
a polyurethane condom forming method based on wet process technology comprises the following steps:
the method comprises the following steps:
preparation of emulsion:
1-1) preparation of emulsion of a third isolating layer:
the third isolating layer emulsion comprises the following components in parts by weight:
mixing the fumed silica with a dispersing agent and water, grinding and dispersing by adopting a nano sand mill or a circulating grinder, and stopping grinding when the particle size of the fumed silica is detected to reach 50-500nm to obtain the fumed silica aqueous dispersion. And stirring and mixing the dispersion liquid, the waterborne polyurethane emulsion A, the film forming agent, the defoaming agent and the flatting agent to obtain a third isolation layer emulsion.
1-2) preparation of emulsion of a second isolation layer:
99.98 parts of waterborne polyurethane emulsion B
0.03 portion of defoaming agent
0.03 part of flatting agent
And stirring and mixing the aqueous polyurethane emulsion B, the defoaming agent and the flatting agent to obtain a second isolation layer emulsion.
1-3 preparation of emulsion of a first isolation layer:
and (3) mixing the fumed silica with a dispersing agent and water, grinding and dispersing by adopting a nano sand mill or a circulating grinder, and stopping grinding when the particle size of the fumed silica is detected to reach 500nm to obtain the fumed silica aqueous dispersion. And stirring and mixing the dispersion liquid, the waterborne polyurethane emulsion C, the film forming agent, the defoaming agent and the flatting agent to obtain the first isolation layer emulsion.
Film forming:
respectively immersing the condom die into the third isolation layer emulsion, the second isolation layer emulsion and the first isolation layer emulsion to form a film sleeve layer with a multilayer film structure on the surface of the condom die;
when the condom die is immersed in the emulsion of the third isolation layer, the temperature of the emulsion is 35 ℃, the time of the die in the emulsion is 60 seconds, and after the condom die is taken out of the emulsion of the third isolation layer, the condom die is dried in a drying tunnel at the temperature of 120 ℃;
when the condom die is immersed in the emulsion of the second isolation layer, the temperature of the emulsion is 35 ℃, the time of the die in the emulsion is 10-60 seconds, and after the condom die is taken out of the emulsion of the second isolation layer, the condom die is dried in a drying tunnel at 120 ℃;
when the condom die is immersed in the emulsion of the first isolation layer, the temperature of the emulsion is 35 ℃, the time of the die in the emulsion is 60 seconds, and after the condom die is taken out of the emulsion of the first isolation layer, the condom die is dried in a drying tunnel at 120 ℃.
And 3, curling the surface film layer on the mould to form the tail edge of the condom. Namely, the rubber roller is adopted to carry out rolling brush curling treatment on the film sleeve layer on the surface of the die, so that the opening end of the film sleeve layer forms the tail edge of the condom.
Completely immersing the mould and the membrane sleeve layer into a swelling agent; the swelling agent is: ethyl acetate, temperature 40 ℃.
And 5, adopting high-pressure fluid to wash the film sleeve layer from the mould and demould the film sleeve layer to finish the forming of the polyurethane condom.
After demolding, drying the obtained film sleeve; and (4) sequentially inspecting the dried film sleeve, adding lubricating oil and packaging to obtain the finished product condom.
When drying, firstly, immersing the film sleeve into the desiccant water dispersion liquid to obtain the condom with the surface adsorbed with the desiccant dispersion liquid; and then putting the condom with the surface adsorbed with the drying agent dispersion liquid into a dryer for baking to remove the moisture in the condom, wherein the baking temperature is 100 ℃.
Example 3:
this example provides three aqueous polyurethane emulsion preparation processes that can be used in the above method:
the first scheme is as follows:
synthesis of aqueous polyurethane emulsion:
1-1. into a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, 18 parts by weight of dehydrated polymer polyol and 1 part by weight of hydroxy-terminated siloxane diol are sequentially chargedAnd 4 parts of toluene diisocyanateStirring, mixing and heating to 70 ℃, reacting for 2 hours, adding 1 part of dimethylolpropionic acid (DMPA) and a proper amount of diluent acetone, continuing to react for 2 hours, then cooling to 40 ℃, and adding a proper amount of diluent acetone to adjust the viscosity, thus obtaining the prepolymer.
1-2) neutralizing the prepolymer product of the step 1-1) with 1 part of triethylamine for 30 minutes, and then adding 65 parts of an ice-water mixture for high-speed emulsification.
1-3 ] dispersing the prepolymer, slowly adding 0.1 part of polyetheramine 200 aqueous solution for post-chain extension, dropwise adding the amine chain extender aqueous solution in half an hour, continuously stirring for 1 hour after dropwise adding, and standing for defoaming to obtain a blue semitransparent emulsion.
And 1-4, distilling under reduced pressure to remove the solvent to obtain the aqueous polyurethane emulsion.
Preparation of curing agent emulsion:
30 parts of epoxy modified silicone oil (with the epoxy value of 0.1) and 1 part of sodium cocoamidoalkanol sulfate as an emulsifier are sequentially added into a reaction kettle provided with a stirring device, and the mixture is stirred and mixed uniformly. Then 60 parts of deionized water is added, the stirring speed is adjusted to 2000r/min, and emulsification is carried out for 30min, so as to obtain the curing agent emulsion.
Preparing aqueous polyurethane condom emulsion:
and mixing the aqueous polyurethane emulsion and the curing agent emulsion according to the mass ratio of 5: 1 to obtain the aqueous polyurethane condom emulsion.
Scheme II:
synthesis of aqueous polyurethane emulsion:
1-1. into a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, 25 parts by weight of dehydrated polymer polyol and 2 parts by weight of hydroxy-terminated siloxane diol are sequentially chargedAnd 8 parts of isophorone diisocyanate (IPDI), stirring, mixing, heating to 80 ℃, reacting for 3 hours, adding 2 parts of dimethylolbutyric acid (DMBA) and a proper amount of butanone serving as a diluent, continuously reacting for 3 hours, cooling to 60 ℃, and adding a proper amount of butanone serving as a diluent to adjust the viscosity to obtain a prepolymer.
1-2) neutralizing the prepolymer product obtained in the step 1-1 with 2 parts of triethylamine for 30 minutes, and then adding 75 parts of an ice-water mixture for high-speed emulsification.
1-3, after dispersing the prepolymer, slowly adding 0.8 part of polyetheramine 400 (amine chain extender) aqueous solution for post chain extension, dropwise adding the amine chain extender aqueous solution for half an hour, continuously stirring for 1 hour after dropwise adding, and standing for defoaming to obtain a blue semitransparent emulsion.
And 1-4, distilling under reduced pressure to remove the solvent to obtain the aqueous polyurethane emulsion.
Preparation of curing agent emulsion:
40 parts of epoxy modified silicone oil (with the epoxy value of 0.6) and 3 parts of emulsifier polyoxyethylene (60) sorbitan monostearate are sequentially added into a reaction kettle provided with a stirring device, and the mixture is stirred and mixed uniformly. And then 70 parts of deionized water is added, the stirring speed is adjusted to 2000r/min, and emulsification is carried out for 60min, so as to obtain the curing agent emulsion.
Preparing aqueous polyurethane condom emulsion:
and mixing the aqueous polyurethane emulsion and the curing agent emulsion according to the mass ratio of 15: 1 to obtain the aqueous polyurethane condom emulsion.
The third scheme is as follows:
synthesis of aqueous polyurethane emulsion:
1-1. into a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, 20 parts by weight of dehydrated polymer polyol and 1.5 parts by weight of hydroxy-terminated siloxane diol are sequentially chargedAnd 6 parts of hydrogenated phenyl methane diisocyanate, stirring, mixing, heating to 80 ℃, reacting for 1.5 hours, adding 1.5 parts of dimethylolbutyric acid (DMBA) and a proper amount of diluent N-methylpyrrolidone, continuing to react for 3 hours, cooling to 50 ℃, and adding a proper amount of diluent N-methylpyrrolidone to adjust the viscosity, thus obtaining the prepolymer.
1-2) neutralizing the prepolymer product of the step 1-1) with 1.5 parts of triethylamine for 30 minutes, and then adding 70 parts of an ice-water mixture for high-speed emulsification.
1-3, after dispersing the prepolymer, slowly adding 0.5 part of polyetheramine 200 (amine chain extender) aqueous solution for chain extension, dripping the amine chain extender aqueous solution for half an hour, continuously stirring for 1 hour after dripping, and standing for defoaming to obtain a blue semitransparent emulsion.
And 1-4, distilling under reduced pressure to remove the solvent to obtain the aqueous polyurethane emulsion.
Preparation of curing agent emulsion:
adding 35 parts of epoxy modified silicone oil (with an epoxy value of 0.3) and 2 parts of emulsifier nonylphenol polyoxyethylene (9) ether disodium sulfosuccinate into a reaction kettle provided with a stirring device in sequence, and opening, stirring and uniformly mixing. Then 65 parts of deionized water is added, the stirring speed is adjusted to 2000r/min, and emulsification is carried out for 50min, thus obtaining the curing agent emulsion.
Preparing aqueous polyurethane condom emulsion:
and mixing the aqueous polyurethane emulsion and the curing agent emulsion according to the mass ratio of 10: 1 to obtain the aqueous polyurethane condom emulsion.
Claims (10)
1. A polyurethane condom forming method based on a wet process is characterized by comprising the following steps:
preparation of emulsion:
1-1) preparation of emulsion of a third isolating layer:
the third isolating layer emulsion comprises the following components in parts by weight:
0.1-1 part of waterborne polyurethane emulsion A
0.1-1 part of fumed silica
92.84-99.47 parts of water
0.3-5 parts of film-forming agent
1-2) preparation of emulsion of a second isolation layer:
99.94-99.98 parts of waterborne polyurethane emulsion B
1-3 preparation of emulsion of a first isolation layer:
0.1-3 parts of waterborne polyurethane emulsion C
0.1-3 parts of fumed silica
93.34-99.76 parts of pure water
0.01-0.5 part of film-forming agent
Film forming:
respectively immersing the condom die into the third isolation layer emulsion, the second isolation layer emulsion and the first isolation layer emulsion to form a film sleeve layer with a multilayer film structure on the surface of the condom die;
curling the surface film layer on the mould to form the tail edge of the condom;
completely immersing the mould and the membrane sleeve layer into a swelling agent;
and 5, adopting high-pressure fluid to wash the film sleeve layer from the mould and demould the film sleeve layer to finish the forming of the polyurethane condom.
2. A polyurethane condom forming method based on a wet process is characterized by comprising the following steps:
preparation of emulsion:
1-1) preparation of emulsion of a second isolation layer:
99.94-99.98 parts of waterborne polyurethane emulsion B
1-2) preparing emulsion of a first isolation layer:
0.1-3 parts of waterborne polyurethane emulsion C
0.1-3 parts of fumed silica
93.34-99.76 parts of pure water
0.01-0.5 part of film-forming agent
Film forming:
respectively immersing the condom die into the second isolation layer emulsion and the first isolation layer emulsion to form a film sleeve layer with a multilayer film structure on the surface of the condom die;
curling the surface film layer on the mould to form the tail edge of the condom;
completely immersing the mould and the membrane sleeve layer into a swelling agent;
and 5, adopting high-pressure fluid to wash the film sleeve layer from the mould and demould the film sleeve layer to finish the forming of the polyurethane condom.
3. The method for forming polyurethane condoms according to claim 1, which is based on wet process, is characterized in that:
the preparation process of the emulsion of the third isolating layer comprises the following steps:
mixing, grinding and dispersing the fumed silica, a dispersing agent and water to obtain the fumed silica aqueous dispersion liquid.
And stirring and mixing the dispersion liquid, the waterborne polyurethane emulsion A, the film forming agent, the defoaming agent and the flatting agent to obtain a third isolation layer emulsion.
The preparation process of the emulsion of the second isolating layer comprises the following steps: and stirring and mixing the aqueous polyurethane emulsion B, the defoaming agent and the flatting agent to obtain a second isolation layer emulsion.
The preparation process of the emulsion of the first isolating layer comprises the following steps:
mixing, grinding and dispersing the fumed silica, a dispersing agent and water to obtain a fumed silica aqueous dispersion liquid; and stirring and mixing the dispersion liquid, the waterborne polyurethane emulsion C, the film forming agent, the defoaming agent and the flatting agent to obtain the first isolation layer emulsion.
4. The method for manufacturing polyurethane condoms according to claim 1, wherein: the aqueous polyurethane emulsion A, the aqueous polyurethane emulsion B and the aqueous polyurethane emulsion C are different types of polyurethane materials.
5. The method for manufacturing polyurethane condoms according to claim 1, wherein: the aqueous polyurethane emulsion A, the aqueous polyurethane emulsion B and the aqueous polyurethane emulsion C are polyurethane materials of the same type.
6. The method for manufacturing polyurethane condoms according to claim 1, wherein:
when the condom die is immersed into the emulsion of the third isolation layer, the temperature of the emulsion is 20-35 ℃, the time of the die in the emulsion is 10-60 seconds, and after the condom die is taken out of the emulsion of the third isolation layer, the condom die is dried in a drying tunnel at the temperature of 90-120 ℃;
when the condom die is immersed in the emulsion of the second isolation layer, the temperature of the emulsion is 20-35 ℃, the time of the die in the emulsion is 10-60 seconds, and after the condom die is taken out of the emulsion of the second isolation layer, the condom die is dried in a drying tunnel at the temperature of 90-120 ℃;
when the condom die is immersed in the emulsion of the first isolation layer, the temperature of the emulsion is 20-35 ℃, the time of the die in the emulsion is 10-60 seconds, and after the condom die is taken out of the emulsion of the first isolation layer, the condom die is dried in a drying tunnel at the temperature of 90-120 ℃.
7. The method for manufacturing polyurethane condoms according to claim 1, wherein: in the step 3, a rubber roller is adopted to brush the surface film sleeve layer on the die in a rolling way, so that the opening end of the film sleeve layer forms a tail edge.
8. The method for manufacturing polyurethane condoms according to claim 1, wherein: in step 4, the swelling agent is: one or a mixture of water, methanol, ethanol, isopropanol, butanol, isobutanol, ethylene glycol methyl ether, ethylene glycol ethyl ether, ethylene glycol butyl ether, ethylene glycol monomethyl ether, ethylene glycol monobutyl ether, propylene glycol methyl ether, propylene glycol butyl ether, propylene glycol methyl ether acetate, propylene glycol ethyl ether acetate, ethylene glycol methyl ether acetate, acetone, butanone, cyclohexanone, methyl isobutyl ketone, ethyl acetate, butyl acetate, tetrahydrofuran, dichloromethane, dimethylformamide and dimethylacetamide, and the temperature is 20-40 ℃.
9. The method for manufacturing polyurethane condoms according to claim 1, wherein: step 5, after demoulding, drying the obtained film sleeve; and (4) sequentially inspecting the dried film sleeve, adding lubricating oil and packaging to obtain the finished product condom.
10. The method for manufacturing polyurethane condoms according to claim 6, wherein: when drying, firstly, immersing the film sleeve into the desiccant water dispersion liquid to obtain the condom with the surface adsorbed with the desiccant dispersion liquid; and then putting the condom with the surface adsorbed with the drying agent dispersion liquid into a dryer for baking to remove the moisture in the condom.
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